[Title 40 CFR ]
[Code of Federal Regulations (annual edition) - July 1, 2006 Edition]
[From the U.S. Government Printing Office]
[[Page i]]
40
Part 63 (Sec. 63.8980 to End)
Revised as of July 1, 2006
Protection of Environment
________________________
Containing a codification of documents of general
applicability and future effect
As of July 1, 2006
With Ancillaries
Published by
Office of the Federal Register
National Archives and Records
Administration
A Special Edition of the Federal Register
[[Page ii]]
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[[Page iii]]
Table of Contents
Page
Explanation................................................. v
Title 40:
Chapter I--Environmental Protection Agency
(Continued) 3
Finding Aids:
Material Approved for Incorporation by Reference........ 393
Table of CFR Titles and Chapters........................ 395
Alphabetical List of Agencies Appearing in the CFR...... 413
List of CFR Sections Affected........................... 423
[[Page iv]]
----------------------------
Cite this Code: CFR
To cite the regulations in
this volume use title,
part and section number.
Thus, 40 CFR 63.8980
refers to title 40, part
63, section 8980.
----------------------------
[[Page v]]
EXPLANATION
The Code of Federal Regulations is a codification of the general and
permanent rules published in the Federal Register by the Executive
departments and agencies of the Federal Government. The Code is divided
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parts covering specific regulatory areas.
Each volume of the Code is revised at least once each calendar year
and issued on a quarterly basis approximately as follows:
Title 1 through Title 16.................................as of January 1
Title 17 through Title 27..................................as of April 1
Title 28 through Title 41...................................as of July 1
Title 42 through Title 50................................as of October 1
The appropriate revision date is printed on the cover of each
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LEGAL STATUS
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HOW TO USE THE CODE OF FEDERAL REGULATIONS
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[[Page vi]]
Many agencies have begun publishing numerous OMB control numbers as
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Provisions that become obsolete before the revision date stated on
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What is a proper incorporation by reference? The Director of the
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(a) The incorporation will substantially reduce the volume of
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(b) The matter incorporated is in fact available to the extent
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(c) The incorporating document is drafted and submitted for
publication in accordance with 1 CFR part 51.
Properly approved incorporations by reference in this volume are
listed in the Finding Aids at the end of this volume.
What if the material incorporated by reference cannot be found? If
you have any problem locating or obtaining a copy of material listed in
the Finding Aids of this volume as an approved incorporation by
reference, please contact the agency that issued the regulation
containing that incorporation. If, after contacting the agency, you find
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20408, or call 202-741-6010.
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the revision dates of the 50 CFR titles.
[[Page vii]]
REPUBLICATION OF MATERIAL
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Director,
Office of the Federal Register.
July 1, 2006.
[[Page ix]]
THIS TITLE
Title 40--Protection of Environment is composed of thirty-one
volumes. The parts in these volumes are arranged in the following order:
parts 1-49, parts 50-51, part 52 (52.01-52.1018), part 52 (52.1019-End),
parts 53-59, part 60 (60.1-End), part 60 (Appendices), parts 61-62, part
63 (63.1-63.599), part 63 (63.600-63.1199), part 63 (63.1200-63.1439),
part 63 (63.1440-63.6175), part 63 (63.6580-63.8830), part 63 (63.8980-
End) parts 64-71, parts 72-80, parts 81-85, part 86 (86.1-86.599-99)
part 86 (86.600-1-End), parts 87-99, parts 100-135, parts 136-149, parts
150-189, parts 190-259, parts 260-265, parts 266-299, parts 300-399,
parts 400-424, parts 425-699, parts 700-789, and part 790 to End. The
contents of these volumes represent all current regulations codified
under this title of the CFR as of July 1, 2006.
Chapter I--Environmental Protection Agency appears in all thirty-one
volumes. An alphabetical Listing of Pesticide Chemicals Index appears in
parts 150-189. Regulations issued by the Council on Environmental
Quality appear in the volume containing part 790 to End. The OMB control
numbers for title 40 appear in Sec. 9.1 of this chapter.
For this volume, Robert J. Sheehan was Chief Editor. The Code of
Federal Regulations publication program is under the direction of
Frances D. McDonald, assisted by Alomha S. Morris.
[[Page 1]]
TITLE 40--PROTECTION OF ENVIRONMENT
(This book contains part 63)
--------------------------------------------------------------------
Part
chapter i--Environmental Protection Agency (Continued)...... 63
[[Page 3]]
CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)
--------------------------------------------------------------------
Editorial Note: Nomenclature changes to chapter I appear at 65 FR
47324, 47325, Aug. 2, 2000.
SUBCHAPTER C--AIR PROGRAMS (CONTINUED)
Part Page
63 National emission standards for hazardous
air pollutants for source categories.... 5
[[Page 5]]
SUBCHAPTER C_AIR PROGRAMS (CONTINUED)
PART 63_NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR
SOURCE CATEGORIES--Table of Contents
Subpart NNNNN_National Emission Standards for Hazardous Air Pollutants:
Hydrochloric Acid Production
What This Subpart Covers
63.8980 What is the purpose of this subpart?
63.8985 Am I subject to this subpart?
63.8990 What parts of my plant does this subpart cover?
63.8995 When do I have to comply with this subpart?
Emission Limitations and Work Practice Standards
63.9000 What emission limitations and work practice standards must I
meet?
General Compliance Requirements
63.9005 What are my general requirements for complying with this
subpart?
Testing and Initial Compliance Requirements
63.9010 By what date must I conduct performance tests?
63.9015 When must I conduct subsequent performance tests?
63.9020 What performance tests and other procedures must I use?
63.9025 What are my monitoring installation, operation, and maintenance
requirements?
63.9030 How do I demonstrate initial compliance with the emission
limitations and work practice standards?
Continuous Compliance Requirements
63.9035 How do I monitor and collect data to demonstrate continuous
compliance?
63.9040 How do I demonstrate continuous compliance with the emission
limitations and work practice standards?
Notifications, Reports, and Records
63.9045 What notifications must I submit and when?
63.9050 What reports must I submit and when?
63.9055 What records must I keep?
63.9060 In what form and how long must I keep my records?
Other Requirements and Information
63.9065 What parts of the General Provisions apply to me?
63.9070 Who implements and enforces this subpart?
63.9075 What definitions apply to this subpart?
Table 1 to Subpart NNNNN of Part 63--Emission Limits and Work Practice
Standards
Table 2 to Subpart NNNNN of Part 63--Operating Limits
Table 3 to Subpart NNNNN of Part 63--Performance Test Requirements for
HCl Production Affected Sources
Table 4 to Subpart NNNNN of Part 63--Initial Compliance with Emission
Limitations and Work Practice Standards
Table 5 to Subpart NNNNN of Part 63--Continuous Compliance with Emission
Limitations and Work Practice Standards
Table 6 to Subpart NNNNN of Part 63--Requirements for Reports
Table 7 to Subpart NNNNN of Part 63--Applicability of General Provisions
to Subpart NNNNN
Subpart OOOOO [Reserved]
Subpart PPPPP_National Emission Standards for Hazardous Air Pollutants
for Engine Test Cells/Stands
What This Subpart Covers
63.9280 What is the purpose of subpart PPPPP?
63.9285 Am I subject to this subpart?
63.9290 What parts of my plant does this subpart cover?
63.9295 When do I have to comply with this subpart?
Emission Limitations
63.9300 What emission limitation must I meet?
63.9301 What are my options for meeting the emission limits?
63.9302 What operating limits must I meet?
General Compliance Requirements
63.9305 What are my general requirements for complying with this
subpart?
63.9306 What are my continuous parameter monitoring system (CPMS)
installation, operation, and maintenance requirements?
63.9307 What are my continuous emissions monitoring system installation,
operation, and maintenance requirements?
Testing and Initial Compliance Requirements
63.9310 By what date must I conduct the initial compliance
demonstrations?
[[Page 6]]
63.9320 What procedures must I use?
63.9321 What are the general requirements for performance tests?
63.9322 How do I determine the emission capture system efficiency?
63.9323 How do I determine the add-on control device emission
destruction or removal efficiency?
63.9324 How do I establish the emission capture system and add-on
control device operating limits during the performance test?
63.9330 How do I demonstrate initial compliance with the emission
limitation?
Continuous Compliance Requirements
63.9335 How do I monitor and collect data to demonstrate continuous
compliance?
63.9340 How do I demonstrate continuous compliance with the emission
limitation?
Notifications, Reports, and Records
63.9345 What notifications must I submit and when?
63.9350 What reports must I submit and when?
63.9355 What records must I keep?
63.9360 In what form and how long must I keep my records?
Other Requirements and Information
63.9365 What parts of the General Provisions apply to me?
63.9370 Who implements and enforces this subpart?
63.9375 What definitions apply to this subpart?
Table 1 to Subpart PPPPP of Part 63--Emission Limitations
Table 2 to Subpart PPPPP of Part 63--Operating Limits
Table 3 to Subpart PPPPP of Part 63--Requirements for Initial Compliance
Demonstrations
Table 4 to Subpart PPPPP of Part 63--Initial Compliance with Emission
Limitations
Table 5 to Subpart PPPPP of Part 63--Continuous Compliance with Emission
Limitations
Table 6 to Subpart PPPPP of Part 63--Requirements for Reports
Table 7 to Subpart PPPPP of Part 63--Applicability of General Provisions
to Subpart PPPPP
Subpart QQQQQ_National Emission Standards for Hazardous Air Pollutants
for Friction Materials Manufacturing Facilities
What This Subpart Covers
63.9480 What is the purpose of this subpart?
63.9485 Am I subject to this subpart?
63.9490 What parts of my plant does this subpart cover?
63.9495 When do I have to comply with this subpart?
Emission Limitations
63.9500 What emission limitations must I meet?
General Compliance Requirements
63.9505 What are my general requirements for complying with this
subpart?
Initial Compliance Demonstration Requirements
63.9510 By what date must I conduct my initial compliance demonstration?
63.9515 How do I demonstrate initial compliance with the emission
limitation that applies to me?
63.9520 What procedures must I use to demonstrate initial compliance?
63.9525 What are the installation, operation, and maintenance
requirements for my weight measurement device?
Continuous Compliance Requirements
63.9530 How do I demonstrate continuous compliance with the emission
limitation that applies to me?
Notifications, Reports, and Records
63.9535 What notifications must I submit and when?
63.9540 What reports must I submit and when?
63.9545 What records must I keep?
63.9550 In what form and how long must I keep my records?
Other Requirements and Information
63.9555 What parts of the General Provisions apply to me?
63.9560 Who implements and enforces this subpart?
63.9565 What definitions apply to this subpart?
63.9570 How do I apply for alternative compliance requirements?
63.9571-63.9579 [Reserved]
Table 1 to Subpart QQQQQ--Applicability of General Provisions to Subpart
QQQQQ
Subpart RRRRR_National Emission Standards for Hazardous Air Pollutants:
Taconite Iron Ore Processing
What This Subpart Covers
63.9580 What is the purpose of this subpart?
63.9581 Am I subject to this subpart?
63.9582 What parts of my plant does this subpart cover?
63.9583 When do I have to comply with this subpart?
[[Page 7]]
Emission Limitations and Work Practice Standards
63.9590 What emission limitations must I meet?
63.9591 What work practice standards must I meet?
Operation and Maintenance Requirements
63.9600 What are my operation and maintenance requirements?
General Compliance Requirements
63.9610 What are my general requirements for complying with this
subpart?
Initial Compliance Requirements
63.9620 On which units and by what date must I conduct performance tests
or other initial compliance demonstrations?
63.9621 What test methods and other procedures must I use to demonstrate
initial compliance with the emission limits for particulate
matter?
63.9622 What test methods and other procedures must I use to establish
and demonstrate initial compliance with the operating limits?
63.9623 How do I demonstrate initial compliance with the emission
limitations that apply to me?
63.9624 How do I demonstrate initial compliance with the work practice
standards that apply to me?
63.9625 How do I demonstrate initial compliance with the operation and
maintenance requirements that apply to me?
Continuous Compliance Requirements
63.9630 When must I conduct subsequent performance tests?
63.9631 What are my monitoring requirements?
63.9632 What are the installation, operation, and maintenance
requirements for my monitoring equipment?
63.9633 How do I monitor and collect data to demonstrate continuous
compliance?
63.9634 How do I demonstrate continuous compliance with the emission
limitations that apply to me?
63.9635 How do I demonstrate continuous compliance with the work
practice standards that apply to me?
63.9636 How do I demonstrate continuous compliance with the operation
and maintenance requirements that apply to me?
63.9637 What other requirements must I meet to demonstrate continuous
compliance?
Notifications, Reports, and Records
63.9640 What notifications must I submit and when?
63.9641 What reports must I submit and when?
63.9642 What records must I keep?
63.9643 In what form and how long must I keep my records?
Other Requirements and Information
63.9650 What parts of the General Provisions apply to me?
63.9651 Who implements and enforces this subpart?
63.9652 What definitions apply to this subpart?
Table 1 to Subpart RRRRR of Part 63--Emission Limits
Table 2 to Subpart RRRRR of Part 63--Applicability of General Provisions
to Subpart RRRRR of Part 63
Subpart SSSSS_National Emission Standards for Hazardous Air Pollutants
for Refractory Products Manufacturing
What This Subpart Covers
63.9780 What is the purpose of this subpart?
63.9782 Am I subject to this subpart?
63.9784 What parts of my plant does this subpart cover?
63.9786 When do I have to comply with this subpart?
Emission Limitations and Work Practice Standards
63.9788 What emission limits, operating limits, and work practice
standards must I meet?
63.9790 What are my options for meeting the emission limits?
General Compliance Requirements
63.9792 What are my general requirements for complying with this
subpart?
63.9794 What do I need to know about operation, maintenance, and
monitoring plans?
Testing and Initial Compliance Requirements
63.9796 By what date must I conduct performance tests?
63.9798 When must I conduct subsequent performance tests?
63.9800 How do I conduct performance tests and establish operating
limits?
63.9802 How do I develop an emissions profile?
63.9804 What are my monitoring system installation, operation, and
maintenance requirements?
63.9806 How do I demonstrate initial compliance with the emission
limits, operating limits, and work practice standards?
Continuous Compliance Requirements
63.9808 How do I monitor and collect data to demonstrate continuous
compliance?
[[Page 8]]
63.9810 How do I demonstrate continuous compliance with the emission
limits, operating limits, and work practice standards?
Notifications, Reports, and Records
63.9812 What notifications must I submit and when?
63.9814 What reports must I submit and when?
63.9816 What records must I keep?
63.9818 In what form and how long must I keep my records?
Other Requirements and Information
63.9820 What parts of the General Provisions apply to me?
63.9822 Who implements and enforces this subpart?
63.9824 What definitions apply to this subpart?
Table 1 to Subpart SSSSS of Part 63--Emission Limits
Table 2 to Subpart SSSSS of Part 63--Operating Limits
Table 3 to Subpart SSSSS of Part 63--Work Practice Standards
Table 4 to Subpart SSSSS to Part 63--Requirements for Performance Tests
Table 5 to Subpart SSSSS of Part 63--Initial Compliance with Emission
Limits
Table 6 to Subpart SSSSS of Part 63--Initial Compliance with Work
Practice Standards
Table 7 to Subpart SSSSS to Part 63--Continuous Compliance with Emission
Limits
Table 8 to Subpart SSSSS of Part 63--Continuous Compliance with
Operating Limits
Table 9 to Subpart SSSSS of Part 63--Continuous Compliance with Work
Practice Standards
Table 10 to Subpart SSSSS of Part 63--Requirements for Reports
Table 11 to Subpart SSSSS of Part 63--Applicability of General
Provisions to Subpart SSSSS
Subpart TTTTT_National Emissions Standards for Hazardous Air Pollutants
for Primary Magnesium Refining
What This Subpart Covers
63.9880 What is the purpose of this subpart?
63.9881 Am I subject to this subpart?
63.9882 What parts of my plant does this subpart cover?
63.9883 When do I have to comply with this subpart?
Emission Limitations and Work Practice Standards
63.9890 What emission limitations must I meet?
63.9891 What work practice standards must I meet for my fugitive dust
sources?
Operation and Maintenance Requirements
63.9900 What are my operation and maintenance requirements?
General Compliance Requirements
63.9910 What are my general requirements for complying with this
subpart?
Initial Compliance Requirements
63.9911 By what date must I conduct performance tests or other initial
compliance demonstrations?
63.9912 When must I conduct subsequent performance tests?
63.9913 What test methods and other procedures must I use to demonstrate
initial compliance with the emission limits for particulate
matter and PM10?
63.9914 What test methods and other procedures must I use to demonstrate
initial compliance with chlorine and hydrochloric acid
emission limits?
63.9915 What test methods and other procedures must I use to demonstrate
initial compliance with dioxin/furan emission limits?
63.9916 What test methods and other procedures must I use to establish
and demonstrate initial compliance with the operating limits?
63.9917 How do I demonstrate initial compliance with the emission
limitations and work practice standards that apply to me?
63.9918 How do I demonstrate initial compliance with the operation and
maintenance requirements that apply to me?
Continuous Compliance Requirements
63.9920 What are my monitoring requirements?
63.9921 What are the installation, operation, and maintenance
requirements for my monitors?
63.9922 How do I monitor and collect data to demonstrate continuous
compliance?
63.9923 How do I demonstrate continuous compliance with the emission
limitations and work practice standards that apply to me?
63.9924 How do I demonstrate continuous compliance with the operation
and maintenance requirements that apply to me?
63.9925 What other requirements must I meet to demonstrate continuous
compliance?
Notifications, Reports, and Records
63.9930 What notifications must I submit and when?
63.9931 What reports must I submit and when?
63.9932 What records must I keep?
[[Page 9]]
63.9933 In what form and how long must I keep my records?
Other Requirements and Information
63.9940 What parts of the General Provisions apply to me?
63.9941 Who implements and enforces this subpart?
63.9942 What definitions apply to this subpart?
Table 1 to Subpart TTTTT of Part 63--Emission Limits
Table 2 to Subpart TTTTT of Part 63--Toxic Equivalency Factors
Table 3 to Subpart TTTTT of Part 63--Initial Compliance with Emission
Limits
Table 4 to Subpart TTTTT of Part 63--Continuous Compliance with Emission
Limits
Table 5 to Subpart TTTTT of Part 63--Applicability of General Provisions
to Subpart TTTTT of Part 63
Appendix A to Part 63--Test Methods
Appendix B to Part 63--Sources Defined for Early Reduction Provisions
Appendix C to Part 63--Determination of the Fraction Biodegraded
(Fbio) in a Biological Treatment Unit
Appendix D to Part 63--Alternative Validation Procedure for EPA Waste
and Wastewater Methods
Appendix E to Part 63--Monitoring Procedure for Nonthoroughly Mixed Open
Biological Treatment Systems at Kraft Pulp Mills Under Unsafe
Sampling Conditions
Authority: 42 U.S.C. 7401 et seq.
Source: 57 FR 61992, Dec. 29, 1992, unless otherwise noted.
Subpart NNNNN_National Emission Standards for Hazardous Air Pollutants:
Hydrochloric Acid Production
Source: 68 FR 19090, Apr. 17, 2003, unless otherwise noted.
What This Subpart Covers
Sec. 63.8980 What is the purpose of this subpart?
This subpart establishes national emission standards for hazardous
air pollutants (NESHAP) and work practice standards for hazardous air
pollutants (HAP) emitted from hydrochloric acid (HCl) production. This
subpart also establishes requirements to demonstrate initial and
continuous compliance with the emission limitations and work practice
standards.
Sec. 63.8985 Am I subject to this subpart?
(a) You are subject to this subpart if you own or operate an HCl
production facility that produces a liquid HCl product at a
concentration of 30 weight percent or greater during its normal
operations and is located at, or is part of, a major source of HAP. This
does not include HCl production facilities that only produce
occasionally liquid HCl product at a concentration of 30 weight percent
or greater.
(1) An HCl production facility is the collection of unit operations
and equipment associated with the production of liquid HCl product. The
HCl production facility begins at the point where a gaseous stream
containing HCl enters the HCl production unit. The HCl production
facility includes all HCl storage tanks that contain liquid HCl product
that is produced in the HCl production unit, with the exceptions noted
in paragraph (a)(2) of this section. The HCl production facility also
includes all HCl transfer operations that load HCl product produced in
the HCl production unit into a tank truck, rail car, ship, or barge,
along with the piping and other equipment in HCl service used to
transfer liquid HCl product from the HCl production unit to the HCl
storage tanks and/or HCl transfer operations. The HCl production
facility ends at the point that the liquid HCl product produced in the
HCl production unit is loaded into a tank truck, rail car, ship, or
barge, at the point the HCl product enters another process on the plant
site, or at the point the HCl product leaves the plant site via
pipeline.
(2) Storage tanks that are dedicated feedstock tanks for another
process and storage tanks that store HCl dedicated for use in wastewater
treatment are not considered part of an HCl production facility.
(3) A major source of HAP emissions is any stationary source or
group of stationary sources within a contiguous area under common
control that emits or has the potential to emit any single HAP at a rate
of 9.07 megagrams (10 tons) or more per year or any combination of HAP
at a rate of 22.68 megagrams (25 tons) or more per year.
[[Page 10]]
(b) An HCl production facility is not subject to this subpart if it
is also subject to NESHAP under one of the subparts listed in paragraphs
(b)(1) through (5) of this section.
(1) 40 CFR part 63, subpart S, National Emission Standards for
Hazardous Air Pollutants from the Pulp and Paper Industry.
(2) 40 CFR part 63, subpart CCC, National Emission Standards for
Hazardous Air Pollutants for Steel Pickling--HCl Process Facilities and
Hydrochloric Acid Regeneration Plants.
(3) 40 CFR part 63, subpart MMM, National Emission Standards for
Hazardous Air Pollutants for Pesticide Active Ingredient Production.
(4) 40 CFR part 63, section 63.994, subpart SS, National Emission
Standards for Closed Vent Systems, Control Devices, Recovery Devices and
Routing to a Fuel Gas System or a Process.
(5) 40 CFR part 63, subpart GGG, National Emission Standards for
Pharmaceuticals Production.
(c) An HCl production facility is not subject to this subpart if it
is located following the incineration of chlorinated waste gas streams,
waste liquids, or solid wastes, and the emissions from the HCl
production facility are subject to section 63.113(c), subpart G,
National Emission Standards for Organic Hazardous Air Pollutants from
the Synthetic Organic Chemical Manufacturing Industry for Process Vents,
Storage Vessels, Transfer Operations, and Wastewater.
(d) An HCl production facility is not subject to this subpart if it
produces HCl through the direct synthesis of hydrogen and chlorine and
is part of a chlor-alkali facility.
(e) An HCl production facility is not subject to this subpart if it
is a research and development facility.
(f) An HCl production facility is not subject to this subpart if all
of the gaseous streams containing HCl and chlorine (Cl2) from
HCl process vents, HCl storage tanks, and HCl transfer operations are
recycled or routed to another process prior to being discharged to the
atmosphere.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
Sec. 63.8990 What parts of my plant does this subpart cover?
(a) This subpart applies to each new, reconstructed, or existing
affected source at an HCl production facility.
(b) The affected source is the group of one or more HCl production
facilities at a plant site that are subject to this subpart, and all
associated wastewater operations, which contain the collection of
emission streams listed in paragraphs (b)(1) through (5) of this
section.
(1) Each emission stream from an HCl process vent.
(2) Each emission stream from an HCl storage tank.
(3) Each emission stream from an HCl transfer operation.
(4) Each emission stream resulting from leaks from equipment in HCl
service.
(5) Each emission stream from HCl wastewater operations. There are
no emission limitations or other requirements in this subpart that apply
to HCl wastewater operations.
(c) An affected source is a new affected source if you commenced
construction of the affected source after September 18, 2001 and you met
the applicability criteria of Sec. 63.8985 at the time you commenced
construction.
(d) An affected source is reconstructed if you meet the criteria as
defined in Sec. 63.2.
(e) An affected source is existing if it is not new or
reconstructed.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
Sec. 63.8995 When do I have to comply with this subpart?
(a) If you have a new or reconstructed affected source, you must
comply with this subpart according to paragraphs (a)(1) or (2) of this
section.
(1) If you start up your affected source before April 17, 2003, you
must comply with the emission limitations and work practice standards in
this subpart no later than April 17, 2003.
(2) If you start up your affected source after April 17, 2003, you
must comply with the emission limitations and work practice standards in
this subpart upon startup of your affected source.
(b) If you have an existing affected source, you must comply with
the
[[Page 11]]
emission limitations and work practice standards no later than 3 years
after April 17, 2003.
(c) If you have an area source that increases its emissions or its
potential to emit such that it becomes a major source of HAP, the
provisions in paragraphs (c)(1) and (2) of this section apply.
(1) Any portion of the existing facility that is a new affected
source or a new reconstructed source must be in compliance with this
subpart upon startup.
(2) All other parts of the source must be in compliance with this
subpart no later than the date 3 years after the area source becomes a
major source.
(d) You must meet the notification requirements in Sec. 63.9045
according to the schedule in Sec. 63.9045 and in subpart A of this
part. Some of the notifications must be submitted before you are
required to comply with the emission limitations in this subpart.
Emission Limitations and Work Practice Standards
Sec. 63.9000 What emission limitations and work practice standards
must I meet?
(a) With the exceptions noted in paragraphs (c) and (d) of this
section, you must meet the applicable emission limit and work practice
standard in table 1 to this subpart for each emission stream listed
under Sec. 63.8990(b)(1) through (4) that is part of your affected
source.
(b) With the exceptions noted in paragraph (c) of this section, you
must meet the applicable operating limit in Table 2 to this subpart for
each emission stream listed under Sec. 63.8990(b)(1) through (3) that
is part of your affected source.
(c) The emission streams listed in paragraphs (c)(1) through (4) of
this section are exempt from the emission limitations, work practice
standards, and all other requirements of this subpart.
(1) Emission streams from HCl storage tanks that never store liquid
HCl product with a concentration of 30 weight percent or greater.
(2) Emission streams from HCl transfer operations that never load
liquid HCl product with a concentration of 30 weight percent or greater.
(3) Emission streams from HCl wastewater operations.
(4) Emission streams from HCl process vents, HCl storage tanks, and
HCl transfer operations that are also subject to 40 CFR part 63, subpart
EEE, National Emission Standards for Hazardous Air Pollutants for
Hazardous Waste Combustors, or 40 CFR 266.107, subpart H, Burning of
Hazardous Waste in Boilers and Industrial Furnaces.
(d) The emission limits for HCl storage tanks in table 1 to this
subpart do not apply during periods of planned routine maintenance of
HCl storage tank control devices. Periods of planned routine maintenance
of each HCl storage tank control device, during which the control device
does not meet the emission limits specified in table 1 to this subpart,
shall not exceed 240 hours per year.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
General Compliance Requirements
Sec. 63.9005 What are my general requirements for complying with this
subpart?
(a) You must be in compliance with the emission limitations and work
practice standards in this subpart at all times, except during periods
of startup, shutdown, and malfunction.
(b) You must always operate and maintain your affected source,
including air pollution control and monitoring equipment, according to
the provisions in Sec. 63.6(e)(1)(i).
(c) You must develop a written startup, shutdown, and malfunction
plan according to the provisions in Sec. 63.6(e)(3).
(d) All monitoring equipment shall be installed, calibrated,
maintained, and operated according to manufacturer's specifications or
other written procedures that provide adequate assurance that the
equipment would reasonably be expected to monitor accurately. For each
monitoring system required in this section, you must develop, implement,
and submit to the Administrator a site-specific monitoring plan that
addresses the installation requirements in paragraphs (d)(1) through (3)
of this section, the ongoing
[[Page 12]]
procedures in paragraphs (d)(4) through (6) of this section, and the
requirements in Sec. 63.9025, as applicable. You must submit the plan
with your Notification of Compliance Status. Upon request of the
Administrator, you must promptly correct any deficiencies in a site-
specific monitoring plan and submit the revised plan.
(1) Installation of the continuous monitoring system (CMS) sampling
probe or other interface at a measurement location relative to each
affected process unit such that the measurement is representative of
control of the exhaust emissions (e.g., on or downstream of the last
control device).
(2) Performance and equipment specifications for the sample
interface, the pollutant concentration or parametric signal analyzer,
and the data collection and reduction system.
(3) Performance evaluation procedures and acceptance criteria (e.g.,
calibrations).
(4) Ongoing operation and maintenance (O&M) procedures in accordance
with the general requirements of Sec. Sec. 63.8(c)(1), (3), (4)(ii),
(7), and (8), and 63.9025.
(5) Ongoing data quality assurance procedures in accordance with the
general requirements of Sec. 63.8(d).
(6) Ongoing recordkeeping and reporting procedures in accordance
with the general requirements of Sec. 63.10(c) and (e)(1) and (2)(i).
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Testing and Initial Compliance Requirements
Sec. 63.9010 By what date must I conduct performance tests?
(a) If you have a new or reconstructed affected source, you must
conduct performance tests within 180 calendar days after the compliance
date that is specified for your source in Sec. 63.8995(a) and according
to the provisions in Sec. 63.7(a)(2).
(b) If you have an existing affected source, you must conduct
performance tests within 180 calendar days after the compliance date
that is specified for your existing affected source in Sec. 63.8995(b)
and according to the provisions in Sec. 63.7(a)(2).
(c) If you commenced construction or reconstruction between
September 18, 2001 and April 17, 2003, you must demonstrate initial
compliance with either the proposed emission limitation or the
promulgated emission limitation no later than 180 calendar days after
April 17, 2003 or within 180 calendar days after startup of the source,
whichever is later, according to Sec. 63.7(a)(2)(ix).
Sec. 63.9015 When must I conduct subsequent performance tests?
(a) You must conduct all applicable performance tests according to
the procedures in Sec. 63.9020 on the earlier of your title V operating
permit renewal or within 5 years of issuance of your title V permit. For
emission points meeting the outlet concentration limits in table 1 to
this subpart without the use of a control device, all applicable
performance tests must also be conducted whenever process changes are
made that could reasonably be expected to increase the outlet
concentration. Examples of process changes include, but are not limited
to, changes in production capacity, production rate, feedstock type, or
catalyst type, or whenever there is replacement, removal, or addition of
recovery equipment. For purposes of this paragraph, process changes do
not include: process upsets and unintentional, temporary process
changes.
(b) You must report the results of subsequent performance tests
within 60 days after the completion of the test. This report should also
verify that the operating limits for your affected source have not
changed or provide documentation of revised operating limits established
as specified in Table 2 to this subpart. The reports for all subsequent
performance tests should include all applicable information required in
Sec. 63.9050.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
Sec. 63.9020 What performance tests and other procedures must I use?
(a) You must conduct each performance test in Table 3 to this
subpart that applies to you as directed in paragraphs (a)(1) through (4)
of this section, except as noted in paragraphs (b) and (c) of this
section.
[[Page 13]]
(1) You must develop a site-specific test plan according to Sec.
63.7(c)(2) and conduct each performance test according to the site-
specific test plan.
(2) You must conduct each performance test under representative
conditions according to the requirements in Sec. 63.7(e)(1) and under
the specific conditions that this subpart specifies in Table 3.
(3) You may not conduct performance tests during periods of startup,
shutdown, or malfunction, as specified in Sec. 63.7(e)(1).
(4) You must conduct at least three separate test runs for each
performance test required in this section, as specified in Sec.
63.7(e)(3). Each test run must last at least 1 hour.
(b) If you are complying with a percent reduction emission
limitation, you must determine the percent reduction in accordance with
paragraphs (b)(1) and (2) of this section.
(1) Calculate the mass rate of either HCl or chlorine using
Equations 1 and 2 of this section:
[GRAPHIC] [TIFF OMITTED] TR17AP03.000
where:
Ci, Co = Concentration of HCl or Cl2 in
the gas stream at the inlet and outlet of the control device(s),
respectively, dry basis, parts per million by volume.
Ei, Eo = Mass rate of HCl or Cl2 at the
inlet and outlet of the control device(s), respectively, dry basis,
kilogram per hour.
Mi, Mo = Molecular weight of HCl or Cl2
at the inlet and outlet of the control device(s), respectively, gram/
gram-mole.
Qi, Qo = Flow rate of gas stream at the inlet and
outlet of the control device(s), respectively, dry standard cubic meter
per minute.
K2 = Constant, 2.494 x 10-6 (parts per million)\-
1\ (gram-mole per standard cubic meter) (kilogram/gram) (minute/hour),
where standard temperature (gram-mole per standard cubic meter) is 20
[deg]C.
(2) Calculate the percent reduction of HCl or Cl2 using
Equation 3 of this section:
[GRAPHIC] [TIFF OMITTED] TR17AP03.001
where:
R = Control efficiency of control device(s).
Ei = Mass rate of HCl or Cl2 to the inlet to the
control device(s), kilograms per hour.
Eo = Mass rate of HCl or Cl2 at the outlet of the
control device(s), kilograms per hour.
(c) You may prepare a design evaluation in lieu of conducting a
performance test for HCl storage tanks and HCl transfer operations that
are not routed to a control device that also controls HCl process vent
emissions or any other continuous vent stream. The design evaluation
shall include documentation demonstrating that the control technique
being used achieves the required control efficiency when a liquid HCl
product with a concentration of 30 weight percent or greater is being
loaded into the storage tank, or a tank truck, rail car, ship, or barge.
(1) If you use a caustic scrubber control device or a water scrubber
control device, the design evaluation shall address the vent stream
composition, constituent concentrations, liquid-to-vapor ratio,
scrubbing liquid flow rate and concentration, temperature, and the
reaction kinetics of the constituents with the scrubbing liquid. The
design evaluation shall establish the design exhaust vent concentration
level and shall include the additional information in paragraphs
(c)(1)(i) and (ii) of this section for trays and a packed column
scrubber.
(i) Type and total number of theoretical and actual trays.
(ii) Type and total surface area of packing for entire column and
for individual packed sections, if the column contains more than one
packed section.
(2) If you use any other control device, the design evaluation shall
address the composition and HAP concentration of the vent stream
immediately preceding the control device, as well as other parameters
necessary to demonstrate that the control technique being used achieves
the required control efficiency when a liquid HCl product with a
concentration of 30 weight percent or greater is being loaded into the
storage tank, or a tank truck, rail car, ship, or barge.
(d) You are not required to conduct a performance test for an
emission point
[[Page 14]]
for which a performance test was conducted within the previous 5-year
period, using the same test methods specified in this section and for
which either no deliberate process changes have been made since the
test, or the owner or operator can demonstrate that the results of the
performance test, with or without adjustments, reliably demonstrate
compliance despite process changes. The operating limits reported under
the previous performance test shall be sufficient to meet the monitoring
requirements in this subpart.
(e) You must establish all operating limits with which you will
demonstrate continuous compliance with the applicable emission limits in
Table 1 to this subpart as described in paragraphs (e)(1) through (3) of
this section.
(1) If you use a caustic scrubber control device or water scrubber
control device and you conduct a performance test, you must establish
operating limits according to paragraphs (e)(1)(i) and (ii) of this
section. If a series of control devices are used, you must establish
separate operating limits for each device.
(i) You must establish the minimum value as the operating limit for
scrubber inlet liquid or recirculating liquid flow rate, as appropriate.
The minimum value shall be based on the scrubber inlet liquid or
recirculating liquid flow rate, as appropriate, values measured during
the performance test.
(ii) You must establish the minimum and maximum values as the
operating limits for scrubber effluent pH. The minimum and maximum
values shall be based on the scrubber effluent pH values measured during
the performance test.
(2) If you use any other control device and you conduct a
performance test, you must establish operating limits according to your
site-specific test plan submitted in accordance with Sec.
63.7(c)(2)(i). The operating limits shall be based on the operating
parameter values measured during the performance test. If a series of
control devices are used, you must establish separate operating limits
for each device.
(3) If you do not conduct a performance test for a HCl storage tank
or HCl transfer operation, you must use engineering assessments and/or
manufacturer's recommendations to establish the operating limits
specified in paragraphs (e)(1)(i) and (ii), or (e)(2), of this section.
(4) As needed in applicability determinations, you must use ASTM
E224 to determine the HCl concentration in liquid products.
Sec. 63.9025 What are my monitoring installation, operation, and
maintenance requirements?
(a) For each operating parameter that you are required by Sec.
63.9020(e) to monitor, you must install, operate, and maintain each CMS
according to the requirements in paragraphs (a)(1) through (6) of this
section.
(1) You must operate your CMS and collect data at all times the
process is operating.
(2) You must collect data from at least four equally spaced periods
each hour.
(3) For at least 75 percent of the operating hours in a 24-hour
period, you must have valid data (as defined in your site-specific
monitoring plan) for at least 4 equally spaced periods each hour.
(4) For each hour that you have valid data from at least four
equally spaced periods, you must calculate the hourly average value
using all valid data or, where data are collected from an automated CMS,
using at least one measured value per minute if measured more frequently
than once per minute.
(5) You must calculate the daily average using all of the hourly
averages calculated according to paragraph (a)(4) of this section for
the 24-hour period.
(6) You must record the results for each inspection, calibration,
and validation check as specified in your site-specific monitoring plan.
(b) For scrubber control devices, you may request approval, in
accordance with Sec. 63.8(f), to monitor parameters other than those
specified in Sec. 63.9020(e). In accordance with Sec. 63.8(f), you
must submit a monitoring plan to the Administrator and the plan must
meet the requirements in paragraphs (a) and (b)(1) through (3) of this
section. You must conduct monitoring in accordance with the plan
submitted to
[[Page 15]]
the Administrator unless comments received from the Administrator
require an alternate monitoring scheme.
(1) Identify the operating parameter to be monitored to ensure that
the control or capture efficiency measured during the initial compliance
test is maintained.
(2) Discuss why this parameter is appropriate for demonstrating
ongoing compliance.
(3) Identify the specific monitoring procedures.
(c) For any other control device, you must ensure that the CMS is
operated according to a monitoring plan submitted to the Administrator
as required by Sec. 63.8(f). The monitoring plan must meet the
requirements in paragraphs (a) and (c)(1) through (3) of this section.
You must conduct monitoring in accordance with the plan submitted to the
Administrator, as amended, unless comments received from the
Administrator require an alternate monitoring scheme.
(1) Identify the operating parameter to be monitored to ensure that
the control or capture efficiency measured during the initial compliance
test is maintained.
(2) Discuss why this parameter is appropriate for demonstrating
ongoing compliance.
(3) Identify the specific monitoring procedures.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
Sec. 63.9030 How do I demonstrate initial compliance with the emission
limitations and work practice standards?
(a) You must demonstrate initial compliance with each emission limit
and work practice standard that applies to you according to Table 4 to
this subpart.
(b) You must establish each site-specific operating limit in Table 2
to this subpart that applies to you according to the requirements in
Sec. 63.9020 and Table 3 to this subpart.
(c) You must submit the Notification of Compliance Status containing
the results of the initial compliance demonstration according to the
requirements in Sec. 63.9045(e).
Continuous Compliance Requirements
Sec. 63.9035 How do I monitor and collect data to demonstrate continuous
compliance?
(a) You must monitor and collect data according to this section.
(b) If you use a caustic scrubber or a water scrubber/absorber to
meet the emission limits in Table 1 to this subpart, you must keep the
records specified in paragraphs (b)(1) and (2) of this section to
support your compliance demonstration.
(1) Records of daily average scrubber inlet liquid or recirculating
liquid flow rate, as appropriate.
(2) Records of the daily average scrubber effluent pH.
(c) If you use any other control device to meet the emission limits
in Table 1 to this subpart, you must keep records of the operating
parameter values identified in your monitoring plan in Sec. 63.9025(c)
to support your compliance demonstration.
(d) Except for monitor malfunctions, associated repairs, and
required quality assurance or control activities (including, as
applicable, calibration checks and required zero and span adjustments),
you must monitor continuously (or collect data at all required
intervals) at all times that the affected source is operating. This
includes periods of startup, shutdown, or malfunction when the affected
source is operating. A monitoring malfunction includes, but is not
limited to, any sudden, infrequent, not reasonably preventable failure
of the monitoring equipment to provide valid data. Monitoring failures
that are caused in part by poor maintenance or careless operation are
not malfunctions.
(e) You may not use data recorded during monitoring malfunctions,
associated repairs, and required quality assurance or control activities
in data averages and calculations used to report emission or operating
levels, nor may such data be used in fulfilling a minimum data
availability requirement, if applicable. You must use all the data
collected during all other periods in assessing the operation of the
control device and associated control system.
[[Page 16]]
Sec. 63.9040 How do I demonstrate continuous compliance with the
emission limitations and work practice standards?
(a) You must demonstrate continuous compliance with each emission
limit and work practice standard in Table 1 to this subpart that applies
to you according to Table 4 to this subpart.
(b) You must demonstrate continuous compliance with each operating
limit in Table 2 of this subpart that applies to you according to Tables
4 and 5 to this subpart.
(c) You must report each instance in which you did not meet an
emission limit, work practice standard or operating limit in Table 1 or
2 to this subpart, respectively, that applies to you. This includes
periods of startup, shutdown, and malfunction. These instances are
deviations from the emission limitations in this subpart. These
deviations must be reported according to the requirements in Sec.
63.9050.
(d) [Reserved]
(e) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations
that occur during a period of startup, shutdown, or malfunction are not
violations if you demonstrate to the Administrator's satisfaction that
you were operating in accordance with Sec. 63.6(e)(1). The
Administrator will determine whether deviations that occur during a
period of startup, shutdown, or malfunction are violations, according to
the provisions in Sec. 63.6(e).
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Notifications, Reports, and Records
Sec. 63.9045 What notifications must I submit and when?
(a) You must submit all of the notifications in Sec. Sec. 63.7(b)
and (c), 63.8(f)(4) and (6), and 63.9 (b) through (h) that apply to you
by the dates specified.
(b) As specified in Sec. 63.9(b)(2), if you start up your affected
source before April 17, 2003, you must submit an Initial Notification
not later than 120 calendar days after April 17, 2003.
(c) As specified in Sec. 63.9(b)(4), if you start up your new or
reconstructed affected source on or after April 17, 2003, you must
submit the application for construction or reconstruction required by
Sec. 63.9(b)(1)(iii) in lieu of the initial notification.
(d) You must submit a notification of intent to conduct a
performance test at least 60 calendar days before the performance test
is scheduled to begin, as required in Sec. 63.7(b)(1).
(e) [Reserved]
(f) You must submit the Notification of Compliance Status, including
the performance test results, within 240 calendar days after the
applicable compliance dates specified in Sec. 63.8995.
(g) The Notification of Compliance Status must also include the
information in paragraphs (g)(1) through (2) of this section that
applies to you.
(1) Each operating parameter value averaged over the full period of
the performance test (for example, average pH).
(2) Each operating parameter range within which HAP emissions are
reduced to the level corresponding to meeting the applicable emission
limits in Table 1 to this subpart.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
Sec. 63.9050 What reports must I submit and when?
(a) You must submit each report in Table 6 to this subpart that
applies to you.
(b) Unless the Administrator has approved a different schedule for
submission of reports under Sec. 63.10(a), you must submit each report
according to paragraphs (b)(1) through (5) of this section.
(1) The first compliance report must cover the period beginning on
the compliance date that is specified for your affected source in Sec.
63.8995 and ending on June 30 or December 31, whichever date is the
first date following the end of the first calendar half after the
compliance date that is specified for your source in Sec. 63.8995
(i.e., June 30, 2006, for sources existing on April 17, 2006).
(2) The first compliance report must be postmarked or delivered no
later than July 31 or January 31, whichever date follows the end of the
first calendar half after the compliance date that is specified for your
affected source in Sec. 63.8995 (i.e., July 31, 2006, for sources
existing on April 17, 2006).
[[Page 17]]
(3) Each subsequent compliance report must cover the semiannual
reporting period from January 1 through June 30 or the semiannual
reporting period from July 1 through December 31.
(4) Each subsequent compliance report must be postmarked or
delivered no later than July 31 or January 31, whichever date is the
first date following the end of the semiannual reporting period.
(5) For each affected source that is subject to permitting
regulations pursuant to 40 CFR part 70 or 71, and if the permitting
authority has established dates for submitting semiannual reports
pursuant to 40 CFR 70.6 (a)(3)(iii)(A) or 71.6 (a)(3)(iii)(A), you may
submit the first and subsequent compliance reports according to the
dates the permitting authority has established instead of according to
the dates in paragraphs (b)(1) through (4) of this section.
(c) The compliance report must contain the following information in
paragraphs (c)(1) through (10) of this section.
(1) Company name and address.
(2) Statement by a responsible official with that official's name,
title, and signature, certifying the truth, accuracy, and completeness
of the content of the report.
(3) Date of report and beginning and ending dates of the reporting
period.
(4) If you had a startup, shutdown, or malfunction during the
reporting period and you took actions consistent with your startup,
shutdown, and malfunction plan, the compliance report must include the
information in Sec. 63.10(d)(5)(i).
(5) If there are no deviations from any emission limitations that
apply to you, a statement that there were no deviations from the
emission limitations during the reporting period.
(6) If there were no periods during which the CMS was out-of-control
in accordance with the monitoring plan, a statement that there were no
periods during which the CMS was out-of-control during the reporting
period.
(7) Verification that you continue to use the equipment LDAR plan
and information that explains any periods when the procedures in the
plan were not followed and the corrective actions were not taken.
(8) If you did not make revisions to your site-specific monitoring
plan and/or LDAR plan during the reporting period, a statement that you
did not make any revisions to your site-specific monitoring plan and/or
LDAR plan during the reporting period. If you made revisions to your
site-specific monitoring plan and/or LDAR plan during the reporting
period, a copy of the revised plan.
(9) If you meet the outlet concentration limit in table 1 to this
subpart without the use of a control device for any emission point,
verification that you have not made any process changes that could
reasonably be expected to increase the outlet concentration since your
most recent performance test for that emission point.
(10) The information specified in paragraphs (c)(10)(i) and (ii) of
this section for those planned routine maintenance operations that
caused or may cause an HCl storage tank control device not to meet the
emission limits in table 1 to this subpart, as applicable.
(i) A description of the planned routine maintenance that was
performed for each HCl storage tank control device during the reporting
period. This description shall include the type of maintenance performed
and the total number of hours during the reporting period that the HCl
storage tank control device did not meet the emission limits in table 1
to this subpart, as applicable, due to planned routine maintenance.
(ii) A description of the planned routine maintenance that is
anticipated to be performed for each HCl storage tank control device
during the next reporting period. This description shall include the
type of maintenance necessary, planned frequency of maintenance, and
lengths of maintenance periods.
(d) For each deviation from an emission limitation occurring at an
affected source where you are using a CMS to comply with the emission
limitation in this subpart, you must include the information in
paragraphs (c)(1) through (6) of this section and the following
information in paragraphs (d)(1) through (9) of this section. This
[[Page 18]]
includes periods of startup, shutdown, and malfunction.
(1) The date and time that each malfunction started and stopped.
(2) The date and time that each CMS was inoperative, except for zero
(low-level) and high-level checks.
(3) The date, time, and duration that each CMS was out-of-control,
including the information in Sec. 63.8(c)(8).
(4) The date and time that each deviation started and stopped, and
whether each deviation occurred during a period of startup, shutdown, or
malfunction or during another period.
(5) A summary of the total duration of the deviation during the
reporting period and the total duration as a percent of the total source
operating time during that reporting period.
(6) A breakdown of the total duration of the deviations during the
reporting period into those that are due to startup, shutdown, control
equipment problems, process problems, other known causes, and other
unknown causes.
(7) A summary of the total duration of CMS downtime during the
reporting period, and the total duration of CMS downtime as a percent of
the total source operating time during that reporting period.
(8) A brief description of the process units.
(9) A description of any changes in CMS, processes, or controls
since the last reporting period.
(e) Each affected source that has obtained a title V operating
permit pursuant to 40 CFR part 70 or 71 must report all deviations as
defined in this subpart in the semiannual monitoring report required by
40 CFR 70.6(a)(3)(iii)(A) or 71.6(a)(3)(iii)(A). If an affected source
submits a compliance report pursuant to Table 6 to this subpart along
with, or as part of, the semiannual monitoring report required by 40 CFR
70.6(a)(3)(iii)(A) or 71.6(a)(3)(iii)(A), and the compliance report
includes all required information concerning deviations from any
emission limitation in this subpart, submission of the compliance report
shall be deemed to satisfy any obligation to report the same deviations
in the semiannual monitoring report. However, submission of a compliance
report shall not otherwise affect any obligation the affected source may
have to report deviations from permit requirements to the permit
authority.
(f) For each startup, shutdown, or malfunction during the reporting
period that is not consistent with your startup, shutdown, and
malfunction plan you must submit an immediate startup, shutdown and
malfunction report. Unless the Administrator has approved a different
schedule for submission of reports under Sec. 63.10(a), you must submit
each report according to paragraphs (f)(1) and (2) of this section.
(1) An initial report containing a description of the actions taken
for the event must be submitted by fax or telephone within 2 working
days after starting actions inconsistent with the plan.
(2) A follow-up report containing the information listed in Sec.
63.10(d)(5)(ii) must be submitted within 7 working days after the end of
the event unless you have made alternative reporting arrangements with
the permitting authority.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17745, Apr. 7, 2006]
Sec. 63.9055 What records must I keep?
(a) You must keep a copy of each notification and report that you
submitted to comply with this subpart, including all documentation
supporting any Initial Notification or Notification of Compliance Status
that you submitted, as required in Sec. 63.10(b)(2)(xiv).
(b) You must also keep the following records specified in paragraphs
(b)(1) through (5) of this section.
(1) The records in Sec. 63.6(e)(3)(iii) through (v) related to
startup, shutdown, and malfunction.
(2) Records of performance tests as required in Sec.
63.10(b)(2)(viii).
(3) Records of operating parameter values that are consistent with
your monitoring plan.
(4) Records of the date and time that each deviation started and
stopped and whether the deviation occurred during a period of startup,
shutdown, or malfunction or during another period.
(5) Copies of the current versions of the site-specific monitoring
plan and the equipment LDAR plan. You also must submit copies of these
plans and
[[Page 19]]
any revisions or updates to the Administrator for comment only (not for
approval).
(6) Records of the planned routine maintenance performed on each HCl
storage tank control device including the duration of each time the
control device does not meet the emission limits in table 1 to this
subpart, as applicable, due to planned routine maintenance. Such a
record shall include the information specified in paragraphs (b)(6)(i)
and (ii) of this section.
(i) The first time of day and date the emission limits in table 1 to
this subpart, as applicable, were not met at the beginning of the
planned routine maintenance, and
(ii) The first time of day and date the emission limits in table 1
to this subpart, as applicable, were met at the conclusion of the
planned routine maintenance.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17746, Apr. 7, 2006]
Sec. 63.9060 In what form and how long must I keep my records?
(a) Your records must be in a form suitable and readily available
for expeditious inspection and review, according to Sec. 63.10(b)(1).
(b) As specified in Sec. 63.10(b)(1), you must keep each record for
5 years following the date of each occurrence, measurement, maintenance,
corrective action, report, or record.
(c) You must keep each record on site, or readily accessible from on
site through a computer or other means, for at least 2 years after the
date of each occurrence, measurement, maintenance, corrective action,
report, or record, according to Sec. 63.10(b)(1). You can keep the
records off site for the remaining 3 years. Records may be maintained in
hard copy or computer-readable format including, but not limited to, on
paper, microfilm, hard disk drive, floppy disk, compact disk, magnetic
tape, or microfiche.
(d) You must keep each previous (i.e., superseded) version of the
site-specific monitoring plan and the LDAR plan for a period of 5 years
after revision of the plan. If, at any time after adoption of a site-
specific monitoring plan or an LDAR plan, your affected source ceases
operation or is otherwise no longer subject to the provisions of this
subpart, you must retain a copy of the most recent plan for 5 years from
the date your source ceases operation or is no longer subject to this
subpart.
Other Requirements and Information
Sec. 63.9065 What parts of the General Provisions apply to me?
(a) Table 7 to this subpart shows which parts of the General
Provisions in Sec. Sec. 63.1 through 63.15 apply to you.
Sec. 63.9070 Who implements and enforces this subpart?
(a) This subpart can be implemented and enforced by us, the U.S.
EPA, or a delegated authority such as your State, local, or tribal
agency. If the U.S. EPA Administrator has delegated authority to your
State, local, or tribal agency, then that agency, as well as U.S. EPA,
has the authority to implement and enforce this subpart. You should
contact your U.S. EPA Regional Office to find out if this subpart is
delegated to your State, local, or tribal agency.
(b) In delegating implementation and enforcement authority of this
subpart to a State, local, or tribal agency under section 40 CFR part
63, subpart E, the authorities contained in paragraph (c) of this
section are retained by the Administrator of U.S. EPA and are not
transferred to the State, local, or tribal agency.
(c) The authorities in paragraphs (c)(1) through (4) of this section
that cannot be delegated to State, local, or tribal agencies are as
follows.
(1) Approval of alternatives to requirements in Sec. Sec. 63.8980,
63.8985, 63.8990, 63.8995, and 63.9000.
(2) Approval of major changes to test methods under Sec.
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
(3) Approval of major changes to monitoring under Sec. 63.8(f) and
as defined in Sec. 63.90.
(4) Approval of major changes to recordkeeping and reporting under
Sec. 63.10(f) and as defined in Sec. 63.90.
[[Page 20]]
Sec. 63.9075 What definitions apply to this subpart?
Terms used in this subpart are defined in the Clean Air Act in 40
CFR 63.2 and in this section as follows:
Caustic scrubber control device means any add-on device that mixes
an aqueous stream or slurry containing a caustic substance with the
exhaust gases from an HCl process vent, HCl storage tank, or HCl
transfer operation to control emissions of HCl and/or Cl2.
Chlor-alkali facility means a facility where chlorine and sodium or
potassium hydroxide are produced as co-products and hydrogen is produced
as a by-product in an electrolytic process using either mercury cells,
diaphragm cells, or membrane cells.
Continuous monitoring system, for purposes of the final rule, means
liquid flow monitoring devices that meet the performance specifications
given in Sec. 63.9025(a); or pH monitoring devices that meet the
performance specifications given in Sec. 63.9025(a); or other control
devices as mentioned in 63.9025(a) and (b) or Sec. 63.9025(a) and (c).
Control device means an add-on device used to reduce HCl and/or
Cl2 emissions from an HCl process vent, HCl storage tank, or
HCl transfer operation at an HCl production facility. An HCl production
unit is not a control device.
Deviation means any instance in which an affected source subject to
this subpart, or an owner or operator of such a source:
(1) Fails to meet any requirement or obligation established by this
subpart, including but not limited to any emission limitation or work
practice standard;
(2) Fails to meet any term or condition that is adopted to implement
an applicable requirement in this subpart and that is included in the
operating permit for any affected source required to obtain such a
permit; or
(3) Fails to meet any emission limitation or work practice standard
in this subpart during startup, shutdown, or malfunction, regardless of
whether or not such failure is permitted by this subpart.
Emission limitation means any emission limit or operating limit.
Emission stream means a gaseous stream from an HCl process vent, an
HCl storage tank, an HCl transfer operation, leaking equipment in HCl
service, or HCl wastewater operations that is discharged to the
atmosphere. Gaseous streams from HCl process vents, HCl storage tanks,
and HCl transfer operations that are routed to another process or
recycled for reaction or other use (i.e., for pH control) of the HCl
and/or Cl2 are not emission streams. Gaseous streams from HCl
transfer operations that are vapor balanced to an HCl storage tank
subject to this subpart are not emission streams.
Equipment in HCl service means each pump, compressor, agitator,
pressure relief device, sampling connection system, open-ended valve or
line, valve, connector, and instrumentation system in an HCl production
facility that contains 30 weight percent or greater of liquid HCl or 5
weight percent or greater of gaseous HCl at any time.
HCl process vent means the point of discharge to the atmosphere, or
point of entry into a control device, of a gaseous stream that
originates from an HCl production unit. The following points of
discharge are not HCl process vents:
(1) A leak from equipment in HCl service subject to this subpart.
(2) An exit from a control device used to comply with this subpart.
(3) An HCl storage tank vent or HCl transfer operation vent subject
to this subpart.
(4) A HCl wastewater operation vent subject to this subpart.
(5) A point of discharge from a relief valve.
(6) A point of discharge from an analyzer.
HCl production facility is defined in Sec. 63.8985(a)(1).
HCl production unit means an absorber or other vessel in which a
liquid HCl product is manufactured by absorbing gaseous HCl into either
water or an aqueous HCl solution.
HCl storage tank means a tank or other vessel that is used to store
liquid HCl product. Tanks or vessels permanently attached to motor
vehicles (such as trucks, railcars, barges, or ships) are not HCl
storage tanks.
HCl transfer operation means the loading, into a tank truck,
railcar, ship, or
[[Page 21]]
barge, of liquid HCl from a transfer (or loading) rack (as defined in
this section) for which the predominant use is liquid HCl. The
predominant use of a transfer (or loading) rack is the material that is
loaded by the transfer (or loading) rack in the greatest amount.
HCl wastewater operation means an operation that handles and
processes water containing HCl that is discarded from an HCl production
facility.
Plant site means all contiguous or adjoining property that is under
common control, including properties that are separated only by a road
or other public right-of-way. Common control includes properties that
are owned, leased, or operated by the same entity, parent entity,
subsidiary, or any combination thereof.
Research and development facility means laboratory and pilot plant
operations whose primary purpose is to conduct research and development
into new processes and products, where the operations are under close
supervision of technically trained personnel, and the operations are not
engaged in the manufacture of products for commercial sale, except in a
de minimis manner.
Responsible official means responsible official as defined in 40 CFR
70.2 of this chapter.
Transfer (or loading) rack means the collection of loading arms and
loading hoses, at a single loading rack, that are used to fill tank
trucks, railcars, ships, and/or barges. Transfer rack includes the
associated pumps, meters, shutoff valves, relief valves, and other
piping and valves.
Vapor balanced means connected to a piping system that is designed
to collect vapors displaced from tank trucks, rail cars, ships, or
barges during loading, and to route the collected vapors to the storage
vessel from which the liquid being loaded originated, or to another
storage vessel connected by a common header.
Vent means the point of discharge to the atmosphere or to a control
device from either an HCl process vent, an HCl storage tank, or an HCl
transfer operation.
Water scrubber control device means any add-on device that mixes an
aqueous stream not containing a caustic substance with the exhaust gases
from an HCl process vent, HCl storage tank, or HCl transfer operation to
control emissions of HCl and/or Cl2.
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17746, Apr. 7, 2006]
Table 1 to Subpart NNNNN of Part 63--Emission Limits and Work Practice
Standards
As stated in Sec. 63.9000(a), you must comply with the following
emission limits and work practice standards for each emission stream
that is part of an affected source.
------------------------------------------------------------------------
You must meet the following
For each . . . emission limit and work practice
standard
------------------------------------------------------------------------
1. Emission stream from an HCl a. Reduce HCl emissions by 99
process vent at an existing source. percent or greater or achieve an
outlet concentration of 20 ppm by
volume or less; and
b. Reduce Cl2 emissions by 99
percent or greater or achieve an
outlet concentration of 100 ppm by
volume or less.
2. Emission stream from an HCl Reduce HCl emissions by 99 percent
storge tank at an existing source. or greater or achieve an outlet
concentration of 120 ppm by volume
or less.
3. Emission stream from an HCl Reduce HCl emissions by 99 percent
transfer operation at an existing or greater or achieve an outlet
source. concentration of 120 ppm by volume
or less.
4. Emission stream from leaking a. Prepare and operate at all times
equipment in HCl service at according to an equipment LDAR
existing and new sources. plan that describes in detail the
measures that will be put in place
to detect leaks and repair them in
a timely fashion; and
b. Submit the plan to the
Administrator for comment only
with your Notification of
Compliance Status; and
c. You may incorporate by reference
in such plan existing manuals that
describe the measures in place to
control leaking equipment
emissions required as part of
other federally enforceable
requirements, provided that all
manuals that are incorporated by
reference are submitted to the
Administrator.
[[Page 22]]
5. Emission stream from an HCl a. Reduce HCl emissions by 99.4
process vent at a new source. percent or greater or achieve an
outlet concentration of 12 ppm by
volume or less; and
b. Reduce Cl2 emissions by 99.8
percent or greater or achieve an
outlet concentration of 20 ppm by
volume or less.
6. Emission stream from an HCl Reduce HCl emissions by 99.9
storage tank at a new source. percent or greater or achieve an
outlet concentration of 12 ppm by
volume or less.
7. Emission stream from an HCl Reduce HCl emissions by 99 percent
transfer operation at a new source. or greater or achieve an outlet
concentration of 120 ppm by volume
or less.
------------------------------------------------------------------------
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17746, Apr. 7, 2006]
Table 2 to Subpart NNNNN of Part 63--Operating Limits
As stated in Sec. 63.9000(b), you must comply with the following
operating limits for each emission stream that is part of an affected
source that is vented to a control device.
------------------------------------------------------------------------
For each . . . You must . . .
------------------------------------------------------------------------
1. Caustic scrubber or water scrubber/ a. Maintain the daily average
absorber. scrubber inlet liquid or
recirculating liquid flow
rate, as appropriate, above
the operating limit; and
b. Maintain the daily average
scrubber effluent pH within
the operating limits; or
c. Instead of a. and b.,
maintain your operating
parameter(s) within the
operating limits established
according to your monitoring
plan established under Sec.
63.8(f).
------------------------------------------------------------------------
2. Other type of control device to Maintain your operating
which HCl emissions are ducted. parameter(s) within the limits
established during the
performance test and according
to your monitoring plan.
------------------------------------------------------------------------
Table 3 to Subpart NNNNN of Part 63--Performance Test Requirements for
HCl Production Affected Sources
As stated in Sec. 63.9020, you must comply with the following
requirements for performance tests for HCl production for each affected
source.
------------------------------------------------------------------------
For each HCl process vent and
each HCl storage tank and HCl
transfer operation for which Additional
you are conducting a Using . . . Information . . .
performance test, you must . .
.
------------------------------------------------------------------------
1. Select sampling port a. Method 1 or 1A i. If complying with
location(s) and the number of in appendix A to a percent reduction
traverse points. 40 CFR part 60 emission limitation,
of this chapter. sampling sites must
located at the inlet
and outlet of the
control device prior
to any releases to
the atmosphere (or,
if a series of
control devices are
used, at the inlet
of the first control
device and at the
outlet of the final
control device prior
to any releases to
the atmosphere); or
ii. If complying with
an outlet
concentration
emission limitation,
the sampling site
must be located at
the outlet of the
final control device
and prior to any
releases to the
atmosphere or, if no
control device is
used, prior to any
releases to the
atmosphere.
2. Determine velocity and Method 2, 2A, 2C,
volumetric flow rate. 2D, 2F, or 2G in
appendix A to 40
CFR part 60 of
this chapter.
3. Determine gas molecular a. Not applicable i. Assume a molecular
weight. weight of 29 (after
moisture correction)
for calculation
purposes.
4. Measure moisture content of Method 4 in
the stack gas. appendix A to 40
CFR part 60 of
this chapter.
[[Page 23]]
5. Measure HCl concentration a. Method 26A in i. An owner or
and Cl2 concentration from appendix A to 40 operator may be
HCl process vents. CFR part 60 of exempted from
this chapter. measuring the Cl2
concentration from
an HCl process vent
provided that a
demonstration that
Cl2 is not likely to
be present in the
stream is submitted
as part of the site-
specific test plan
required by Sec.
63.9020(a)(2). This
demonstration may be
based on process
knowledge,
engineering
judgment, or
previous test
results.
6. Establish operating limits
with which you will
demonstrate continuous
compliance with the emission
limits in Table 1 to this
subpart, in accordance with
Sec. 63.9020(e)(1) or (2).
------------------------------------------------------------------------
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17747, Apr. 7, 2006]
Table 4 to Subpart NNNNN of Part 63--Initial Compliance With Emission
Limitations and Work Practice Standards
As stated in Sec. 63.9030, you must comply with the following
requirements to demonstrate initial compliance with the applicable
emission limits for each affected source vented to a control device and
each work practice standard.
------------------------------------------------------------------------
For the following
emission limit or You have
For each . . . work practice demonstrated initial
standard . . . compliance if . . .
------------------------------------------------------------------------
1. HCl process vent and each a. In Table 1 to i. The average
HCl storage tank and HCl this subpart. percent reduction
transfer operation for of HCl and Cl2 (if
which you are conducting a applicable),
performance test. measured over the
period of the
performance test
conducted according
to Table 3 of this
subpart and
determined in
accordance with
Sec. 63.9020(b),
is greater than or
equal to the
applicable percent
reduction emission
limitation
specified in Table
1 of this subpart;
or
ii. The average HCl
and Cl2 (if
applicable)
concentration,
measured over the
period of the
performance test
conducted according
to Table 3 of this
subpart, is less
than or equal to
the applicable
concentration
emission limitation
specified in Table
1 of this subpart.
------------------------------------------------------------------------
2. HCl storage tank and HCl a. In Table 1 to i. The percent
transfer operation for this subpart. reduction of HCl,
which you are preparing a demonstrated by a
design evaluation in lieu design evaluation
of conducting a performance prepared in
test. accordance with
Sec. 63.9020(c),
is greater than or
equal to the
applicable percent
reduction emission
limitation
specified in Table
1 of this subpart;
or
ii. The HCl
concentration,
demonstrated by a
design evaluation
prepared in
accordance with
Sec. 63.9020(c),
is less than or
equal to the
applicable
concentration
emission limitation
specified in Table
1 of this subpart.
------------------------------------------------------------------------
3. Leaking equipment........ a. In Table 1 to i. You certify in
this subpart. your Notification
of Compliance
Status that you
have developed and
implemented your
LDAR plan and
submitted it to the
Administrator for
comment only.
------------------------------------------------------------------------
[[Page 24]]
Table 5 to Subpart NNNNN of Part 63--Continuous Compliance With Emission
Limitations and Work Practice Standards
As stated in Sec. 63.9040, you must comply with the following
requirements to demonstrate continuous compliance with the applicable
emission limitations for each affected source vented to a control device
and each work practice standard.
------------------------------------------------------------------------
For the following
emission
limitation and You must demonstrate
For each . . . work practice continuous compliance
standard . . . by . . .
------------------------------------------------------------------------
1. Affected source using a a. In Tables 1 i. Collecting the
caustic scrubber or water and 2 to this scrubber inlet
scrubber/adsorber. subpart. liquid or
recirculating liquid
flow rate, as
appropriate, and
effluent pH
monitoring data
according to Sec.
63.9025, consistent
with your monitoring
plan; and
ii. Reducing the data
to 1-hour and daily
block averages
according to the
requirements in Sec.
63.9025; and
iii. Maintaining the
daily average
scrubber inlet
liquid or
recirculating liquid
flow rate, as
appropriate, above
the operating limit;
and
iv. Maintaining the
daily average
scrubber effluent pH
within the operating
limits.
2. Affected source using any a. In Tables 1 i. Conducting
other control device. and 2 to this monitoring according
subpart. to your monitoring
plan established
under Sec. 63.8(f)
in accordance with
Sec. 63.9025(c);
and
ii. Collecting the
parameter data
according to your
monitoring plan
established under
Sec. 63.8(f); and
iii. Reducing the
data to 1-hour and
daily block averages
according to the
requirements in Sec.
63.9025; and
iv. Maintaining the
daily average
parameter values
within the operating
limits established
according to your
monitoring plan
established under
Sec. 63.8(f).
3. Affected source using no a. In Tables 1 i. Verifying that you
control device. and 2 to this have not made any
subpart.. process changes that
could reasonably be
expected to change
the outlet
concentration since
your most recent
performance test for
an emission point.
4. Leaking equipment affected a. In Table 1 to i. Verifying that you
source. this subpart. continue to use a
LDAR plan; and
ii. Reporting any
instances where you
deviated from the
plan and the
corrective actions
taken.
------------------------------------------------------------------------
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17747, Apr. 7, 2006]
Table 6 to Subpart NNNNN of Part 63--Requirements for Reports
As stated in Sec. 63.9050(a), you must submit a compliance report
that includes the information in Sec. 63.9050(c) through (e) as well as
the information in the following table. You must also submit startup,
shutdown, and malfunction (SSM) reports according to the requirements in
Sec. 63.9050(f) and the following:
------------------------------------------------------------------------
Then you must submit a report
If... or statement that:
------------------------------------------------------------------------
1. There are no deviations from any There were no deviations from
emission limitations that apply to you. any emission limitations that
apply to you during the
reporting period.
------------------------------------------------------------------------
2. There were no periods during which There were no periods during
the operating parameter monitoring which the CMS were out-of-
systems were out-of-control in control during the reporting
accordance with the monitoring plan. period.
------------------------------------------------------------------------
3. There was a deviation from any Contains the information in
emission limitation during the Sec. 63.9050(d).
reporting period.
------------------------------------------------------------------------
4. There were periods during which the Contains the information in
operating parameter monitoring systems Sec. 63.9050(d).
were out-of-control in accordance with
the monitoring plan.
------------------------------------------------------------------------
[[Page 25]]
5. There was a SSM during the reporting Contains the information in
period that is not consistent with Sec. 63.9050(f).
your SSM plan.
------------------------------------------------------------------------
6. There were periods when the Contains the information in
procedures in the LDAR plan were not Sec. 63.9050(c)(7).
followed.
------------------------------------------------------------------------
Table 7 to Subpart NNNNN of Part 63--Applicability of General Provisions
to Subpart NNNNN
As stated in Sec. 63.9065, you must comply with the applicable
General Provisions requirements according to the following:
------------------------------------------------------------------------
Applies to
Citation Requirement subpart NNNNN Explanation
------------------------------------------------------------------------
Sec. 63.1...... Initial applicability Yes.
determination;
applicability after
standard
established; permit
requirements;
extensions;
notifications.
Sec. 63.2...... Definitions.......... Yes.......... Additional
definitions
are found in
Sec.
63.9075.
Sec. 63.3...... Units and Yes.
abbreviations.
Sec. 63.4...... Prohibited Yes.
activities;
compliance date;
circumvention,
severability.
Sec. 63.5...... Construction/ Yes.
reconstruction
applicability;
applications;
approvals.
Sec. 63.6(a)... Compliance with Yes.
standards and
maintenance
requirements-
applicability.
Sec. 63.6(b)(1)- Compliance dates for Yes.......... Sec. 63.8995
(4). new or reconstructed specifies
sources. compliance
dates.
Sec. 63.6(b)(5) Notification if Yes.
commenced
construction or
reconstruction after
proposal.
Sec. 63.6(b)(6) [Reserved]........... Yes.
Sec. 63.6(b)(7) Compliance dates for Yes.......... Sec. 63.8995
new or reconstructed specifies
area sources that compliance
become major. dates.
Sec. 63.6(c)(1)- Compliance dates for Yes.......... Sec. 63.8995
(2). existing sources. specifies
compliance
dates.
Sec. 63.6(c)(3)- [Reserved]........... Yes.
(4).
Sec. 63.6(c)(5) Compliance dates for Yes.......... Sec. 63.8995
existing area specifies
sources that become compliance
major. dates.
Sec. 63.6(d)... [Reserved]........... Yes.
Sec. 63.6(e)(1)- Operation and Yes.
(2). maintenance
requirements.
Sec. 63.6(e)(3) SSM plans............ Yes.
Sec. 63.6(f)(1) Compliance except Yes.
during SSM.
Sec. 63.6(f)(2)- Methods for Yes.
(3). determining
compliance.
Sec. 63.6(g)... Use of an alternative Yes.
non-opacity emission
standard.
Sec. 63.6(h)... Compliance with No........... Subpart NNNNN
opacity/visible does not
emission standards. specify
opacity or
visible
emission
standards.
Sec. 63.6(i)... Extension of Yes.
compliance with
emission standards.
Sec. 63.6(j)... Presidential Yes.
compliance exemption.
Sec. 63.7(a)(1)- Performance test Yes.......... Except for
(2). dates. existing
affected
sources as
specified in
Sec.
63.9010(b).
Sec. 63.7(a)(3) Administrator's Clean Yes.
Air Act section 114
authority to require
a performance test.
Sec. 63.7(b)... Notification of Yes.
performance test and
rescheduling.
Sec. 63.7(c)... Quality assurance Yes.
program and site-
specific test plans.
Sec. 63.7(d)... Performance testing Yes.
facilities.
Sec. 63.7(e)(1) Conditions for Yes.
conducting
performance tests.
Sec. 63.7(f)... Use of an alternative Yes.
test method.
Sec. 63.7(g)... Performance test data Yes.
analysis,
recordkeeping, and
reporting.
Sec. 63.7(h)... Waiver of performance Yes.
tests.
Sec. 63.8(a)(1)- Applicability of Yes.......... Additional
(3). monitoring monitoring
requirements. requirements
are found in
Sec.
63.9005(d) and
63.9035.
63.8(a)(4)....... Monitoring with No........... Subpart NNNNN
flares. does not refer
directly or
indirectly to
Sec. 63.11.
Sec. 63.8(b)... Conduct of monitoring Yes.
and procedures when
there are multiple
effluents and
multiple monitoring
systems.
Sec. 63.8(c)(1)- Continuous monitoring Yes.......... Applies as
(3). system O&M. modified by
Sec.
63.9005(d).
[[Page 26]]
Sec. 63.8(c)(4) Continuous monitoring Yes.......... Applies as
system requirements modified by
during breakdown, Sec.
out-of-control, 63.9005(d).
repair, maintenance,
and high-level
calibration drifts.
Sec. 63.8(c)(5) Continuous opacity No........... Subpart NNNNN
monitoring system does not have
(COMS) minimum opacity or
procedures. visible
emission
standards.
Sec. 63.8(c)(6) Zero and high level Yes.......... Applies as
calibration checks. modified by
Sec.
63.9005(d).
Sec. 63.8(c)(7)- Out-of-control Yes.
(8). periods, including
reporting.
Sec. 63.8(d)- Quality control No........... Applies as
(e). program and CMS modified by
performance Sec.
evaluation. 63.9005(d).
Sec. 63.8(f)(1)- Use of an alternative Yes.
(5). monitoring method.
Sec. 63.8(f)(6) Alternative to No........... Only applies to
relative accuracy sources that
test. use continuous
emissions
monitoring
systems
(CEMS).
Sec. 63.8(g)... Data reduction....... Yes.......... Applies as
modified by
Sec.
63.9005(d).
Sec. 63.9(a)... Notification Yes.
requirements--applic
ability.
Sec. 63.9(b)... Initial notifications Yes.......... Except Sec.
63.9045(c)
requires new
or
reconstructed
affected
sources to
submit the
application
for
construction
or
reconstruction
required by
Sec.
63.9(b)(1)(iii
) in lieu of
the initial
notification.
Sec. 63.9(c)... Request for Yes.
compliance extension.
Sec. 63.9(d)... Notification that a Yes.
new source is
subject to special
compliance
requirements.
Sec. 63.9(e)... Notification of Yes.
performance test.
Sec. 63.9(f)... Notification of No........... Subpart NNNNN
visible emissions/ does not have
opacity test. opacity or
visible
emission
standards.
Sec. 63.9(g)(1) Additional CMS Yes.
notifications--date
of CMS performance
evaluation.
Sec. 63.9(g)(2) Use of COMS data..... No........... Subpart NNNNN
does not
require the
use of COMS.
Sec. 63.9(g)(3) Alternative to No........... Applies only to
relative accuracy sources with
testing. CEMS.
Sec. 63.9(h)... Notification of Yes.......... Except the
compliance status. submission
date specified
in Sec.
63.9(h)(2)(ii)
is superseded
by the date
specified in
Sec.
63.9045(f).
Sec. 63.9(i)... Adjustment of Yes.
submittal deadlines.
Sec. 63.9(j)... Change in previous Yes.
information.
Sec. 63.10(a).. Recordkeeping/ Yes.
reporting
applicability.
Sec. General recordkeeping Yes.......... Sec. Sec.
63.10(b)(1). requirements. 63.9055 and
63.9060
specify
additional
recordkeeping
requirements.
Sec. Records related to Yes.
63.10(b)(2)(i)-( SSM periods and CMS.
xi).
Sec. Records when under Yes.
63.10(b)(2)(xii). waiver.
Sec. Records when using No........... Applies only to
63.10(b)(2)(xiii alternative to sources with
). relative accuracy CEMS.
test.
Sec. All documentation Yes.
63.10(b)(2)(xiv). supporting initial
notification and
notification of
compliance status.
Sec. Recordkeeping Yes. ...............
63.10(b)(3). requirements for
applicability
determinations.
Sec. 63.10(c).. Additional Yes.......... Applies as
recordkeeping modified by
requirements for Sec. 63.9005
sources with CMS. (d).
Sec. General reporting Yes.......... Sec. 63.9050
63.10(d)(1). requirements. specifies
additional
reporting
requirements.
Sec. Performance test Yes.......... Sec.
63.10(d)(2). results. 63.9045(f)
specifies
submission
date.
Sec. Opacity or visible No........... Subpart NNNNN
63.10(d)(3). emissions does not
observations. specify
opacity or
visible
emission
standards.
Sec. Progress reports for Yes.
63.10(d)(4). sources with
compliance
extensions.
Sec. SSM reports.......... Yes.
63.10(d)(5).
Sec. Additional CMS Yes.......... Applies as
63.10(e)(1). reports--general. modified by
Sec.
63.9005(d).
[[Page 27]]
Sec. Results of CMS Yes.......... Applies as
63.10(e)(2)(i). performance modified by
evaluations. Sec.
63.9005(d).
Sec. Results of COMS No........... Subpart NNNNN
63.10(e)(2). performance does not
evaluations. require the
use of COMS.
Sec. Excess emissions/CMS Yes.
63.10(e)(3). performance reports.
Sec. Continuous opacity No........... Subpart NNNNN
63.10(e)(4). monitoring system does not
data reports. require the
use of COMS.
Sec. 63.10(f).. Recordkeeping/ Yes.
reporting waiver.
Sec. 63.11..... Control device No........... Facilities
requirements--applic subject to
ability. subpart NNNNN
do not use
flares as
control
devices.
Sec. 63.12..... State authority and Yes.......... Sec. 63.9070
delegations. lists those
sections of
subparts NNNNN
and A that are
not delegated.
Sec. 63.13..... Addresses............ Yes.
Sec. 63.14..... Incorporation by Yes.......... Subpart NNNNN
reference. does not
incorporate
any material
by reference.
Sec. 63.15..... Availability of Yes.
information/
confidentiality.
------------------------------------------------------------------------
[68 FR 19090, Apr. 17, 2003, as amended at 71 FR 17748, Apr. 7, 2006]
Subpart OOOOO [Reserved]
Subpart PPPPP_National Emission Standards for Hazardous Air Pollutants
for Engine Test Cells/Stands
Source: 68 FR 28785, May 27, 2003, unless otherwise noted.
What This Subpart Covers
Sec. 63.9280 What is the purpose of subpart PPPPP?
This subpart PPPPP establishes national emission standards for
hazardous air pollutants (NESHAP) for engine test cells/stands located
at major sources of hazardous air pollutants (HAP) emissions. This
subpart also establishes requirements to demonstrate initial and
continuous compliance with the emission limitations contained in this
NESHAP.
Sec. 63.9285 Am I subject to this subpart?
You are subject to this subpart if you own or operate an engine test
cell/stand that is located at a major source of HAP emissions.
(a) An engine test cell/stand is any apparatus used for testing
uninstalled stationary or uninstalled mobile (motive) engines.
(b) An uninstalled engine is an engine that is not installed in, or
an integrated part of, the final product.
(c) A major source of HAP emissions is a plant site that emits or
has the potential to emit any single HAP at a rate of 10 tons (9.07
megagrams) or more per year or any combination of HAP at a rate of 25
tons (22.68 megagrams) or more per year.
Sec. 63.9290 What parts of my plant does this subpart cover?
This subpart applies to each new, reconstructed, or existing
affected source.
(a) Affected source. An affected source is the collection of all
equipment and activities associated with engine test cells/stands used
for testing uninstalled stationary or uninstalled mobile (motive)
engines located at a major source of HAP emissions.
(1) Existing affected source. An affected source is existing if you
commenced construction or reconstruction of the affected source on or
before May 14, 2002. A change in ownership of an existing affected
source does not make that affected source a new or reconstructed
affected source.
(2) New affected source. An affected source is new if you commenced
construction of the affected source after May 14, 2002.
(3) Reconstructed affected source. An affected source is
reconstructed if you
[[Page 28]]
meet the definition of reconstruction in Sec. 63.2 of subpart A of this
part and reconstruction is commenced after May 14, 2002. Changes made to
an existing affected source primarily for the purpose of complying with
revisions to engine testing requirements under 40 CFR parts 80, 86, 89,
90, 91, or 92 are not considered a modification or reconstruction. In
addition, passive measurement and control instrumentation and
electronics are not included as part of any affected source
reconstruction evaluation.
(b) Existing affected sources do not have to meet the requirements
of this subpart and of subpart A of this part.
(c) Any portion of a new or reconstructed affected source located at
a major source that is used exclusively for testing internal combustion
engines with rated power of less than 25 horsepower (hp) (19
kilowatts(kW)) does not have to meet the requirements of this subpart
and of subpart A of this part except for the initial notification
requirements of Sec. 63.9345(b).
(d) Any portion of a new or reconstructed affected source located at
a major source that meets any of the criteria specified in paragraphs
(d)(1) through (4) of this section does not have to meet the
requirements of this subpart and of subpart A of this part.
(1) Any portion of the affected source used exclusively for testing
combustion turbine engines.
(2) Any portion of the affected source used exclusively for testing
rocket engines.
(3) Any portion of the affected source used in research and teaching
activities at facilities that are not engaged in the development of
engines or engine test services for commercial purposes.
(4) Any portion of the affected source operated to test or evaluate
fuels (such as knock engines), transmissions, or electronics.
Sec. 63.9295 When do I have to comply with this subpart?
(a) Affected sources. (1) If you start up your new or reconstructed
affected source before May 27, 2003, you must comply with the emission
limitations in this subpart no later than May 27, 2003.
(2) If you start up your new or reconstructed affected source on or
after May 27, 2003, you must comply with the emission limitations in
this subpart upon startup.
(b) Area sources that become major sources. If your new or
reconstructed affected source is located at an area source that
increases its emissions or its potential to emit such that it becomes a
major source of HAP, your new or reconstructed affected source must be
in compliance with this subpart when the area source becomes a major
source.
(c) You must meet the notification requirements in Sec. 63.9345 and
in 40 CFR part 63, subpart A.
Emission Limitations
Sec. 63.9300 What emission limitations must I meet?
For each new or reconstructed affected source that is used in whole
or in part for testing internal combustion engines with rated power of
25 hp (19 kW) or more and that is located at a major source, you must
comply with the emission limitations in Table 1 to this subpart. (Tables
are found at the end of this subpart.)
Sec. 63.9301 What are my options for meeting the emission limits?
You may use either a continuous parameter monitoring system (CPMS)
or a continuous emission monitoring system (CEMS) to demonstrate
compliance with the emission limitations. Continuous monitoring systems
must meet the requirements in Sec. 63.9306 (CPMS) and Sec. 63.9307
(CEMS).
Sec. 63.9302 What operating limits must I meet?
(a) For any new or reconstructed affected source on which you use
add-on controls, you must meet the operating limits specified in Table 2
to this subpart. These operating limits must be established during the
performance test according to the requirements in Sec. 63.9324. You
must meet the operating limits at all times after you establish them.
(b) If you use an add-on control device other than those listed in
Table 2 to this subpart, or wish to monitor an
[[Page 29]]
alternative parameter and comply with a different operating limit, you
must apply to the Administrator for approval of alternative monitoring
under Sec. 63.8(f).
General Compliane Requirements
Sec. 63.9305 What are my general requirements for complying with this
subpart?
(a) You must be in compliance with the emission limitation that
applies to you at all times, except during periods of startup, shutdown,
or malfunction (SSM) of your control device or associated monitoring
equipment.
(b) If you must comply with the emission limitation, you must
operate and maintain your engine test cell/stand, air pollution control
equipment, and monitoring equipment in a manner consistent with good air
pollution control practices for minimizing emissions at all times.
(c) You must develop a written SSM plan (SSMP) for emission control
devices and associated monitoring equipment according to the provisions
in Sec. 63.6(e)(3). The plan will apply only to emission control
devices, and not to engine test cells/stands.
[68 FR 28785, May 27, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Sec. 63.9306 What are my continuous parameter monitoring system (CPMS)
installation, operation, and maintenance requirements?
(a) General. You must install, operate, and maintain each CPMS
specified in paragraphs (c) and (d) of this section according to
paragraphs (a)(1) through (7) of this section. You must install,
operate, and maintain each CPMS specified in paragraph (b) of this
section according to paragraphs (a)(3) through (5) of this section.
(1) The CPMS must complete a minimum of one cycle of operation for
each successive 15-minute period. You must have a minimum of four
equally spaced successive cycles of CPMS operation in 1 hour.
(2) You must determine the average of all recorded readings for each
successive 3-hour period of the emission capture system and add-on
control device operation.
(3) You must record the results of each inspection, calibration, and
validation check of the CPMS.
(4) You must maintain the CPMS at all times and have available
necessary parts for routine repairs of the monitoring equipment.
(5) You must operate the CPMS and collect emission capture system
and add-on control device parameter data at all times that an engine
test cell/stand is operating, except during monitoring malfunctions,
associated repairs, and required quality assurance or control activities
(including, if applicable, calibration checks and required zero and span
adjustments).
(6) You must not use emission capture system or add-on control
device parameter data recorded during monitoring malfunctions,
associated repairs, out-of-control periods, or required quality
assurance or control activities when calculating data averages. You must
use all the data collected during all other periods in calculating the
data averages for determining compliance with the emission capture
system and add-on control device operating limits.
(7) A monitoring malfunction is any sudden, infrequent, not
reasonably preventable failure of the CPMS to provide valid data.
Monitoring failures that are caused in part by poor maintenance or
careless operation are not malfunctions. Any period for which the
monitoring system is out-of-control and data are not available for
required calculations is a deviation from the monitoring requirements.
(b) Capture system bypass line. You must meet the requirements of
paragraphs (b)(1) and (2) of this section for each emission capture
system that contains bypass lines that could divert emissions away from
the add-on control device to the atmosphere.
(1) You must monitor or secure the valve or closure mechanism
controlling the bypass line in a nondiverting position in such a way
that the valve or closure mechanism cannot be opened without creating a
record that the valve was opened. The method used to monitor or secure
the valve or closure mechanism must meet one of the requirements
specified in paragraphs (b)(1)(i) through (iv) of this section.
[[Page 30]]
(i) Flow control position indicator. Install, calibrate, maintain,
and operate according to the manufacturer's specifications a flow
control position indicator that takes a reading at least once every 15
minutes and provides a record indicating whether the emissions are
directed to the add-on control device or diverted from the add-on
control device. The time of occurrence and flow control position must be
recorded, as well as every time the flow direction is changed. The flow
control position indicator must be installed at the entrance to any
bypass line that could divert the emissions away from the add-on control
device to the atmosphere.
(ii) Car-seal or lock-and-key valve closures. Secure any bypass line
valve in the closed position with a car-seal or a lock-and-key type
configuration. You must visually inspect the seal or closure mechanism
at least once every month to ensure that the valve is maintained in the
closed position, and the emissions are not diverted away from the add-on
control device to the atmosphere.
(iii) Valve closure monitoring. Ensure that any bypass line valve is
in the closed (nondiverting) position through monitoring of valve
position at least once every 15 minutes. You must inspect the monitoring
system at least once every month to verify that the monitor will
indicate valve position.
(iv) Automatic shutdown system. Use an automatic shutdown system in
which the engine testing operation is stopped when flow is diverted by
the bypass line away from the add-on control device to the atmosphere
when an engine test cell/stand is operating. You must inspect the
automatic shutdown system at least once every month to verify that it
will detect diversions of flow and shut down the engine test cell/stand
in operation.
(2) If any bypass line is opened, you must include a description of
why the bypass line was opened and the length of time it remained open
in the semiannual compliance reports required in Sec. 63.9350.
(c) Thermal oxidizers and catalytic oxidizers. If you are using a
thermal oxidizer or catalytic oxidizer as an add-on control device, you
must comply with the requirements in paragraphs (c)(1) through (3) of
this section.
(1) For a thermal oxidizer, install a gas temperature monitor in the
firebox of the thermal oxidizer or in the duct immediately downstream of
the firebox before any substantial heat exchange occurs.
(2) For a catalytic oxidizer, you must install a gas temperature
monitor in the gas stream immediately before the catalyst bed, and if
you established operating limits according to Sec. 63.9324(b)(1) and
(2), also install a gas temperature monitor in the gas stream
immediately after the catalyst bed.
(i) If you establish operating limits according to Sec.
63.9324(b)(1) and (2), then you must install the gas temperature
monitors both upstream and downstream of the catalyst bed. The
temperature monitors must be in the gas stream immediately before and
after the catalyst bed to measure the temperature difference across the
bed.
(ii) If you establish operating limits according to Sec.
63.9324(b)(3) and (4), then you must install a gas temperature monitor
upstream of the catalyst bed. The temperature monitor must be in the gas
stream immediately before the catalyst bed to measure the temperature.
(3) For all thermal oxidizers and catalytic oxidizers, you must meet
the requirements in paragraphs (a) and (c)(3)(i) through (vii) of this
section for each gas temperature monitoring device.
(i) Locate the temperature sensor in a position that provides a
representative temperature.
(ii) Use a temperature sensor with a measurement sensitivity of 4
degrees Fahrenheit or 0.75 percent of the temperature value, whichever
is larger.
(iii) Shield the temperature sensor system from electromagnetic
interference and chemical contaminants.
(iv) If a gas temperature chart recorder is used, it must have a
measurement sensitivity in the minor division of at least 20 degrees
Fahrenheit.
(v) Perform an electronic calibration at least semiannually
according to the procedures in the manufacturer's owner's manual.
Following the electronic calibration, you must conduct a temperature
sensor validation check in
[[Page 31]]
which a second or redundant temperature sensor placed near the process
temperature sensor must yield a reading within 30 degrees Fahrenheit of
the process temperature sensor reading.
(vi) Conduct calibration and validation checks anytime the sensor
exceeds the manufacturer's specified maximum operating temperature range
or install a new temperature sensor.
(vii) At least monthly, inspect components for integrity and
electrical connections for continuity, oxidation, and galvanic
corrosion.
(d) Emission capture systems. The capture system monitoring system
must comply with the applicable requirements in paragraphs (d)(1) and
(2) of this section.
(1) For each flow measurement device, you must meet the requirements
in paragraphs (a) and (d)(1)(i) through (iv) of this section.
(i) Locate a flow sensor in a position that provides a
representative flow measurement in the duct from each capture device in
the emission capture system to the add-on control device.
(ii) Reduce swirling flow or abnormal velocity distributions due to
upstream and downstream disturbances.
(iii) Conduct a flow sensor calibration check at least semiannually.
(iv) At least monthly, inspect components for integrity, electrical
connections for continuity, and mechanical connections for leakage.
(2) For each pressure drop measurement device, you must comply with
the requirements in paragraphs (a) and (d)(2)(i) through (vi) of this
section.
(i) Locate the pressure sensor(s) in or as close to a position that
provides a representative measurement of the pressure drop across each
opening you are monitoring.
(ii) Minimize or eliminate pulsating pressure, vibration, and
internal and external corrosion.
(iii) Check pressure tap pluggage daily.
(iv) Using an inclined manometer with a measurement sensitivity of
0.0002 inch water, check gauge calibration quarterly and transducer
calibration monthly.
(v) Conduct calibration checks any time the sensor exceeds the
manufacturer's specified maximum operating pressure range or install a
new pressure sensor.
(vi) At least monthly, inspect components for integrity, electrical
connections for continuity, and mechanical connections for leakage.
Sec. 63.9307 What are my continuous emissions monitoring system
installation, operation, and maintenance requirements?
(a) You must install, operate, and maintain each CEMS to monitor
carbon monoxide (CO) or total hydrocarbons (THC) and oxygen
(O2) at the outlet of the exhaust system of the engine test
cell/stand or at the outlet of the emission control device.
(b) To comply with the CO or THC percent reduction emission
limitation, you may install, operate, and maintain a CEMS to monitor CO
or THC and O2 at both the inlet and the outlet of the
emission control device.
(c) To comply with either emission limitations, the CEMS must be
installed and operated according to the requirements described in
paragraphs (c)(1) through (4) of this section.
(1) You must install, operate, and maintain each CEMS according to
the applicable Performance Specification (PS) of 40 CFR part 60,
appendix B (PS-3 or PS-4A).
(2) You must conduct a performance evaluation of each CEMS according
to the requirements in 40 CFR 63.8 and according to PS-3 of 40 CFR part
60, appendix B, using Reference Method 3A or 3B for the O2
CEMS, and according to PS-4A of 40 CFR part 60, appendix B, using
Reference Method 10 or 10B for the CO CEMS. If the fuel used in the
engines being tested is natural gas, you may use ASTM D 6522-00,
Standard Test Method for Determination of Nitrogen Oxides, Carbon
Monoxide and Oxygen Concentrations in Emissions from Natural Gas Fired
Reciprocating Engines, Combustion Turbines, Boilers, and Process Heaters
Using Portable Analyzers (incorporated by reference, see Sec. 63.14).
As an alternative to Method 3B, you may use ANSI/ASME PTC 19.10-1981,
``Flue and Exhaust Gas Analyses [Part 10, Instruments and Apparatus],''
(incorporated by reference, see Sec. 63.14).
[[Page 32]]
(3) As specified in Sec. 63.8(c)(4)(ii), each CEMS must complete a
minimum of one cycle of operation (sampling, analyzing, and data
recording) for each successive 15-minute period. You must have at least
two data points, each representing a different 15-minute period within
the same hour, to have a valid hour of data.
(4) All CEMS data must be reduced as specified in Sec. 63.8(g)(2)
and recorded as CO concentration in parts per million by volume, dry
basis (ppmvd), corrected to 15 percent O2 content.
(d) If you have CEMS that are subject to paragraph (a) or (b) of
this section, you must properly maintain and operate the monitors
continuously according to the requirements described in paragraphs
(d)(1) and (2) of this section.
(1) Proper Maintenance. You must maintain the monitoring equipment
at all times that the engine test cell/stand is operating, including but
not limited to, maintaining necessary parts for routine repairs of the
monitoring equipment.
(2) Continued Operation. You must operate your CEMS according to
paragraphs (d)(2)(i) and (ii) of this section.
(i) You must conduct all monitoring in continuous operation at all
times that the engine test cell/stand is operating, except for, as
applicable, monitoring malfunctions, associated repairs, and required
quality assurance or control activities (including, as applicable,
calibration drift checks and required zero and high-level adjustments).
Quality assurance or control activities must be performed according to
procedure 1 of 40 CFR part 60, appendix F.
(ii) Data recorded during monitoring malfunctions, associated
repairs, out-of-control periods, and required quality assurance or
control activities must not be used for purposes of calculating data
averages. You must use all of the data collected from all other periods
in assessing compliance. A monitoring malfunction is any sudden,
infrequent, not reasonably preventable failure of the monitoring
equipment to provide valid data. Monitoring failures that are caused in
part by poor maintenance or careless operation are not malfunctions. Any
period for which the monitoring system is out-of-control and data are
not available for required calculations constitutes a deviation from the
monitoring requirements.
Testing and Initial Compliance Requirements
Sec. 63.9310 By what date must I conduct the initial compliance
demonstrations?
You must conduct the initial compliance demonstrations that apply to
you in Table 3 to this subpart within 180 calendar days after the
compliance date that is specified for your new or reconstructed affected
source in Sec. 63.9295 and according to the provisions in Sec.
63.7(a)(2).
Sec. 63.9320 What procedures must I use?
(a) You must conduct each initial compliance demonstration that
applies to you in Table 3 to this subpart.
(b) You must conduct an initial performance evaluation of each
capture and control system according to Sec. Sec. 63.9321, 63.9322,
63.9323 and 63.9324, and each CEMS according to the requirements in 40
CFR 63.8 and according to the applicable Performance Specification of 40
CFR part 60, appendix B (PS-3 or PS-4A).
(c) The initial demonstration of compliance with the carbon monoxide
(CO) or total hydrocarbon (THC) concentration limitation consists of the
first 4-hour rolling average CO or THC concentration recorded after
completion of the CEMS performance evaluation. You must correct the CO
or THC concentration at the outlet of the engine test cell/stand or the
emission control device to a dry basis and to 15 percent O2
content according to Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.002
Where:
Cc = concentration of CO or THC, corrected to 15 percent
oxygen, ppmvd
Cunc = total uncorrected concentration of CO or THC, ppmvd
%O2d = concentration of oxygen measured in gas stream, dry
basis, percent by volume.
(d) The initial demonstration of compliance with the CO or THC
percent reduction emission limitation consists of
[[Page 33]]
the first 4-hour rolling average percent reduction in CO or THC recorded
after completion of the performance evaluation of the capture/control
system and/or CEMS. You must complete the actions described in
paragraphs (d)(1) through (2) of this section.
(1) Correct the CO or THC concentrations at the inlet and outlet of
the emission control device to a dry basis and to 15 percent
O2 content using Equation 1 of this section.
(2) Calculate the percent reduction in CO or THC using Equation 2 of
this section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.003
Where:
R = percent reduction in CO or THC
Ci = corrected CO or THC concentration at inlet of the
emission control device
Co = corrected CO or THC concentration at the outlet of the
emission control device.
Sec. 63.9321 What are the general requirements for performance tests?
(a) You must conduct each performance test required by Sec. 63.9310
according to the requirements in Sec. 63.7(e)(1) and under the
conditions in this section unless you obtain a waiver of the performance
test according to the provisions in Sec. 63.7(h).
(1) Representative engine testing conditions. You must conduct the
performance test under representative operating conditions for the test
cell/stand. Operations during periods of SSM, and during periods of
nonoperation do not constitute representative conditions. You must
record the process information that is necessary to document operating
conditions during the test and explain why the conditions represent
normal operation.
(2) Representative emission capture system and add-on control device
operating conditions. You must conduct the performance test when the
emission capture system and add-on control device are operating at a
representative flow rate, and the add-on control device is operating at
a representative inlet concentration. You must record information that
is necessary to document emission capture system and add-on control
device operating conditions during the test and explain why the
conditions represent normal operation.
(b) You must conduct each performance test of an emission capture
system according to the requirements in Sec. 63.9322. You must conduct
each performance test of an add-on control device according to the
requirements in Sec. 63.9323.
Sec. 63.9322 How do I determine the emission capture system efficiency?
You must use the procedures and test methods in this section to
determine capture efficiency as part of the performance test required by
Sec. 63.9310.
(a) Assuming 100 percent capture efficiency. You may assume the
capture system efficiency is 100 percent if both conditions in
paragraphs (a)(1) and (2) of this section are met:
(1) The capture system meets the criteria in Method 204 of appendix
M to 40 CFR part 51 for a potential to emit (PTE) and directs all the
exhaust gases from the enclosure to an add-on control device.
(2) All engine test operations creating exhaust gases for which the
test is applicable are conducted within the capture system.
(b) Measuring capture efficiency. If the capture system does not
meet the criteria in paragraphs (a)(1) and (2) of this section, then you
must use one of the two protocols described in paragraphs (c) and (d) of
this section to measure capture efficiency. The capture efficiency
measurements use total volatile hydrocarbon (TVH) capture efficiency as
a surrogate for organic HAP capture efficiency. For the protocol in
paragraph (c) of this section, the capture efficiency measurement must
consist of three test runs. Each test run must be at least 3 hours in
duration or the length of a production run, whichever is longer, up to 8
hours. For the purposes of this test, a production run means the time
required for a single engine test to go from the beginning to the end.
(c) Gas-to-gas protocol using a temporary total enclosure or a
building enclosure. The gas-to-gas protocol compares the mass of TVH
emissions captured by the emission capture system to the mass of TVH
emissions not captured. Use a temporary total enclosure or a
[[Page 34]]
building enclosure and the procedures in paragraphs (c)(1) through (5)
of this section to measure emission capture system efficiency using the
gas-to-gas protocol.
(1) Either use a building enclosure or construct an enclosure around
the engine test cell/stand and all areas where emissions from the engine
testing subsequently occur. The enclosure must meet the applicable
definition of a temporary total enclosure or building enclosure in
Method 204 of appendix M to 40 CFR part 51.
(2) Use Method 204B or 204C of appendix M to 40 CFR part 51 to
measure the total mass, kg, of TVH emissions captured by the emission
capture system during each capture efficiency test run as measured at
the inlet to the add-on control device. To make the measurement,
substitute TVH for each occurrence of the term VOC in the methods.
(i) The sampling points for the Method 204B or 204C of appendix M to
40 CFR part 51 measurement must be upstream from the add-on control
device and must represent total emissions routed from the capture system
and entering the add-on control device.
(ii) If multiple emission streams from the capture system enter the
add-on control device without a single common duct, then the emissions
entering the add-on control device must be simultaneously measured in
each duct, and the total emissions entering the add-on control device
must be determined.
(3) Use Method 204D or 204E of appendix M to 40 CFR part 51 to
measure the total mass, kg, of TVH emissions that are not captured by
the emission capture system; they are measured as they exit the
temporary total enclosure or building enclosure during each capture
efficiency test run. To make the measurement, substitute TVH for each
occurrence of the term VOC in the methods.
(i) Use Method 204D of appendix M to 40 CFR part 51 if the enclosure
is a temporary total enclosure.
(ii) Use Method 204E of appendix M to 40 CFR part 51 if the
enclosure is a building enclosure. During the capture efficiency
measurement, all organic compound emitting operations inside the
building enclosure, other than the engine test cell/stand operation for
which capture efficiency is being determined, must be shut down, but all
fans and blowers must be operating normally.
(4) For each capture efficiency test run, determine the percent
capture efficiency of the emission capture system using Equation 1 of
this section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.004
Where:
CE = capture efficiency of the emission capture system vented to the
add-on control device, percent
TVHcaptured = total mass of TVH captured by the emission
capture system as measured at the inlet to the add-on control device
during the emission capture efficiency test run, kg, determined
according to paragraph (c)(2) of this section
TVHuncaptured = total mass of TVH that is not captured by the
emission capture system and that exits from the temporary total
enclosure or building enclosure during the capture efficiency test run,
kg, determined according to paragraph (c)(3) of this section.
(5) Determine the capture efficiency the emission capture system as
the average of the capture efficiencies measured in the three test runs.
(d) Alternative capture efficiency protocol. As an alternative to
the procedure specified in paragraph (c) of this section, you may
determine capture efficiency using any other capture efficiency protocol
and test methods that satisfy the criteria of either the data quality
objective or lower control limit approach as described in appendix A to
subpart KK of this part.
[[Page 35]]
Sec. 63.9323 How do I determine the add-on control device emission
destruction or removal efficiency?
You must use the procedures and test methods in this section to
determine the add-on control device emission destruction or removal
efficiency as part of the performance test required by Sec. 63.9310.
You must conduct three test runs as specified in Sec. 63.7(e)(3), and
each test run must last at least 1 hour.
(a) For all types of add-on control devices, use the test methods
specified in paragraphs (a)(1) through (5) of this section.
(1) Use Method 1 or 1A of appendix A to 40 CFR part 60, as
appropriate, to select sampling sites and velocity traverse points.
(2) Use Method 2, 2A, 2C, 2D, 2F, or 2G of appendix A to 40 CFR part
60, as appropriate, to measure gas volumetric flow rate.
(3) Use Method 3, 3A, or 3B of appendix A to 40 CFR part 60, as
appropriate, for gas analysis to determine dry molecular weight. The
ANSI/ASME PTC 19.10-1981 Part 10 is an acceptable alternative to Method
3B (incorporated by reference, see Sec. 63.14).
(4) Use Method 4 of appendix A to 40 CFR part 60, to determine stack
gas moisture.
(5) Methods for determining gas volumetric flow rate, dry molecular
weight, and stack gas moisture must be performed, as applicable, during
each test run.
(b) Measure total gaseous organic mass emissions as carbon at the
inlet and outlet of the add-on control device simultaneously, using
either Method 25 or 25A of appendix A to 40 CFR part 60, as specified in
paragraphs (b)(1) through (3) of this section. You must use the same
method for both the inlet and outlet measurements.
(1) Use Method 25 of appendix A to 40 CFR part 60 if the add-on
control device is an oxidizer, and you expect the total gaseous organic
concentration as carbon to be more than 50 parts per million at the
control device outlet.
(2) Use Method 25A of appendix A to 40 CFR part 60 if the add-on
control device is an oxidizer, and you expect the total gaseous organic
concentration as carbon to be 50 ppm or less at the control device
outlet.
(c) For each test run, determine the total gaseous organic emissions
mass flow rates for the inlet and the outlet of the add-on control
device, using Equation 1 of this section. If there is more than one
inlet or outlet to the add-on control device, you must calculate the
total gaseous organic mass flow rate using Equation 1 of this section
for each inlet and each outlet and then total all of the inlet emissions
and total all of the outlet emissions.
[GRAPHIC] [TIFF OMITTED] TR27MY03.005
Where:
Mf = total gaseous organic emissions mass flow rate, kg/hour
(kg/h)
Cc = concentration of organic compounds as carbon in the vent
gas, as determined by Method 25 or Method 25A, parts per million by
volume (ppmv), dry basis
Qsd = volumetric flow rate of gases entering or exiting the
add-on control device, as determined by Method 2, 2A, 2C, 2D, 2F, or 2G,
dry standard cubic meters/hour (dscm/h)
0.0416 = conversion factor for molar volume, kg-moles per cubic meter
(mol/m\3\) (@ 293 Kelvin [K] and 760 millimeters of mercury [mmHg]).
(d) For each test run, determine the add-on control device organic
emissions destruction or removal efficiency, using Equation 2 of this
section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.006
Where:
DRE = organic emissions destruction or removal efficiency of the add-on
control device, percent
Mfi = total gaseous organic emissions mass flow rate at the
inlet(s) to the add-on control device, using Equation 1 of this section,
kg/h
[[Page 36]]
Mfo = total gaseous organic emissions mass flow rate at the
outlet(s) of the add-on control device, using Equation 1 of this
section, kg/h.
(e) Determine the emission destruction or removal efficiency of the
add-on control device as the average of the efficiencies determined in
the three test runs and calculated in Equation 2 of this section.
Sec. 63.9324 How do I establish the emission capture system and add-on
control device operating limits during the performance test?
During the performance test required by Sec. 63.9310, you must
establish the operating limits required by Sec. 63.9302 according to
this section, unless you have received approval for alternative
monitoring and operating limits under Sec. 63.8(f) as specified in
Sec. 63.9302.
(a) Thermal oxidizers. If your add-on control device is a thermal
oxidizer, establish the operating limits according to paragraphs (a)(1)
and (2) of this section.
(1) During the performance test, you must monitor and record the
combustion temperature at least once every 15 minutes during each of the
three test runs. You must monitor the temperature in the firebox of the
thermal oxidizer or immediately downstream of the firebox before any
substantial heat exchange occurs.
(2) Use the data collected during the performance test to calculate
and record the average combustion temperature maintained during the
performance test. This average combustion temperature is the minimum
operating limit for your thermal oxidizer.
(b) Catalytic oxidizers. If your add-on control device is a
catalytic oxidizer, establish the operating limits according to either
paragraphs (b)(1) and (2) or paragraphs (b)(3) and (4) of this section.
(1) During the performance test, you must monitor and record the
temperature just before the catalyst bed and the temperature difference
across the catalyst bed at least once every 15 minutes during each of
the three test runs.
(2) Use the data collected during the performance test to calculate
and record the average temperature just before the catalyst bed and the
average temperature difference across the catalyst bed maintained during
the performance test. These are the minimum operating limits for your
catalytic oxidizer.
(3) As an alternative to monitoring the temperature difference
across the catalyst bed, you may monitor the temperature at the inlet to
the catalyst bed and implement a site-specific inspection and
maintenance plan for your catalytic oxidizer as specified in paragraph
(b)(4) of this section. During the performance test, you must monitor
and record the temperature just before the catalyst bed at least once
every 15 minutes during each of the three test runs. Use the data
collected during the performance test to calculate and record the
average temperature just before the catalyst bed during the performance
test. This is the minimum operating limit for your catalytic oxidizer.
(4) You must develop and implement an inspection and maintenance
plan for your catalytic oxidizer(s) for which you elect to monitor
according to paragraph (b)(3) of this section. The plan must address, at
a minimum, the elements specified in paragraphs (b)(4)(i) through (iii)
of this section.
(i) Annual sampling and analysis of the catalyst activity (i.e.,
conversion efficiency) following the manufacturer's or catalyst
supplier's recommended procedures.
(ii) Monthly inspection of the oxidizer system, including the burner
assembly and fuel supply lines for problems and, as necessary, adjust
the equipment to assure proper air-to-fuel mixtures.
(iii) Annual internal and monthly external visual inspection of the
catalyst bed to check for channeling, abrasion, and settling. If
problems are found, you must take corrective action consistent with the
manufacturer's recommendation and conduct a new performance test to
determine destruction efficiency according to Sec. 63.9323.
(c) Emission capture system. For each capture device that is not
part of a PTE that meets the criteria of Sec. 63.9322(a), establish an
operating limit for either the gas volumetric flow rate or duct static
pressure, as specified in paragraphs (c)(1) and (2) of this section.
[[Page 37]]
The operating limit for a PTE is specified in Table 3 to this subpart.
(1) During the capture efficiency determination required by Sec.
63.9310, you must monitor and record either the gas volumetric flow rate
or the duct static pressure for each separate capture device in your
emission capture system at least once every 15 minutes during each of
the three test runs at a point in the duct between the capture device
and the add-on control device inlet.
(2) Calculate and record the average gas volumetric flow rate or
duct static pressure for the three test runs for each capture device.
This average gas volumetric flow rate or duct static pressure is the
minimum operating limit for that specific capture device.
Sec. 63.9330 How do I demonstrate initial compliance with the emission
limitation?
(a) You must demonstrate initial compliance with the emission
limitation that applies to you according to Table 3 to this subpart.
(b) You must submit the Notification of Compliance Status containing
results of the initial compliance demonstration according to the
requirements in Sec. 63.9345(c).
Continuous Compliance Requirements
Sec. 63.9335 How do I monitor and collect data to demonstrate continuous
compliance?
(a) Except for monitor malfunctions, associated repairs, and
required quality assurance or quality control activities (including, as
applicable, calibration drift checks and required zero and high-level
adjustments of the monitoring system), you must conduct all monitoring
in continuous operation at all times the engine test cell/stand is
operating.
(b) Do not use data recorded during monitor malfunctions, associated
repairs, and required quality assurance or quality control activities
for meeting the requirements of this subpart, including data averages
and calculations. You must use all the data collected during all other
periods in assessing the performance of the emission control device or
in assessing emissions from the new or reconstructed affected source.
Sec. 63.9340 How do I demonstrate continuous compliance with the
emission limitations?
(a) You must demonstrate continuous compliance with the emission
limitation in Table 1 to this subpart that applies to you according to
methods specified in Table 5 to this subpart.
(b) You must report each instance in paragraphs (b)(1) and (2) of
this section. These instances are deviations from the emission
limitation in this subpart and must be reported according to the
requirements in Sec. 63.9350.
(1) You must report each instance in which you did not meet the
emission limitation that applies to you.
(2) You must report each instance in which you did not meet the
requirements in Table 7 to this subpart that apply to you.
(c) Startups, shutdowns, and malfunctions. (1) Consistent with
Sec. Sec. 63.6(e) and 63.7(e)(1), deviations that occur during a period
of SSM of control devices and associated monitoring equipment are not
violations if you demonstrate to the Administrator's satisfaction that
you were operating in accordance with Sec. 63.6(e)(1).
(2) The Administrator will determine whether deviations that occur
during a period of SSM of control devices and associated monitoring
equipment are violations, according to the provisions in Sec. 63.6(e).
[68 FR 28785, May 27, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Notifications, Reports, and Records
Sec. 63.9345 What notifications must I submit and when?
(a) You must submit all of the notifications in Sec. Sec. 63.8(e),
63.8(f)(4) and (6), and 63.9(b), (g)(1), (g)(2) and (h) that apply to
you by the dates specified.
(b) If you own or operate a new or reconstructed test cell/stand
used for testing internal combustion engines, you are required to submit
an Initial Notification as specified in paragraphs (b)(1) through (3) of
this section.
(1) As specified in Sec. 63.9(b)(2), if you start up your new or
reconstructed affected source before the effective date of this subpart,
you must submit an Initial Notification not later than 120 calendar days
after May 27, 2003.
[[Page 38]]
(2) As specified in Sec. 63.9(b), if you start up your new or
reconstructed affected source on or after the effective date of this
subpart, you must submit an Initial Notification not later than 120
calendar days after you become subject to this subpart.
(3) If you are required to submit an Initial Notification but are
otherwise not affected by the requirements of this subpart, in
accordance with Sec. 63.9290(c), your notification should include the
information in Sec. 63.9(b)(2)(i) through (v) and a statement that your
new or reconstructed engine test cell/stand has no additional
requirements and explain the basis of the exclusion (for example, that
the test cell/stand is used exclusively for testing internal combustion
engines with rated power of less than 25 hp (19 kW)).
(c) If you are required to comply with the emission limitations in
Table 1 to this subpart, you must submit a Notification of Compliance
Status according to Sec. 63.9(h)(2)(ii). For each initial compliance
demonstration with the emission limitation, you must submit the
Notification of Compliance Status before the close of business on the
30th calendar day following the completion of the initial compliance
demonstration.
(d) You must submit a notification of initial performance evaluation
of your CEMS or performance testing of your control device at least 60
calendar days before the performance testing/evaluation is scheduled to
begin as required in Sec. 63.8(e)(2).
Sec. 63.9350 What reports must I submit and when?
(a) If you own or operate a new or reconstructed affected source
that must meet the emission limitation, you must submit a semiannual
compliance report according to Table 6 to this subpart by the applicable
dates specified in paragraphs (a)(1) through (6) of this section, unless
the Administrator has approved a different schedule.
(1) The first semiannual compliance report must cover the period
beginning on the compliance date specified in Sec. 63.9295 and ending
on June 30 or December 31, whichever date is the first date following
the end of the first calendar half after the compliance date specified
in Sec. 63.9295.
(2) The first semiannual compliance report must be postmarked or
delivered no later than July 31 or January 31, whichever date follows
the end of the first calendar half after the compliance date that is
specified in Sec. 63.9295.
(3) Each subsequent semiannual compliance report must cover the
semiannual reporting period from January 1 through June 30 or the
semiannual reporting period from July 1 through December 31.
(4) Each subsequent semiannual compliance report must be postmarked
or delivered no later than July 31 or January 31, whichever date is the
first date following the end of the semiannual reporting period.
(5) For each new or reconstructed engine test cell/stand that is
subject to permitting regulations pursuant to 40 CFR part 70 or 71, and
if the permitting authority has established the date for submitting
semiannual reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance
reports according to the dates the permitting authority has established
instead of according to the dates in paragraphs (a)(1) through (4) of
this section.
(6) If you had an SSM of a control device or associated monitoring
equipment during the reporting period and you took actions consistent
with your SSMP, the compliance report must include the information in
paragraphs Sec. 63.10(d)(5)(i).
(b) If there is no deviation from the applicable emission limitation
and the CEMS or CPMS was not out-of-control, according to Sec.
63.8(c)(7), the semiannual compliance report must contain the
information described in paragraphs (b)(1) through (4) of this section.
(1) Company name and address.
(2) Statement by a responsible official, with that official's name,
title, and signature, certifying the truth, accuracy, and completeness
of the content of the report.
(3) Date of report and beginning and ending dates of the reporting
period.
(4) A statement that no deviation from the emission limit occurred
during the reporting period and that no
[[Page 39]]
CEMS or CPMS was out-of-control, according to Sec. 63.8(c)(7).
(c) For each deviation from an emission limit, the semiannual
compliance report must include the information in paragraphs (b)(1)
through (3) of this section and the information included in paragraphs
(c)(1) through (4) of this section.
(1) The date and time that each deviation started and stopped.
(2) The total operating time of each new or reconstructed engine
test cell/stand during the reporting period.
(3) A summary of the total duration of the deviation during the
reporting period (recorded in 4-hour periods), and the total duration as
a percent of the total operating time during that reporting period.
(4) A breakdown of the total duration of the deviations during the
reporting period into those that are due to control equipment problems,
process problems, other known causes, and other unknown causes.
(d) For each CEMS or CPMS deviation, the semiannual compliance
report must include the information in paragraphs (b)(1) through (3) of
this section and the information included in paragraphs (d)(1) through
(10) of this section.
(1) The date and time that each CEMS or CPMS was inoperative except
for zero (low-level) and high-level checks.
(2) The date and time that each CEMS or CPMS was out-of-control
including the information in Sec. 63.8(c)(8).
(3) A summary of the total duration of CEMS or CPMS downtime during
the reporting period (reported in 4-hour periods), and the total
duration of CEMS or CPMS downtime as a percent of the total engine test
cell/stand operating time during that reporting period.
(4) A breakdown of the total duration of CEMS or CPMS downtime
during the reporting period into periods that are due to monitoring
equipment malfunctions, nonmonitoring equipment malfunctions, quality
assurance/quality control calibrations, other known causes and other
unknown causes.
(5) The monitoring equipment manufacturer(s) and model number(s) of
each monitor.
(6) The date of the latest CEMS or CPMS certification or audit.
(7) The date and time period of each deviation from an operating
limit in Table 2 to this subpart; date and time period of any bypass of
the add-on control device; and whether each deviation occurred during a
period of SSM or during another period.
(8) A summary of the total duration of each deviation from an
operating limit in Table 2 to this subpart, each bypass of the add-on
control device during the semiannual reporting period, and the total
duration as a percent of the total source operating time during that
semiannual reporting period.
(9) A breakdown of the total duration of the deviations from the
operating limits in Table 2 to this subpart and bypasses of the add-on
control device during the semiannual reporting period by identifying
deviations due to startup, shutdown, control equipment problems, process
problems, other known causes, and other unknown causes.
(10) A description of any changes in CEMS, CPMS, or controls since
the last reporting period.
(e) If you had an SSM of a control device or associated monitoring
equipment during the semiannual reporting period that was not consistent
with your SSMP, you must submit an immediate SSM report according to the
requirements in Sec. 63.10(d)(5)(ii).
Sec. 63.9355 What records must I keep?
(a) You must keep the records as described in paragraphs (a)(1)
through (5) of this section.
(1) A copy of each notification and report that you submitted to
comply with this subpart, including all documentation supporting any
Initial Notification or Notification of Compliance Status that you
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
(2) Records of performance evaluations as required in Sec.
63.10(b)(2)(viii).
(3) Records of the occurrence and duration of each malfunction of
the air pollution control equipment, if applicable, as required in Sec.
63.10(b)(2)(ii).
(4) Records of all maintenance on the air pollution control
equipment, if applicable, as required in Sec. 63.10(b)(iii).
[[Page 40]]
(5) The calculation of the mass of organic HAP emission reduction by
emission capture systems and add-on control devices.
(b) For each CPMS, you must keep the records as described in
paragraphs (b)(1) through (7) of this section.
(1) For each deviation, a record of whether the deviation occurred
during a period of SSM of the control device and associated monitoring
equipment.
(2) The records in Sec. 63.6(e)(3)(iii) through (v) related to SSM.
(3) The records required to show continuous compliance with each
operating limit specified in Table 2 to this subpart that applies to
you.
(4) For each capture system that is a PTE, the data and
documentation you used to support a determination that the capture
system meets the criteria in Method 204 of appendix M to 40 CFR part 51
for a PTE and has a capture efficiency of 100 percent, as specified in
Sec. 63.9322(a).
(5) For each capture system that is not a PTE, the data and
documentation you used to determine capture efficiency according to the
requirements specified in Sec. Sec. 63.9321 and 63.9322(b) through (e),
including the records specified in paragraphs (b)(5)(i) and (ii) of this
section that apply to you.
(i) Records for a gas-to-gas protocol using a temporary total
enclosure or a building enclosure. Records of the mass of TVH emissions
captured by the emission capture system as measured by Method 204B or C
of appendix M to 40 CFR part 51 at the inlet to the add-on control
device, including a copy of the test report. Records of the mass of TVH
emissions not captured by the capture system that exited the temporary
total enclosure or building enclosure during each capture efficiency
test run as measured by Method 204D or E of appendix M to 40 CFR part
51, including a copy of the test report. Records documenting that the
enclosure used for the capture efficiency test met the criteria in
Method 204 of appendix M to 40 CFR part 51 for either a temporary total
enclosure or a building enclosure.
(ii) Records for an alternative protocol. Records needed to document
a capture efficiency determination using an alternative method or
protocol as specified in Sec. 63.9322(e), if applicable.
(6) The records specified in paragraphs (b)(6)(i) and (ii) of this
section for each add-on control device organic HAP destruction or
removal efficiency determination as specified in Sec. 63.9323.
(i) Records of each add-on control device performance test conducted
according to Sec. Sec. 63.9321, 63.9322, and 63.9323.
(ii) Records of the engine testing conditions during the add-on
control device performance test showing that the performance test was
conducted under representative operating conditions.
(7) Records of the data and calculations you used to establish the
emission capture and add-on control device operating limits as specified
in Sec. 63.9324 and to document compliance with the operating limits as
specified in Table 2 to this subpart.
(c) For each CEMS, you must keep the records as described in
paragraphs (c)(1) through (4) of this section.
(1) Records described in Sec. 63.10(b)(2)(vi) through (xi).
(2) Previous (i.e., superceded) versions of the performance
evaluation plan as required in Sec. 63.8(d)(3).
(3) Request for alternatives to the relative accuracy test for CEMS
as required in Sec. 63.8(f)(6)(i), if applicable.
(4) The records in Sec. 63.6(e)(3)(iii) through (v) related to SSM
of the control device and associated monitoring equipment.
(d) You must keep the records required in Table 5 to this subpart to
show continuous compliance with each emission limitation that applies to
you.
Sec. 63.9360 In what form and how long must I keep my records?
(a) You must maintain all applicable records in such a manner that
they can be readily accessed and are suitable for inspection according
to Sec. 63.10(b)(1).
(b) As specified in Sec. 63.10(b)(1), you must keep each records
for 5 years following the date of each occurrence, measurement,
maintenance, corrective action, report, or record.
(c) You must retain your records of the most recent 2 years on site,
or your records must be accessible on site. Your records of the
remaining 3 years may be retained off site.
[[Page 41]]
Other Requirements and Information
Sec. 63.9365 What parts of the General Provisions apply to me?
Table 7 to this subpart shows which parts of the General Provisions
in Sec. Sec. 63.1 through 63.15 apply to you.
Sec. 63.9370 Who implements and enforces this subpart?
(a) This subpart can be implemented and enforced by us, the U.S.
EPA, or a delegated authority such as your State, local, or tribal
agency. If the U.S. EPA Administrator has delegated authority to your
State, local, or tribal agency, then that agency, in addition to the
U.S. EPA, has the authority to implement and enforce this subpart. You
should contact your U.S. EPA Regional Office to find out if
implementation and enforcement of this subpart is delegated to your
State, local, or tribal agency.
(b) In delegating implementation and enforcement authority of this
subpart to a State, local, or tribal agency under section 40 CFR part
63, subpart E, the authorities contained in paragraph (c) of this
section are retained by the Administrator of U.S. EPA and are not
transferred to the State, local, or tribal agency.
(c) The authorities that cannot be delegated to State, local, or
tribal agencies are described in paragraphs (c)(1) through (4) of this
section.
(1) Approval of alternatives to the emission limitations in Sec.
63.9300 under Sec. 63.6(g).
(2) Approval of major changes to test methods under Sec.
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
(3) Approval of major changes to monitoring under Sec. 63.8(f) and
as defined in Sec. 63.90.
(4) Approval of major changes to recordkeeping and reporting under
Sec. 63.10(f) and as defined in Sec. 63.90.
Sec. 63.9375 What definitions apply to this subpart?
Terms used in this subpart are defined in the CAA; in 40 CFR 63.2,
and in this section:
CAA means the Clean Air Act (42 U.S.C. 7401 et seq., as amended by
Public Law 101-549, 104 Statute 2399).
Area source means any stationary source of HAP that is not a major
source as defined in this part.
Combustion turbine engine means a device in which air is compressed
in a compressor, enters a combustion chamber, and is compressed further
by the combustion of fuel injected into the combustion chamber. The hot
compressed combustion gases then expand over a series of curved vanes or
blades arranged on a central spindle that rotates.
Deviation means any instance in which an affected source subject to
this subpart, or an owner or operator of such a source:
(1) Fails to meet any requirement or obligation established by this
subpart, including but not limited to any emission limitations;
(2) Fails to meet any term or condition that is adopted to implement
an applicable requirement in this subpart and that is included in the
operating permit for any affected source required to obtain such a
permit; or
(3) Fails to meet any emission limitation in this subpart during
malfunction, regardless or whether or not such failure is permitted by
this subpart.
Engine means any internal combustion engine, any combustion turbine
engine, or any rocket engine.
Engine Test Cell/Stand means any apparatus used for testing
uninstalled stationary or uninstalled mobile (motive) engines.
Hazardous Air Pollutant (HAP) means any air pollutant listed in or
pursuant to section 112(b) of the CAA.
Internal combustion engine means a device in which air enters a
combustion chamber, is mixed with fuel, compressed in the chamber, and
combusted. Fuel may enter the combustion chamber with the air or be
injected into the combustion chamber. Expansion of the hot combustion
gases in the chamber rotates a shaft, either through a reciprocating or
rotary action. For purposes of this subpart, this definition does not
include combustion turbine engines.
Major source, as used in this subpart, shall have the same meaning
as in Sec. 63.2.
Malfunction means any sudden, infrequent, and not reasonably
preventable
[[Page 42]]
failure of air pollution control equipment, process equipment, or a
process to operate in a normal or usual manner which causes, or has the
potential to cause, the emission limitations in an applicable standard
to be exceeded. Failures that are caused in part by poor maintenance or
careless operation are not malfunctions.
Rated power means the maximum power output of an engine in use.
Potential to emit means the maximum capacity of a stationary source
to emit a pollutant under its physical and operational design. Any
physical or operational limitation on the capacity of the stationary
source to emit a pollutant, including air pollution control equipment
and restrictions on hours of operation or on the type or amount of
material combusted, stored, or processed, shall be treated as part of
its design if the limitation or the effect it would have on emissions is
federally enforceable.
Responsible official means responsible official as defined by 40 CFR
70.2.
Rocket engine means a device consisting of a combustion chamber in
which materials referred to as propellants, which provide both the fuel
and the oxygen for combustion, are burned. Combustion gases escape
through a nozzle, providing thrust.
Uninstalled engine means an engine not installed in, or an
integrated part of, the final product.
[68 FR 28785, May 27, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Table 1 to Subpart PPPPP of Part 63--Emission Limitations
You must comply with the emission limits that apply to your affected
source in the following table as required by Sec. 63.9300.
------------------------------------------------------------------------
For each new or reconstructed affected
source located at a major source You must meet one of the
facility that is used in whole or in following emission limitations:
part for testing . . .
------------------------------------------------------------------------
1. internal combustion engines with a. limit the concentration of
rated power of 25 hp (19 kW) or more. CO or THC to 20 ppmvd or less
(corrected to 15 percent O2
content); or
b. achieve a reduction in CO or
THC of 96 percent or more
between the inlet and outlet
concentrations (corrected to
15 percent O2 content) of the
emission control device.
------------------------------------------------------------------------
Table 2 to Subpart PPPPP of Part 63--Operating Limits
If you are required to comply with operating limits in Sec.
63.9302, you must comply with the applicable operating limits in the
following table:
------------------------------------------------------------------------
and you must
demonstrate
For the following device . . You must meet the continuous
. following operating compliance with the
limit . . . operating limit by .
. .
------------------------------------------------------------------------
1. Thermal oxidizer......... a. The average i. Collecting the
combustion combustion
temperature in any temperature data
3-hour period must according to Sec.
not fall below the 63.9306(c);
combustion ii. Reducing the
temperature limit data to 3-hour
established block averages; and
according to Sec. iii. Maintaining the
63.9324(a). 3-hour average
combustion
temperature at or
above the
temperature limit.
------------------------------------------------------------------------
2. Catalytic oxidizer....... a. The average i. Collecting the
temperature temperature data
measured just according to Sec.
before the catalyst 63.9306(c);
bed in any 3-hour ii. Reducing the
period must not data to 3-hour
fall below the block averages; and
limit established iii. Maintaining the
according to Sec. 3-hour average
63.9324(b). temperature before
the catalyst bed at
or above the
temperature limit.
[[Page 43]]
b. Either ensure i. Either collecting
that the average the temperature
temperature data according to
difference across Sec. 63.9306(c),
the catalyst bed in reducing the data
any 3-hour period to 3-hour block
does not fall below averages, and
the temperature maintaining the 3-
difference limit hour average
established temperature
according to Sec. difference at or
63.9324(b)(2) or above the
develop and temperature
implement an difference limit;
inspection and or
maintenance plan ii. Complying with
according to Sec. the inspection and
63.9324(b)(3) and maintenance plan
(4). developed according
to Sec.
63.9324(b)(3) and
(4).
------------------------------------------------------------------------
3. Emission capture system a. The direction of i. Collecting the
that is a PTE according to the air flow at all direction of air
Sec. 63.9322(a). times must be into flow; and either
the enclosure; and the facial velocity
either of air through all
natural draft
openings according
to Sec.
63.9306(d)(1) or
the pressure drop
across the
enclosure according
to Sec.
63.9306(d)(2); and
ii. Maintaining the
facial velocity of
air flow through
all natural draft
openings or the
pressure drop at or
above the facial
velocity limit or
pressure drop
limit, and
maintaining the
direction of air
flow into the
enclosure at all
times.
b. The average Follow the
facial velocity of requirements in 3ai
air through all and ii of this
natural draft table.
openings in the
enclosure must be
at least 200 feet
per minute; or
c. The pressure drop Follow the
across the requirements in 3ai
enclosure must be and ii of this
at least 0.007 inch table.
H2O, as established
in Method 204 of
appendix M to 40
CFR part 51.
------------------------------------------------------------------------
4. Emission capture system a. The average gas i. Collecting the
that is not a PTE according volumetric flow gas volumetric flow
to Sec. 63.9322(a). rate or duct static rate or duct static
pressure in each pressure for each
duct between a capture device
capture device and according to Sec.
add-on control 63.9306(d);
device inlet in any ii. Reducing the
3-hour period must data to 3-hour
not fall below the block averages; and
average volumetric iii. Maintaining the
flow rate or duct 3-hour average gas
static pressure volumetric flow
limit established rate or duct static
for that capture pressure for each
device according capture device at
Sec. 63.9306(d). or above the gas
volumetric flow
rate or duct static
pressure limit.
------------------------------------------------------------------------
Table 3 to Subpart PPPPP of Part 63--Requirements for Initial Compliance
Demonstrations
As stated in Sec. 63.9321, you must demonstrate initial compliance
with each emission limitation that applies to you according to the
following table:
----------------------------------------------------------------------------------------------------------------
According to the
For each new or reconstructed You must . . . Using . . . following requirements
affected source complying with . . . . . .
----------------------------------------------------------------------------------------------------------------
1. The CO or THC outlet concentration a. Demonstrate CO or i. EPA Methods 3A and You must demonstrate
emission limitation. THC emissions are 20 10 of appendix A to 40 that the outlet
ppmvd or less. CFR part 60 for CO concentration of CO or
measurement or EPA THC emissions from the
Method 25A of appendix test cell/stand or
A to 40 CFR part 60 emission control
for THC measurement; device is 20 ppmvd or
or less, corrected to 15
percent O2 content,
using the first 4-hour
rolling average after
a successful
performance
evaluation.
[[Page 44]]
ii. A CEMS for CO or This demonstration is
THC and O2 at the conducted immediately
outlet of the engine following a successful
test cell/stand or performance evaluation
emission control of the CEMS as
device. required in Sec.
63.9320(b). The
demonstration consists
of the first 4-hour
rolling average of
measurements. The CO
or THC concentration
must be corrected to
15 percent O2 content,
dry basis using
Equation 1 in Sec.
63.9320.
----------------------------------------------------------------------------------------------------------------
2. The CO or THC percent reduction a. Demonstrate a i. You must conduct an You must demonstrate
emission limitation. reduction in CO or THC initial performance that the reduction in
of 96 percent or more. test to determine the CO or THC emissions is
capture and control at least 96 percent
efficiencies of the using the first 4-hour
equipment and to rolling average after
establish operating a successful
limits to be achieved performance
on a continuous basis; evaluation. Your inlet
or and outlet
measurements must be
on a dry basis and
corrected to 15
percent O2 content.
ii. A CEMS for CO or This demonstration is
THC and O2 at both the conducted immediately
inlet and outlet of following a successful
the emission control performance evaluation
device. of the CEMS as
required in Sec.
63.9320(b). The
demonstration consists
of the first 4-hour
rolling average of
measurements. The
inlet and outlet CO or
THC concentrations
must be corrected to
15 percent O2 content
using Equation 1 in
Sec. 63.9320. The
reduction in CO or THC
is calculated using
Equation 2 in Sec.
63.9320.
----------------------------------------------------------------------------------------------------------------
Table 4 to Subpart PPPPP of Part 63--Initial Compliance With Emission
Limitations
As stated in Sec. 63.9330, you must demonstrate initial compliance
with each emission limitation that applies to you according to the
following table:
------------------------------------------------------------------------
You have demonstrated initial
For the . . . compliance if . . .
------------------------------------------------------------------------
1. CO or THC concentration emission The first 4-hour rolling
limitation. average CO or THC
concentration is 20 ppmvd or
less, corrected to 15 percent
O2 content.
------------------------------------------------------------------------
2. CO or THC percent reduction emission The first 4-hour rolling
limitation. average reduction in CO or THC
is 96 percent or more, dry
basis, corrected to 15 percent
O2 content.
------------------------------------------------------------------------
Table 5 to Subpart PPPPP of Part 63--Continuous Compliance with Emission
Limitations
As stated in Sec. 63.9340, you must demonstrate continuous
compliance with each emission limitation that applies to you according
to the following table:
[[Page 45]]
------------------------------------------------------------------------
For the . . . You must . . . By . . .
------------------------------------------------------------------------
1. CO or THC concentration a. Demonstrate CO or i. Collecting the
emission limitation. THC emissions are CPMS data according
20 ppmvd or less to Sec.
over each 4-hour 63.9306(a),
rolling averaging reducing the
period. measurements to 1-
hour averages; or
ii. Collecting the
CEMS data according
to Sec.
63.9307(a),
reducing the
measurements to 1-
hour averages,
correcting them to
15 percent O2
content, dry basis,
according to Sec.
63.9320;
------------------------------------------------------------------------
2. CO or THC percent a. Demonstrate a i. Collecting the
reduction emission reduction in CO or CPMS data according
limitation. THC of 96 percent to Sec.
or more over each 4- 63.9306(a),
hour rolling reducing the
averaging period. measurements to 1-
hour averages; or
ii. Collecting the
CEMS data according
to Sec.
63.9307(b),
reducing the
measurements to 1-
hour averages,
correcting them to
15 percent O2
content, dry basis,
calculating the CO
or THC percent
reduction according
to Sec. 63.9320.
------------------------------------------------------------------------
Table 6 to Subpart PPPPP of Part 63--Requirements for Reports
As stated in Sec. 63.9350, you must submit each report that applies
to you according to the following table:
------------------------------------------------------------------------
If you own or operate a new
or reconstructed affected
source that must comply with The report must You must submit the
emission limitations, you contain . . . report . . .
must submit a . . .
------------------------------------------------------------------------
1. Compliance report........ a. If there are no Semiannually,
deviations from the according to the
emission requirements in
limitations that Sec. 63.9350.
apply to you, a
statement that
there were no
deviations from the
emission
limitations during
the reporting
period.
b. If there were no Semiannually,
periods during according to the
which the CEMS or requirements in
CPMS were out of Sec. 63.9350.
control as
specified in Sec.
63.8(c)(7), a
statement that
there were no
periods during
which the CEMS or
CPMS was out of
control during the
reporting period.
c. If you have a Semiannually,
deviation from any according to the
emission limitation requirements in
during the Sec. 63.9350.
reporting period,
the report must
contain the
information in Sec.
63.9350(c).
d. If there were Semiannually,
periods during according to the
which the CEMS or requirements in
CPMS were out of Sec. 63.9350.
control, as
specified in Sec.
63.8(c)(7), that
report must contain
the information in
Sec. 63.9350(d).
e. If you had an SSM Semiannually,
of a control device according to the
or associated requirements in
monitoring Sec. 63.9350.
equipment during
the reporting
period, the report
must include the
information in Sec.
63.10(d)(5)(i).
------------------------------------------------------------------------
Table 7 to Subpart PPPPP of Part 63--Applicability of General Provisions
to Subpart PPPPP
As stated in 63.9365, you must comply with the General Provisions in
Sec. Sec. 63.1 through 63.15 that apply to you according to the
following table:
----------------------------------------------------------------------------------------------------------------
Applies to subpart
Citation Subject Brief description PPPPP
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(1).................... Applicability.......... General applicability Yes. Additional terms
of the General defined in Sec.
Provisions. 63.9375.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(2)-(4)................ Applicability.......... Applicability of source Yes.
categories.
----------------------------------------------------------------------------------------------------------------
[[Page 46]]
Sec. 63.1(a)(5).................... [Reserved].............
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(6)-(7)................ Applicability.......... Contact for source Yes.
category information;
extension of
compliance through
early reduction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(8).................... Applicability.......... Establishment of State No. Refers to State
rules or programs. programs.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(9).................... [Reserved].............
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(10)-(14).............. Applicability.......... Explanation of time Yes.
periods, postmark
deadlines.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(b)(1).................... Applicability.......... Initial applicability.. Yes. Subpart PPPPP
clarifies
applicability at Sec.
63.9285.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(b)(2).................... Applicability.......... Title V operating Yes. All major affected
permit-reference to sources are required
part 70. to obtain a Title V
permit.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(b)(3).................... Applicability.......... Record of applicability Yes.
determination.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(c)(1).................... Applicability.......... Applicability after Yes. Subpart PPPPP
standards are set. clarifies the
applicability of each
paragraph of subpart A
to sources subject to
subpart PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(c)(2).................... Applicability.......... Title V permit No. Area sources are
requirement for area not subject to subpart
sources. PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(c)(3).................... [Reserved].............
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(c)(4).................... Applicability.......... Extension of compliance No. Existing sources
for existing sources. are not covered by the
substantive control
requirements of
subpart PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(c)(5).................... Applicability.......... Notification Yes.
requirements for an
area source becoming a
major source.
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(d)....................... [Reserved].............
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(e)....................... Applicability.......... Applicability of permit Yes.
program before a
relevant standard has
been set.
----------------------------------------------------------------------------------------------------------------
Sec. 63.2.......................... Definitions............ Definitions for Part 63 Yes. Additional
standards. definitions are
specified in Sec.
63.9375.
----------------------------------------------------------------------------------------------------------------
Sec. 63.3.......................... Units and Abbreviations Units and abbreviations Yes.
for Part 63 standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.4.......................... Prohibited Activities.. Prohibited activities; Yes.
compliance date;
circumvention,
severability.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(a)....................... Construction/ Construction and Yes.
Reconstruction. reconstruction--applic
ability.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(b)(1).................... Construction/ Requirements upon Yes.
Reconstruction. construction or
reconstruction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(b)(2).................... [Reserved].
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(b)(3).................... Construction/ Approval of Yes.
Reconstruction. construction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(b)(4).................... Construction/ Notification of Yes.
Reconstruction. construction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(b)(5).................... Construction/ Compliance............. Yes.
Reconstruction.
----------------------------------------------------------------------------------------------------------------
[[Page 47]]
Sec. 63.5(b)(6).................... Construction/ Addition of equipment.. Yes.
Reconstruction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(c)....................... [Reserved]
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(d)....................... Construction/ Application for Yes.
Reconstruction. construction
reconstruction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(e)....................... Construction/ Approval of Yes.
Reconstruction. construction or
reconstruction.
----------------------------------------------------------------------------------------------------------------
Sec. 63.5(f)....................... Construction/ Approval of Yes.
Reconstruction. construction or
reconstruction based
on prior State review.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(a)....................... Applicability.......... Applicability of Yes.
standards and
monitoring
requirements.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(b)(1)-(2)................ Compliance Dates for Standards apply at Yes.
New and Reconstructed effective date; 3
Sources. years after effective
date; upon startup; 10
years after
construction or
reconstruction
commences for 112(f).
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(b)(3).................... Compliance Dates for Compliance dates for No. Compliance is
New and Reconstructed sources constructed or required by startup or
Sources. reconstructed before effective date.
effective date.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(b)(4).................... Compliance Dates for Compliance dates for Yes.
New and Reconstructed sources also subject
Sources. to Sec. 112(f)
standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(b)(5).................... Compliance Dates for Notification........... Yes.
New and Reconstructed
Sources.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(b)(6).................... [Reserved].
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(b)(7).................... Compliance Dates for Compliance dates for Yes.
New and Reconstructed new and reconstructed
Sources. area sources that
become major.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(c)(1)-(2)................ Compliance Dates for Effective date No. Existing sources
Existing Sources. establishes compliance are not covered by the
date. substantive control
requirements of
subpart PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(c)(3)-(4)................ [Reserved].
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(c)(5).................... Compliance Dates for Compliance dates for Yes. If the area source
Existing Sources. existing area sources become a major source
that becomes major. by addition or
reconstruction, the
added or reconstructed
portion will be
subject to subpart
PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(d)....................... [Reserved].
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(e)(1)-(2)................ Operation and Operation and Yes. Except that you
Maintenance maintenance. are not required to
Requirements. have an SSMP for
control devices and
associated monitoring
equipment.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(e)(3).................... SSMP................... 1. Requirement for SSM Yes.You must develop an
and SSMP. SSMP for each control
2. Content of SSMP..... device and associated
monitoring equipment.
----------------------------------------------------------------------------------------------------------------
[[Page 48]]
Sec. 63.6(f)(1).................... Compliance Except You must comply with Yes, but you must
During SSM. emission standards at comply with emission
all times except standards at all times
during SSM of control except during SSM of
devices or associated control devices and
monitoring equipment. associated monitoring
equipment only.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(f)(2)-(3)................ Methods for Determining Compliance based on Yes.
Compliance. performance test,
operation and
maintenance plans,
records, inspection.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(g)(1)-(3)................ Alternative Standard... Procedures for getting Yes.
an alternative
standard.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(h)....................... Opacity/Visible Requirements for No. Subpart PPPPP does
Emission (VE) opacity/VE standards. not establish opacity/
Standards. VE standards and does
not require continuous
opacity monitoring
systems (COMS).
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(i)(1)-(14)............... Compliance Extension... Procedures and criteria No. Compliance
for Administrator to extension provisions
grant compliance apply to existing
extension. sources, which do not
have emission
limitations in subpart
PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.6(j)....................... Presidential Compliance President may exempt Yes.
Exemption. source category from
requirement to comply
with rule.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(a)(1)-(2)................ Performance Test Dates. Dates for conducting Yes.
initial performance
testing and other
compliance
demonstrations: Must
conduct within 180
days after first
subject to rule.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(a)(3).................... Section 114 Authority.. Administrator may Yes.
require a performance
test under CAA Section
114 at any time.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(b)(1).................... Notification Must notify Yes.
Performance Test. Administrator 60 days
before the test.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(b)(2).................... Notification of If have to reschedule Yes.
Rescheduling. performance test, must
notify Administrator 5
days before schedule
date of rescheduled
date.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(c)....................... Quality Assurance/Test 1. Requirement to Yes.
Plan. submit site-specific
test plan 60 days
before the test or on
date Administrator
agrees with.
2. Test plan approval Yes.
procedures.
3. Performance audit Yes.
requirements.
4. Internal and Yes.
external QA procedures
for testing.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(d)....................... Testing Facilities..... Requirements for Yes.
testing facilities.
----------------------------------------------------------------------------------------------------------------
[[Page 49]]
Sec. 63.7(e)(1).................... Conditions for Performance tests must Yes.
Conducting Performance be conducted under
Tests. representative
conditions; cannot
conduct performance
tests during SSM; not
a violation to exceed
standard during SSM.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(e)(2).................... Conditions for Must conduct according Yes.
Conducting Performance to rule and EPA test
Tests. methods unless
Administrator approves
alternative.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(e)(3).................... Test Run Duration...... 1. Must have three test Yes.
runs of at least 1
hour each.
2. Compliance is based Yes.
on arithmetic mean of
three runs.
3. Conditions when data Yes.
from an additional
test run can be used.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(e)(4).................... Other Performance Administrator may Yes.
Testing. require other testing
under section 114 of
the CAA.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(f)....................... Alternative Test Method Procedures by which Yes.
Administrator can
grant approval to use
an alternative test
method.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(g)....................... Performance Test Data 1. Must include raw Yes.
Analysis. data in performance
test report.
2. Must submit Yes.
performance test data
60 days after end of
test with the
Notification of
Compliance Status.
3. Keep data for 5 Yes.
years.
----------------------------------------------------------------------------------------------------------------
Sec. 63.7(h)....................... Waiver of Tests........ Procedures for Yes.
Administrator to waive
performance test.
Sec. 63.8(a)(1).................... Applicability of Subject to all Yes. Subpart PPPPP
Monitoring monitoring contains specific
Requirements. requirements in requirements for
standard. monitoring at Sec.
63.9325.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(a)(2).................... Performance Performance Yes.
Specifications. Specifications in
appendix B of part 60
apply.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(a)(3).................... [Reserved]
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(a)(4).................... Monitoring with Flares. Unless your rule says No. Subpart PPPPP does
otherwise, the not have monitoring
requirements for requirements for
flares in 63.11 apply. flares.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(b)(1).................... Monitoring............. Must conduct monitoring Yes.
according to standard
unless Administrator
approves alternative.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(b)(2)-(3)................ Multiple Effluents and 1. Specific Yes.
Multiple Monitoring requirements for
Systems. installing monitoring
systems.
2. Must install on each Yes.
effluent before it is
combined and before it
is released to the
atmosphere unless
Administrator approves
otherwise.
[[Page 50]]
3. If more than one Yes.
monitoring system on
an emission point,
must report all
monitoring system
results, unless one
monitoring system is a
backup.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(1).................... Monitoring System Maintain monitoring Yes.
Operation and system in a manner
Maintenance. consistent with good
air pollution control
practices.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(1)(i)................. Routine and predictable 1. Keep parts for Yes.
CMS malfunctions. routine repairs of CMS
readily available.
2. Reporting
requirements for SSM
when action is
described in SSMP.
3. Reporting Yes.
requirements for SSM
when action is
described in SSMP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(1)(ii)................ SSM of CMS Not in SSMP. Reporting requirements Yes.
for SSM of CMS when
action is not
described in SSMP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(1)(iii)............... Compliance with 1. How Administrator Yes.
Operation and determines if source
Maintenance complying with
Requirements. operation and
maintenance
requirements.
2. Review of source O&M
procedures, records,
manufacturer's
instructions and
recommendations, and
inspection.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(2)-(3)................ Monitoring System 1. Must install to get Yes.
Installation. representative
emission of parameter
measurements.
2. Must verify Yes.
operational status
before or at
performance test.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(4).................... Continuous Monitoring 1. CMS must be No. Follow specific
System (CMS) operating except requirements in Sec.
Requirements. during breakdown, out 63.9335(a) and (b) of
of control, repair, subpart PPPPP.
maintenance, and high-
level calibration
drifts.
2. COMS must have a No. Follow specific
minimum of one cycle requirements in Sec.
of sampling and 63.9335(a) and (b) of
analysis for each subpart PPPP.
successive 10-second
period and one cycle
of data recording for
each successive 6-
minute period.
3. CEMS must have a No. Follow specific
minimum of one cycle requirements in Sec.
of operation for each 63.9335(a) and (b) of
successive 15-minute subpart PPPPP.
period.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(5).................... COMS Minimum Procedures COMS minimum procedures No. Subpart PPPPP does
not have opacity/VE
standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(c)(6)-(8)................ CMS Requirements....... Zero and high-level Yes. Except that PPPP
calibration check does not require COMS.
requirements, out-of-
control periods.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(d)....................... CMS Quality Control.... 1. Requirements for CMS Yes.
quality control,
including calibration,
etc.
[[Page 51]]
2. Must keep quality Yes.
control plan on record
for 5 years. Keep old
versions for 5 years
after revisions.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(e)....................... CMS Performance Notification, Yes. Except for Sec.
Evaluation. performance evaluation 63.8(e)(5)(ii), which
test plan, reports. applies to COMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(f)(1)-(5)................ Alternative Monitoring Procedures for Yes.
Method. Administrator to
approve alternative
monitoring.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(f)(6).................... Alternative to Relative Procedures for Yes.
Accuracy Test. Administrator to
approve alternative
relative accuracy
tests for CEMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(g)....................... Data Reduction......... 1. COMS 6-minute Yes. Except that
averages calculated provisions for COMS
over at least 36 are not applicable.
evenly spaced data Averaging periods for
points. demonstrating
2. CEMS 1-hour averages compliance are
computed over at least specified at Sec.
4 equally spaced data 63.9340.
points.
----------------------------------------------------------------------------------------------------------------
Sec. 63.8(g)(5).................... Data Reduction......... Data that cannot be No. Specific language
used in computing is located at Sec.
averages for CEMS and 63.9335(a).
COMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(a)....................... Notification Applicability and State Yes.
Requirements. delegation.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(b)(1)-(5)................ Initial Notifications.. 1. Submit notification Yes.
subject 120 days after
effective date.
2. Notification of Yes.
intent to construct/
reconstruct;
notification of
commencement of
construct/
reconstruct;
notification of
startup.
3. Contents of each.... Yes.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(c)....................... Request for Compliance Can request if cannot No. Compliance
Extension. comply by date or if extensions do not
installed BACT/LAER. apply to new or
reconstructed sources.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(d)....................... Notification of Special For sources that Yes.
Compliance commence construction
Requirements for New between proposal and
Source. promulgation and want
to comply 3 years
after effective date.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(e)....................... Notification of Notify Administrator 60 No. Subpart PPPPP does
Performance Test. days prior. not require
performance testing.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(f)....................... Notification of Opacity/ Notify Administrator 30 No. Subpart PPPPP does
VE Test. days prior. not have opacity/VE
standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(g)(1).................... Additional Notification of Yes.
Notifications when performance evaluation.
Using CMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(g)(2).................... Additional Notification of use of No. Subpart PPPPP does
Notifications when COMS data. not contain opacity or
Using CMS. VE standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(g)(3).................... Additional Notification that Yes. If alternative is
Notifications when exceeded criterion for in use.
Using CMS. relative accuracy.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(h)(1)-(6)................ Notification of 1. Contents............ Yes.
Compliance Status.
[[Page 52]]
2. Due 60 days after Yes.
end of performance
test or other
compliance
demonstration, except
for opacity/VE, which
are due 30 days after.
3. When to submit to Yes.
Federal vs. State
authority.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(i)....................... Adjustment of Submittal Procedures for Yes.
Deadlines. Administrator to
approve change in when
notifications must be
submitted.
----------------------------------------------------------------------------------------------------------------
Sec. 63.9(j)....................... Change in Previous Must submit within 15 Yes.
Information. days after the change.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(a)...................... Recordkeeping/Reporting 1. Applies to all, Yes.
unless compliance
extension.
2. When to submit to Yes.
Federal vs. State
authority.
3. Procedures for Yes.
owners of more than
one source.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(1)................... Recordkeeping/Reporting 1. General requirements Yes.
2. Keep all records Yes.
readily available.
3. Keep for 5 years.... Yes.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(2)(i)-(v)............ Records Related to SSM. 1. Occurrence of each Yes.
of operation (process
equipment).
2. Occurrence of each Yes.
malfunction of air
pollution equipment.
3. Maintenance on air Yes.
pollution control
equipment.
4. Actions during SSM.. Yes.
5. All information Yes.
necessary to
demonstrate
conformance with the
SSMP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(2)(vi)-(xi).......... CMS Records............ Malfunctions, Yes.
inoperative, out of
control.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(2)(xii).............. Records................ Records when under Yes.
waiver.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(2)(xiii)............. Records................ Records when using Yes.
alternative to
relative accuracy test.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(2)(xiv).............. Records................ All documentation Yes.
supporting initial
notification and
notification of
compliance status.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(b)(3)................... Records................ Applicability Yes.
determinations.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(c)(1)-(6), (9)-(15)..... Records................ Additional records for Yes.
CEMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(c)(7)-(8)............... Records................ Records of excess No. Specific language
emissions and is located at Sec.
parameter monitoring 63.9355 of subpart
exceedances for CMS. PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(d)(1)................... General Reporting Requirement to report.. Yes.
Requirements.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(d)(2)................... Report of Performance When to submit to Yes.
Test Results. Federal or State
authority.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(d)(3)................... Reporting Opacity or VE What to report and when No. Subpart PPPPP does
Observations. not have opacity/VE
standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(d)(4)................... Progress Reports....... Must submit progress No. Compliance
reports on schedule if extensions do not
under compliance apply to new or
extension. reconstructed sources.
----------------------------------------------------------------------------------------------------------------
[[Page 53]]
Sec. 63.10(d)(5)................... SSM Reports............ Contents and submission Yes.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(e)(1) and (2)(i)........ Additional CMS Reports. Additional CMS reports. Yes.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(e)(2)(ii)............... Additional CMS Reports. COMS-related report.... No. Subpart PPPPP does
not require COMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(e)(3)................... Additional CMS Reports. Excess emissions and No. Specific language
parameter exceedances is located in Sec.
reports. 63.9350 of subpart
PPPPP.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(e)(4)................... Additional CMS Reports. Reporting COMS data.... No. Subpart PPPPP does
not require COMS.
----------------------------------------------------------------------------------------------------------------
Sec. 63.10(f)...................... Waiver for Procedures for Yes.
Recordkeeping/ Administrator to waive.
Reporting.
----------------------------------------------------------------------------------------------------------------
Sec. 63.11......................... Control Device Requirements for flares No. Subpart PPPPP does
Requirements. not specify use of
flares for compliance.
----------------------------------------------------------------------------------------------------------------
Sec. 63.12......................... State Authority and State authority to Yes.
Delegations. enforce standards.
----------------------------------------------------------------------------------------------------------------
Sec. 63.13......................... Addresses of State Air Addresses where Yes.
Pollution Control reports,
Offices and EPA notifications, and
Regional Offices. requests are sent.
----------------------------------------------------------------------------------------------------------------
Sec. 63.14......................... Incorporations by Test methods Yes. ASTM D 6522-00 and
Reference. incorporated by ANSI/ASME PTC 19.10-
reference. 1981 (incorporated by
reference-See Sec.
63.14).
----------------------------------------------------------------------------------------------------------------
Sec. 63.15......................... Availability of Public and confidential Yes.
Information and information.
Confidentiality.
----------------------------------------------------------------------------------------------------------------
[68 FR 28785, May 27, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Subpart QQQQQ_National Emission Standards for Hazardous Air Pollutants
for Friction Materials Manufacturing Facilities
Source: 67 FR 64506, Oct. 18, 2002, unless otherwise noted.
What This Subpart Covers
Sec. 63.9480 What is the purpose of this subpart?
This subpart establishes national emission standards for hazardous
air pollutants (NESHAP) for friction materials manufacturing facilities
that use a solvent-based process. This subpart also establishes
requirements to demonstrate initial and continuous compliance with all
applicable emission limitations in this subpart.
Sec. 63.9485 Am I subject to this subpart?
(a) You are subject to this subpart if you own or operate a friction
materials manufacturing facility (as defined in Sec. 63.9565) that is
(or is part of) a major source of hazardous air pollutants (HAP)
emissions on the first compliance date that applies to you, as specified
in Sec. 63.9495. Your friction materials manufacturing facility is a
major source of HAP if it emits or has the potential to emit any single
HAP at a rate of 9.07 megagrams (10 tons) or more per year or any
combination of HAP at a rate of 22.68 megagrams (25 tons) or more per
year.
(b) The requirements in this subpart do not apply to research and
development facilities, as defined in section 112(c)(7) of the Clean Air
Act.
Sec. 63.9490 What parts of my plant does this subpart cover?
(a) This subpart applies to each new, reconstructed, or existing
affected source at your friction materials manufacturing facility.
[[Page 54]]
(b) The affected source covered by this subpart is each new,
reconstructed, or existing solvent mixer (as defined in Sec. 63.9565)
at your friction materials manufacturing facility.
(c) A solvent mixer at your friction materials manufacturing
facility is new if you commence construction of the solvent mixer after
October 18, 2002. An affected source is reconstructed if it meets the
definition of ``reconstruction'' in Sec. 63.2, and reconstruction is
commenced after October 18, 2002.
(d) A solvent mixer at your friction materials manufacturing
facility is existing if it is not new or reconstructed.
Sec. 63.9495 When do I have to comply with this subpart?
(a) If you have an existing solvent mixer, you must comply with each
of the requirements for existing sources no later than October 18, 2005.
(b) If you have a new or reconstructed solvent mixer and its initial
startup date is after October 18, 2002, you must comply with the
requirements for new and reconstructed sources upon initial startup.
(c) If your friction materials manufacturing facility is an area
source that increases its emissions or its potential to emit such that
it becomes a (or part of a) major source of HAP emissions, then
paragraphs (c)(1) and (2) of this section apply.
(1) For any portion of the area source that becomes a new or
reconstructed affected source, you must comply with the requirements for
new and reconstructed sources upon startup or no later than October 18,
2002, whichever is later.
(2) For any portion of the area source that becomes an existing
affected source, you must comply with the requirements for existing
sources no later than 1 year after the area source becomes a major
source or no later than October 18, 2005, whichever is later.
(d) You must meet the notification and schedule requirements in
Sec. 63.9535. Several of the notifications must be submitted before the
compliance date for your affected source.
Emission Limitations
Sec. 63.9500 What emission limitations must I meet?
(a) For each new, reconstructed, or existing large solvent mixer at
your friction materials manufacturing facility, you must limit HAP
solvent emissions to the atmosphere to no more than 30 percent of that
which would otherwise be emitted in the absence of solvent recovery and/
or solvent substitution, based on a 7-day block average.
(b) For each new, reconstructed, or existing small solvent mixer at
your friction materials manufacturing facility, you must limit HAP
solvent emissions to the atmosphere to no more than 15 percent of that
which would otherwise be emitted in the absence of solvent recovery and/
or solvent substitution, based on a 7-day block average.
General Compliance Requirements
Sec. 63.9505 What are my general requirements for complying with this
subpart?
(a) You must be in compliance with the emission limitation in this
subpart at all times, except during periods of startup, shutdown, or
malfunction.
(b) You must always operate and maintain your affected source,
including air pollution control and monitoring equipment, according to
the provisions in Sec. 63.6(e)(1)(i).
(c) You must develop a written startup, shutdown, and malfunction
plan according to the provisions in Sec. 63.6(e)(3).
[67 FR 64506, Oct. 18, 2002, as amended at 71 FR 20470, Apr. 20, 2006]
Initial Compliance Demonstration Requirements
Sec. 63.9510 By what date must I conduct my initial compliance
demonstration?
(a) If you use a solvent recovery system and/or solvent
substitution, you must conduct your initial compliance demonstration
within 7 calendar days after the compliance date that is specified for
your source in Sec. 63.9495.
(b) If you use a control technique other than a solvent recovery
system and/or solvent substitution, you must comply with the provisions
in Sec. 63.9570.
[[Page 55]]
Sec. 63.9515 How do I demonstrate initial compliance with the emission
limitation that applies to me?
(a) You have demonstrated initial compliance for each new,
reconstructed, or existing large solvent mixer subject to the emission
limitation in Sec. 63.9500(a) if the HAP solvent discharged to the
atmosphere during the first 7 days after the compliance date, determined
according to the provisions in Sec. 63.9520, does not exceed a 7-day
block average of 30 percent of that which would otherwise be emitted in
the absence of solvent recovery and/or solvent substitution.
(b) You have demonstrated initial compliance for each new,
reconstructed, or existing small solvent mixer subject to the emission
limitation in Sec. 63.9500(b) if the HAP solvent discharged to the
atmosphere during the first 7 days after the compliance date, determined
according to the provisions in Sec. 63.9520, does not exceed a 7-day
block average of 15 percent of that which would otherwise be emitted in
the absence of solvent recovery and/or solvent substitution.
(c) You must submit a notification of compliance status containing
the results of the initial compliance demonstration according to Sec.
63.9535(e).
Sec. 63.9520 What procedures must I use to demonstrate initial
compliance?
(a) If you use a solvent recovery system, you must use the
procedures in paragraphs (a)(1) through (8) of this section to
demonstrate initial compliance with the emission limitations in Sec.
63.9500(a) and (b).
(1) Record the date and time of each mix batch.
(2) Record the identity of each mix batch using a unique batch ID,
as defined in Sec. 63.9565.
(3) Measure and record the weight of HAP solvent loaded into the
solvent mixer for each mix batch.
(4) Measure and record the weight of HAP solvent recovered for each
mix batch.
(5) If you use a solvent recovery system, you must determine the
percent of HAP solvent discharged to the atmosphere for each mix batch
according to Equation 1 of this section as follows:
(Eq. 1)
[GRAPHIC] [TIFF OMITTED] TR18OC02.002
Where:
Pb = Percent of HAP solvent discharged to the atmosphere for
each mix batch, percent;
Srec = Weight of HAP solvent recovered for each mix batch,
lb;
Smix = Weight of HAP solvent loaded into the solvent mixer
for each mix batch, lb.
(6) If you use solvent substitution for a mix batch, you must record
the use of a non-HAP material as a substitute for a HAP solvent for that
mix batch and assign a value of 0 percent to the percent of HAP solvent
discharged to the atmosphere for that mix batch (Pb).
(7) Determine the 7-day block average percent of HAP solvent
discharged to the atmosphere according to Equation 2 of this section as
follows:
[GRAPHIC] [TIFF OMITTED] TR18OC02.003
Where:
%P7 = 7-day block average percent of HAP solvent discharged
to the atmosphere, percent;
i = mix batch;
n = number of mix batches in 7-day block average.
(8) Have valid data for at least 90 percent of the mix batches over
the 7-day averaging period.
(b) If you use a control technique other than a solvent recovery
system and/or solvent substitution, you may apply to EPA for approval to
use an alternative method of demonstrating compliance with the emission
limitations for solvent mixers in Sec. 63.9500(a) and (b), as provided
in Sec. 63.9570.
Sec. 63.9525 What are the installation, operation, and maintenance
requirements for my weight measurement device?
(a) If you use a solvent recovery system, you must install, operate,
and maintain a weight measurement device to measure the weight of HAP
solvent loaded into the solvent mixer and the weight of HAP solvent
recovered for each mix batch.
[[Page 56]]
(b) For each weight measurement device required by this section, you
must develop and submit for approval a site-specific monitoring plan
that addresses the requirements of paragraphs (b)(1) through (6) of this
section:
(1) Procedures for installing the weight measurement device;
(2) The minimum accuracy of the weight measurement device in pounds
and as a percent of the average weight of solvent to be loaded into the
solvent mixer;
(3) Site-specific procedures for how the measurements will be made;
(4) How the measurement data will be recorded, reduced, and stored;
(5) Procedures and acceptance criteria for calibration of the weight
measurement device; and
(6) How the measurement device will be maintained, including a
routine maintenance schedule and spare parts inventory list.
(c) The site-specific monitoring plan required in paragraph (b) of
this section must include, at a minimum, the requirements of paragraphs
(c)(1) through (3) of this section:
(1) The weight measurement device must have a minimum accuracy of
0.05 kilograms (0.1 pounds)
or 1 percent of the average weight of solvent to
be loaded into the solvent mixer, whichever is greater.
(2) An initial multi-point calibration of the weight measurement
device must be made using 5 points spanning the expected range of weight
measurements before the weight measurement device can be used. The
manufacturer's calibration results can be used to meet this requirement.
(3) Once per day, an accuracy audit must be made using a single
Class F calibration weight that corresponds to 20 to 80 percent of the
average weight of solvent to be loaded into the solvent mixer. If the
weight measurement device cannot reproduce the value of the calibration
weight within 0.05 kilograms (0.1 pounds) or
1 percent of the average weight of solvent to be
loaded into the solvent mixer, whichever is greater, the scale must be
recalibrated before being used again. The recalibration must be
performed with at least five Class F calibration weights spanning the
expected range of weight measurements.
(d) You must operate and maintain the weight measurement device
according to the site-specific monitoring plan.
(e) You must maintain records of all maintenance activities,
calibrations, and calibration audits.
Continuous Compliance Requirements
Sec. 63.9530 How do I demonstrate continuous compliance with the emission
limitation that applies to me?
(a) If you use a solvent recovery system and/or solvent
substitution, you must demonstrate continuous compliance with the
emission limitations for solvent mixers in Sec. 63.9500(a) and (b)
according to the provisions in paragraphs (a)(1) through (3) of this
section.
(1) Except for during malfunctions of your weight measurement device
and associated repairs, you must collect and record the information
required in Sec. 63.9520(a)(1) through (8) at all times that the
affected source is operating and record all information needed to
document conformance with these requirements.
(2) For new, reconstructed, or existing large solvent mixers,
maintain the 7-day block average percent of HAP solvent discharged to
the atmosphere at or below 30 percent of that which would otherwise be
emitted in the absence of solvent recovery and/or solvent substitution.
(3) For new, reconstructed, or existing small solvent mixers,
maintain the 7-day block average percent of HAP solvent discharged to
the atmosphere at or below 15 percent of that which would otherwise be
emitted in the absence of solvent recovery and/or solvent substitution.
(b) If you use a control technique other than a solvent recovery
system and/or solvent substitution, you must demonstrate continuous
compliance with the emission limitations for solvent mixers in Sec.
63.9500(a) and (b) according to the provisions in Sec. 63.9570.
(c) You must report each instance in which you did not meet the
emission limitations for solvent mixers in Sec. 63.9500(a) and (b).
This includes periods of startup, shutdown, or malfunction. These
instances are deviations
[[Page 57]]
from the emission limitations in this subpart. These deviations must be
reported according to the requirements in Sec. 63.9540.
(d) [Reserved]
(e) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations
that occur during a period of startup, shutdown, or malfunction are not
violations if you demonstrate to the Administrator's satisfaction that
you were operating in accordance with Sec. 63.6(e)(1). The
Administrator will determine whether deviations that occur during a
period of startup, shutdown, or malfunction are violations, according to
the provisions in Sec. 63.6(e).
[67 FR 64506, Oct. 18, 2002, as amended at 71 FR 20470, Apr. 20, 2006]
Notifications, Reports, and Records
Sec. 63.9535 What notifications must I submit and when?
(a) You must submit all of the notifications in Sec. Sec.
63.8(f)(4) and 63.9(b), (c), (d), and (h) that apply to you by the
specified dates.
(b) If you use a control technique other than a solvent recovery
system and/or solvent substitution, you must comply with the provisions
in Sec. 63.9570.
(c) As specified in Sec. 63.9(b)(2), if you start up your affected
source before October 18, 2002, you must submit your initial
notification no later than 120 calendar days after October 18, 2002.
(d) As specified in Sec. 63.9(b)(3), if you start up your new
affected source on or after October 18, 2002, you must submit your
initial notification no later than 120 calendar days after you become
subject to this subpart.
(e) You must submit a notification of compliance status according to
Sec. 63.9(h)(2)(ii). You must submit the notification of compliance
status before the close of business on the 30th calendar day following
the completion of the initial compliance demonstration.
Sec. 63.9540 What reports must I submit and when?
(a) Unless the Administrator has approved a different schedule, you
must submit each semiannual compliance report according to the
requirements in paragraphs (a)(1) through (5) of this section.
(1) The first compliance report must cover the period beginning on
the compliance date that is specified for your affected source in Sec.
63.9495 and ending on June 30 or December 31, whichever date comes first
after the compliance date that is specified for your source in Sec.
63.9495.
(2) The first compliance report must be postmarked or delivered no
later than July 31 or January 31, whichever date comes first after your
first compliance report is due.
(3) Each subsequent compliance report must cover the semiannual
reporting period from January 1 through June 30 or the semiannual
reporting period from July 1 through December 31.
(4) Each subsequent compliance report must be postmarked or
delivered no later than July 31 or January 31, whichever date comes
first after the end of the semiannual reporting period.
(5) For each affected source that is subject to permitting
regulations pursuant to 40 CFR part 70 or 71 of this chapter, and if the
permitting authority has established dates for submitting semiannual
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A) of this chapter, you may submit the first and
subsequent compliance reports according to the dates the permitting
authority has established instead of according to the dates in
paragraphs (a)(1) through (4) of this section.
(b) Each compliance report must include the information in
paragraphs (b)(1) through (3) of this section, and if applicable,
paragraphs (b)(4) through (6) of this section.
(1) Company name and address.
(2) Statement by a responsible official, with the official's name,
title, and signature, certifying that, based on information and belief
formed after reasonable inquiry, the statements and information in the
report are true, accurate, and complete.
(3) Date of report and beginning and ending dates of the reporting
period.
(4) If you had a startup, shutdown, or malfunction during the
reporting period and you took actions consistent with your startup,
shutdown, and malfunction plan, the compliance report
[[Page 58]]
must include the information in Sec. 63.10(d)(5)(i).
(5) If there were no deviations from the emission limitations for
solvent mixers in Sec. 63.9500(a) and (b), a statement that there were
no deviations from the emission limitations during the reporting period.
(6) If there were no periods during which a monitoring system was
out-of-control as specified in Sec. 63.8(c)(7), a statement that there
were no periods during which a monitoring system was out-of-control
during the reporting period.
(c) For each deviation from an emission limitation occurring at an
affected source, you must include the information in paragraphs (b)(1)
through (4) and (c)(1) and (2) of this section. This includes periods of
startup, shutdown, or malfunction.
(1) The total operating time of each affected source during the
reporting period.
(2) Information on the number, duration, and cause of deviations
(including unknown cause, if applicable), as applicable, and the
corrective action taken.
(d) If you had a startup, shutdown, or malfunction during the
semiannual reporting period that was not consistent with your startup,
shutdown, and malfunction plan, you must submit an immediate startup,
shutdown, and malfunction report according to the requirements in Sec.
63.10(d)(5)(ii).
(e) If you have obtained a title V operating permit for an affected
source pursuant to 40 CFR part 70 or 71 of this chapter, you must report
all deviations as defined in this subpart in the semiannual monitoring
report required by 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A) of this chapter. If you submit a compliance report
for an affected source along with, or as part of, the semiannual
monitoring report required by 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A) of this chapter, and the compliance report includes
all the required information concerning deviations from any emission
limitation in this subpart, then submission of the compliance report
satisfies any obligation to report the same deviations in the semiannual
monitoring report. However, submission of a compliance report does not
otherwise affect any obligation you may have to report deviations from
permit requirements to your permitting authority.
Sec. 63.9545 What records must I keep?
(a) You must keep the records in paragraphs (a)(1) and (2) of this
section that apply to you.
(1) A copy of each notification and report that you submitted to
comply with this subpart, including all documentation supporting any
initial notification or notification of compliance status that you
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
(2) The records in Sec. 63.6(e)(3)(iii) through (v) related to
startup, shutdown, or malfunction.
(b) You must keep the records required in Sec. 63.9525 to show
proper operation and maintenance of the weight measurement device.
(c) You must keep the records required in Sec. 63.9530 to show
continuous compliance with the emission limitations for solvent mixers
in Sec. 63.9500(a) and (b).
Sec. 63.9550 In what form and how long must I keep my records?
(a) You must keep your records in a form suitable and readily
available for expeditious review, according to Sec. 63.10(b)(1).
(b) As specified in Sec. 63.10(b)(1), you must keep each record for
5 years following the date of each occurrence, measurement, maintenance,
corrective action, report, or record.
(c) You must keep each record on site for at least 2 years after the
date of each occurrence, measurement, maintenance, corrective action,
report, or record, according to Sec. 63.10(b)(1). You can keep the
records offsite for the remaining 3 years.
Other Requirements and Information
Sec. 63.9555 What parts of the General Provisions apply to me?
Table 1 to this subpart shows which parts of the General Provisions
in Sec. Sec. 63.1 through 63.15 apply to you.
[[Page 59]]
Sec. 63.9560 Who implements and enforces this subpart?
(a) This subpart can be implemented and enforced by the U.S. EPA, or
a delegated authority such as your State, local, or tribal agency. If
the U.S. EPA Administrator has delegated authority to your State, local,
or tribal agency, then that agency, in addition to the U.S. EPA, has the
authority to implement and enforce this subpart. You should contact your
U.S. EPA Regional Office to find out if this subpart is delegated to
your State, local, or tribal agency.
(b) In delegating implementation and enforcement authority of this
subpart to a State, local, or tribal agency under 40 CFR part 63,
subpart E, the authorities contained in paragraphs (c)(1) through (4) of
this section are retained by the Administrator of the U.S. EPA and are
not transferred to the State, local, or tribal agency.
(c) The authorities that cannot be delegated to State, local or
tribal agencies are as follows:
(1) Approval of alternatives to the emission limitations in Sec.
63.9500(a) and (b) under Sec. 63.6(g).
(2) Approval of major alternatives to test methods under Sec.
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
(3) Approval of major alternatives to monitoring under Sec. 63.8(f)
and as defined in Sec. 63.90.
(4) Approval of major alternatives to recordkeeping and reporting
under Sec. 63.10(f) and as defined in Sec. 63.90.
Sec. 63.9565 What definitions apply to this subpart?
Terms used in this subpart are defined in the Clean Air Act, in
Sec. 63.2, and in this section as follows:
Batch ID means a unique identifier used to differentiate each
individual mix batch.
Deviation means any instance in which an affected source subject to
this subpart, or an owner or operator of such a source:
(1) Fails to meet any requirement or obligation established by this
subpart, including, but not limited to, any emission limitation
(including any operating limit);
(2) Fails to meet any term or condition that is adopted to implement
an applicable requirement in this subpart and that is included in the
operating permit for any affected source required to obtain such a
permit; or
(3) Fails to meet any emission limitation (including any operating
limit) in this subpart during startup, shutdown, or malfunction,
regardless of whether or not such failure is permitted by this subpart.
Friction ingredients means any of the components used in the
manufacture of friction materials, excluding the HAP solvent. Friction
ingredients include, but are not limited to, reinforcement materials,
property modifiers, resins, and other additives.
Friction materials manufacturing facility means a facility that
manufactures friction materials using a solvent-based process. Friction
materials are used in the manufacture of products used to accelerate or
decelerate objects. Products that use friction materials include, but
are not limited to, disc brake pucks, disc brake pads, brake linings,
brake shoes, brake segments, brake blocks, brake discs, clutch facings,
and clutches.
HAP solvent means a solvent that contains 10 percent or more of any
one HAP, as listed in section 112(b) of the Clean Air Act, or any
combination of HAP that is added to a solvent mixer. Examples include
hexane, toluene, and trichloroethylene.
Initial startup means the first time that equipment is put into
operation. Initial startup does not include operation solely for testing
equipment. Initial startup does not include subsequent startups (as
defined in this section) following malfunction or shutdowns or following
changes in product or between batch operations.
Large solvent mixer means a solvent mixer with a design capacity
greater than or equal to 2,000 pounds, including friction ingredients
and HAP solvent.
Mix batch means each batch of friction materials manufactured in a
solvent mixer.
Responsible official means responsible official as defined in Sec.
63.2.
7-day block average means an averaging technique for a weekly
compliance determination where the calculated values for percent HAP
solvent
[[Page 60]]
discharged to the atmosphere are averaged together for all mix batches
(for which there are valid data) in a 7-day block period according to
the equation provided in Sec. 63.9520(a)(6).
Small solvent mixer means a solvent mixer with a design capacity
less than 2,000 pounds, including friction ingredients and HAP solvent.
Solvent mixer means a mixer used in the friction materials
manufacturing process in which HAP solvent is used as one of the
ingredients in at least one batch during a semiannual reporting period.
Trace amounts of HAP solvents in resins or other friction ingredients do
not qualify mixers as solvent mixers.
Solvent recovery system means equipment used for the purpose of
recovering the HAP solvent from the exhaust stream. An example of a
solvent recovery system is a condenser.
Solvent substitution means substitution of a non-HAP material for a
HAP solvent.
Startup means bringing equipment online and starting the production
process.
Startup, shutdown, and malfunction plan means a plan developed
according to the provisions of Sec. 63.6(e)(3).
Sec. 63.9570 How do I apply for alternative compliance requirements?
(a) If you use a control technique other than a solvent recovery
system and/or solvent substitution, you may request approval to use an
alternative method of demonstrating compliance with the emission
limitations in Sec. 63.9500(a) and (b) according to the procedures in
this section.
(b) You can request approval to use an alternative method of
demonstrating compliance in the initial notification for existing
sources, the notification of construction or reconstruction for new
sources, or at any time.
(c) You must submit a description of the proposed testing,
monitoring, recordkeeping, and reporting that will be used and the
proposed basis for demonstrating compliance.
(1) If you have not previously performed testing, you must submit a
proposed test plan. If you are seeking permission to use an alternative
method of compliance based on previously performed testing, you must
submit the results of testing, a description of the procedures followed
in testing, and a description of pertinent conditions during testing.
(2) You must submit a monitoring plan that includes a description of
the control technique, test results verifying the performance of the
control technique, the appropriate operating parameters that will be
monitored, and the frequency of measuring and recording to establish
continuous compliance with the emission limitations in Sec. 63.9500(a)
and (b). You must also include the proposed performance specifications
and quality assurance procedures for the monitors. The monitoring plan
is subject to the Administrator's approval. You must install, calibrate,
operate, and maintain the monitors in accordance with the monitoring
plan approved by the Administrator.
(d) Use of the alternative method of demonstrating compliance must
not begin until approval is granted by the Administrator.
Sec. Sec. 63.9571-63.9579 [Reserved]
Table 1 to Subpart QQQQQ of Part 63--Applicability of General Provisions
to Subpart QQQQQ
As required in Sec. 63.9505, you must comply with each applicable
General Provisions requirement according to the following table:
----------------------------------------------------------------------------------------------------------------
Applies to subpart
Citation Subject QQQQQ? Explanation
----------------------------------------------------------------------------------------------------------------
Sec. 63.1....................... Applicability........... Yes......................
Sec. 63.2....................... Definitions............. Yes......................
Sec. 63.3....................... Units and Abbreviations. Yes......................
Sec. 63.4....................... Prohibited Activities... Yes......................
Sec. 63.5....................... Construction/ Yes......................
Reconstruction.
[[Page 61]]
Sec. 63.6(a)-(c), (e)-(f), (i)- Compliance with Yes......................
(j). Standards and
Maintenance
Requirements.
Sec. 63.6(d).................... [Reserved]..............
Sec. 63.6(g).................... Use of an Alternative No....................... Subpart QQQQQ contains
Nonopacity Emission no work practice
Standard. standards.
Sec. 63.6(h).................... Compliance with Opacity No....................... Subpart QQQQQ contains
and Visible Emission no opacity or VE
Standards. limits.
Sec. 63.7(a)(1)-(2)............. Applicability and No....................... Subpart QQQQQ includes
Performance Test Dates. dates for initial
compliance
demonstrations.
Sec. 63.7(a)(3), (b)-(h)........ Performance Testing No....................... Subpart QQQQQ does not
Requirements. require performance
tests.
Sec. 63.8(a)(1)-(2), (b), (c)(1)- Monitoring Requirements. Yes......................
(3), (f)(1)-(5).
Sec. 63.8(a)(3)................. [Reserved]..............
Sec. 63.8(a)(4)................. Additional Monitoring No....................... Subpart QQQQQ does not
Requirements for require flares.
Control Devices in Sec.
63.11.
Sec. 63.8(c)(4)................. Continuous Monitoring No....................... Subpart QQQQQ does not
System (CMS) require CMS.
Requirements.
Sec. 63.8(c)(5)................. Continuous Opacity No....................... Subpart QQQQQ does not
Monitoring System require COMS.
(COMS) Minimum
Procedures.
Sec. 63.8(c)(6)................. Zero and High Level No....................... Subpart QQQQQ specifies
Calibration Check calibration
Requirements. requirements.
Sec. 63.8(c)(7)-(8)............. Out-of-Control Periods.. No....................... Subpart QQQQQ specifies
out-of-control periods
and reporting
requirements.
Sec. 63.8(d).................... CMS Quality Control..... No....................... Subpart QQQQQ requires
a monitoring plan that
specifies CMS quality
control procedures.
Sec. 63.8(e).................... CMS Performance No....................... Subpart QQQQQ does not
Evaluation. require CMS
performance
evaluations.
Sec. 63.8(f)(6)................. Relative Accuracy Test No....................... Subpart QQQQQ does not
Audit (RATA) require continuous
Alternative. emissions monitoring
systems (CEMS).
Sec. 63.8(g)(1)-(5)............. Data Reduction.......... No....................... Subpart QQQQQ specifies
data reduction
requirements.
Sec. 63.9(a)-(d), (h)-(j)....... Notification Yes...................... Except that subpart
Requirements. QQQQQ does not require
performance tests or
CMS performance
evaluations.
Sec. 63.9(e).................... Notification of No....................... Subpart QQQQQ does not
Performance Test. require performance
tests.
Sec. 63.9(f).................... Notification of VE/ No....................... Subpart QQQQQ contains
Opacity Test. no opacity or VE
limits.
Sec. 63.9(g).................... Additional Notifications No....................... Subpart QQQQQ does not
When Using CMS. require CMS
performance
evaluations.
Sec. 63.10(a), (b), (d)(1), Recordkeeping and Yes......................
(d)(4)-(5), (e)(3), (f). Reporting Requirements.
Sec. 63.10(c)(1)-(6), (9)-(15).. Additional Records for No....................... Subpart QQQQQ specifies
CMS. record requirements.
Sec. 63.10(c)(7)-(8)............ Records of Excess No....................... Subpart QQQQQ specifies
Emissions and Parameter record requirements.
Monitoring Exceedances
for CMS.
Sec. 63.10(d)(2)................ Reporting Results of No....................... Subpart QQQQQ does not
Performance Tests. require performance
tests.
Sec. 63.10(d)(3)................ Reporting Opacity or VE No....................... Subpart QQQQQ contains
Observations. no opacity or VE
limits.
Sec. 63.10(e)(1)-(2)............ Additional CMS Reports.. No....................... Subpart QQQQQ does not
require CMS.
Sec. 63.10(e)(4)................ Reporting COMS Data..... No....................... Subpart QQQQQ does not
require COMS.
Sec. 63.11...................... Control Device No....................... Subpart QQQQQ does not
Requirements. require flares.
Sec. Sec. 63.12-63.15.......... Delegation, Addresses, Yes......................
Incorporation by
Reference Availability
of Information.
----------------------------------------------------------------------------------------------------------------
[[Page 62]]
Subpart RRRRR_National Emission Standards for Hazardous Air Pollutants:
Taconite Iron Ore Processing
Source: 68 FR 61888, Oct. 30, 2003, unless otherwise noted.
What This Subpart Covers
Sec. 63.9580 What is the purpose of this subpart?
This subpart establishes national emission standards for hazardous
air pollutants (NESHAP) for taconite iron ore processing. This subpart
also establishes requirements to demonstrate initial and continuous
compliance with all applicable emission limitations (emission limits and
operating limits), work practice standards, and operation and
maintenance requirements in this subpart.
Sec. 63.9581 Am I subject to this subpart?
You are subject to this subpart if you own or operate a taconite
iron ore processing plant that is (or is part of) a major source of
hazardous air pollutant (HAP) emissions on the first compliance date
that applies to you. Your taconite iron ore processing plant is a major
source of HAP if it emits or has the potential to emit any single HAP at
a rate of 10 tons or more per year or any combination of HAP at a rate
of 25 tons or more per year.
Sec. 63.9582 What parts of my plant does this subpart cover?
(a) This subpart applies to each new and existing affected source at
your taconite iron ore processing plant.
(b) The affected sources are each new or existing ore crushing and
handling operation, ore dryer, indurating furnace, and finished pellet
handling operation at your taconite iron ore processing plant, as
defined in Sec. 63.9652.
(c) This subpart covers emissions from ore crushing and handling
emission units, ore dryer stacks, indurating furnace stacks, finished
pellet handling emission units, and fugitive dust emissions.
(d) An ore crushing and handling operation, ore dryer, indurating
furnace, or finished pellet handling operation at your taconite iron ore
processing plant is existing if you commenced construction or
reconstruction of the affected source before December 18, 2002.
(e) An ore crushing and handling operation, ore dryer, indurating
furnace, or finished pellet handling operation at your taconite iron ore
processing plant is new if you commence construction or reconstruction
of the affected source on or after December 18, 2002. An affected source
is reconstructed if it meets the definition of reconstruction in Sec.
63.2.
Sec. 63.9583 When do I have to comply with this subpart?
(a) If you have an existing affected source, you must comply with
each emission limitation, work practice standard, and operation and
maintenance requirement in this subpart that applies to you no later
than October 30, 2006.
(b) If you have a new affected source and its initial startup date
is on or before October 30, 2003, you must comply with each emission
limitation, work practice standard, and operation and maintenance
requirement in this subpart that applies to you by October 30, 2003.
(c) If you have a new affected source and its initial startup date
is after October 30, 2003, you must comply with each emission
limitation, work practice standard, and operation and maintenance
requirement in this subpart that applies to you upon initial startup.
(d) If your taconite iron ore processing plant is an area source
that becomes a major source of HAP, the compliance dates in paragraphs
(d)(1) and (2) of this section apply to you.
(1) Any portion of the taconite iron ore processing plant that is a
new affected source or a new reconstructed source must be in compliance
with this subpart upon startup.
(2) All other parts of the taconite iron ore processing plant must
be in compliance with this subpart no later than 3 years after the plant
becomes a major source.
(e) You must meet the notification and schedule requirements in
Sec. 63.9640. Several of these notifications must be submitted before
the compliance date for your affected source.
[[Page 63]]
Emission Limitations and Work Practice Standards
Sec. 63.9590 What emission limitations must I meet?
(a) You must meet each emission limit in Table 1 to this subpart
that applies to you.
(b) You must meet each operating limit for control devices in
paragraphs (b)(1) through (5) of this section that applies to you.
(1) Except as provided in paragraph (b)(2) of this section, for each
wet scrubber applied to meet any particulate matter emission limit in
Table 1 to this subpart, you must maintain the daily average pressure
drop and daily average scrubber water flow rate at or above the minimum
levels established during the initial performance test.
(2) For each dynamic wet scrubber applied to meet any particulate
matter emission limit in Table 1 to this subpart, you must maintain the
daily average scrubber water flow rate and either the daily average fan
amperage (a surrogate for fan speed as revolutions per minute) or the
daily average pressure drop at or above the minimum levels established
during the initial performance test.
(3) For each dry electrostatic precipitator applied to meet any
particulate matter emission limit in Table 1 to this subpart, you must
meet the operating limits in paragraph (b)(3)(i) or (ii) of this
section.
(i) Maintain the 6-minute average opacity of emissions exiting the
control device stack at or below the level established during the
initial performance test.
(ii) Maintain the daily average secondary voltage and daily average
secondary current for each field at or above the minimum levels
established during the initial performance test.
(4) For each wet electrostatic precipitator applied to meet any
particulate matter emission limit in Table 1 to this subpart, you must
meet the operating limits in paragraphs (b)(4)(i) through (iii) of this
section.
(i) Maintain the daily average secondary voltage for each field at
or above the minimum levels established during the initial performance
test.
(ii) Maintain the daily average stack outlet temperature at or below
the maximum levels established during the initial performance test.
(iii) Maintain the daily average water flow rate at or above the
minimum levels established during the initial performance test.
(5) If you use any air pollution control device other than a
baghouse, wet scrubber, dynamic scrubber, dry electrostatic
precipitator, or wet electrostatic precipitator, you must submit a site-
specific monitoring plan in accordance with Sec. 63.9631(f).
(c) You may petition the Administrator for approval of alternatives
to the monitoring requirements in paragraphs (b)(1) through (4) of this
section as allowed under Sec. 63.8(f) and as defined in Sec. 63.90.
Sec. 63.9591 What work practice standards must I meet?
(a) You must prepare, and at all times operate according to, a
fugitive dust emissions control plan that describes in detail the
measures that will be put in place to control fugitive dust emissions
from the locations listed in paragraphs (a)(1) through (6) of this
section.
(1) Stockpiles (includes, but is not limited to, stockpiles of
uncrushed ore, crushed ore, or finished pellets);
(2) Material transfer points;
(3) Plant roadways;
(4) Tailings basin;
(5) Pellet loading areas; and
(6) Yard areas.
(b) A copy of your fugitive dust emissions control plan must be
submitted for approval to the Administrator on or before the applicable
compliance date for the affected source as specified in Sec. 63.9583.
The requirement for the plant to operate according to the fugitive dust
emissions control plan must be incorporated by reference in the
operating permit for the plant that is issued by the designated
permitting authority under 40 CFR part 70 or 40 CFR part 71.
(c) You can use an existing fugitive dust emissions control plan
provided it meets the requirements in paragraphs (c)(1) through (3) of
this section.
(1) The plan satisfies the requirements of paragraph (a) of this
section.
[[Page 64]]
(2) The plan describes the current measures to control fugitive dust
emission sources.
(3) The plan has been approved as part of a State implementation
plan or title V permit.
(d) You must maintain a current copy of the fugitive dust emissions
control plan onsite, and it must be available for inspection upon
request. You must keep the plan for the life of the affected source or
until the affected source is no longer subject to the requirements of
this subpart.
Operation and Maintenance Requirements
Sec. 63.9600 What are my operation and maintenance requirements?
(a) As required by Sec. 63.6(e)(1)(i), you must always operate and
maintain your affected source, including air pollution control and
monitoring equipment, in a manner consistent with good air pollution
control practices for minimizing emissions at least to the levels
required by this subpart.
(b) You must prepare, and at all times operate according to, a
written operation and maintenance plan for each control device applied
to meet any particulate matter emission limit in Table 1 to this subpart
and to meet the requirement of each indurating furnace subject to good
combustion practices (GCP). Each site-specific operation and maintenance
plan must be submitted to the Administrator on or before the compliance
date that is specified in Sec. 63.9583 for your affected source. The
plan you submit must explain why the chosen practices (i.e., quantified
objectives) are effective in performing corrective actions or GCP in
minimizing the formation of formaldehyde (and other products of
incomplete combustion). The Administrator will review the adequacy of
the site-specific practices and objectives you will follow and the
records you will keep to demonstrate compliance with your Plan. If the
Administrator determines that any portion of your operation and
maintenance plan is not adequate, we can reject those portions of the
plan, and request that you provide additional information addressing the
relevant issues. In the interim of this process, you will continue to
follow your current site-specific practices and objectives, as
submitted, until your revisions are accepted as adequate by the
Administrator. You must maintain a current copy of the operation and
maintenance plan onsite, and it must be available for inspection upon
request. You must keep the plan for the life of the affected source or
until the affected source is no longer subject to the requirements of
this subpart. Each operation and maintenance plan must address the
elements in paragraphs (b)(1) through (4) of this section.
(1) Preventative maintenance for each control device, including a
preventative maintenance schedule that is consistent with the
manufacturer's instructions for routine and long-term maintenance.
(2) Corrective action procedures for bag leak detection systems. In
the event a bag leak detection system alarm is triggered, you must
initiate corrective action to determine the cause of the alarm within 1
hour of the alarm, initiate corrective action to correct the cause of
the problem within 24 hours of the alarm, and complete the corrective
action as soon as practicable. Corrective actions may include, but are
not limited to, the actions listed in paragraphs (b)(2)(i) through (vi)
of this section.
(i) Inspecting the baghouse for air leaks, torn or broken bags or
filter media, or any other condition that may cause an increase in
emissions.
(ii) Sealing off defective bags or filter media.
(iii) Replacing defective bags or filter media or otherwise
repairing the control device.
(iv) Sealing off a defective baghouse compartment.
(v) Cleaning the bag leak detection system probe, or otherwise
repairing the bag leak detection system.
(vi) Adjusting the process operation producing the particulate
emissions.
(3) Corrective action procedures for continuous parameter monitoring
systems (CPMS) for all air pollution control devices except for
baghouses. In the event you exceed an established operating limit for an
air pollution control device except for a baghouse, you
[[Page 65]]
must initiate corrective action to determine the cause of the operating
limit exceedance and complete the corrective action within 10 calendar
days. The corrective action procedures you take must be consistent with
the installation, operation, and maintenance procedures listed in your
site-specific CPMS monitoring plan in accordance with Sec. 63.9632(b).
(4) Good combustion practices for indurating furnaces. You must
identify and implement a set of site-specific GCP for each type of
indurating furnace at your plant. These GCP should correspond to your
standard operating procedures for maintaining the proper and efficient
combustion within each indurating furnace. Good combustion practices
include, but are not limited to, the elements listed in paragraphs
(b)(4)(i) through (v) of this section.
(i) Proper operating conditions for each indurating furnace (e.g.,
minimum combustion temperature, maximum carbon monoxide concentration in
the furnace exhaust gases, burner alignment, or proper fuel-air
distribution/mixing).
(ii) Routine inspection and preventative maintenance and
corresponding schedules of each indurating furnace.
(iii) Performance analyses of each indurating furnace.
(iv) Keeping applicable operator logs.
(v) Keeping applicable records to document compliance with each
element.
General Compliance Requirements
Sec. 63.9610 What are my general requirements for complying with this
subpart?
(a) You must be in compliance with the requirements in paragraphs
(a)(1) through (6) in this section at all times, except during periods
of startup, shutdown, and malfunction. The terms startup, shutdown, and
malfunction are defined in Sec. 63.2.
(1) The emission limitations in Sec. 63.9590.
(2) The work practice standards in Sec. 63.9591.
(3) The operation and maintenance requirements in Sec. 63.9600.
(4) The notification requirements in Sec. 63.9640.
(5) The reporting requirements in Sec. 63.9641.
(6) The recordkeeping requirements in Sec. 63.9642.
(b) During the period between the compliance date specified for your
affected source in Sec. 63.9583 and the date upon which continuous
monitoring systems have been installed and certified and any applicable
operating limits have been set, you must maintain a log detailing the
operation and maintenance of the process and emissions control
equipment. This includes the daily monitoring and recordkeeping of air
pollution control device operating parameters as specified in Sec.
63.9590(b).
(c) You must develop a written startup, shutdown, and malfunction
plan according to the provisions in Sec. 63.6(e)(3).
[68 FR 61888, Oct. 30, 2003, as amended at 71 FR 20470, Apr. 20, 2006]
Initial Compliance Requirements
Sec. 63.9620 On which units and by what date must I conduct performance
tests or other initial compliance demonstrations?
(a) For each ore crushing and handling affected source, you must
demonstrate initial compliance with the emission limits in Table 1 to
this subpart by conducting an initial performance test for particulate
matter as specified in paragraphs (a)(1) and (2) of this section.
(1) Except as provided in paragraph (e) of this section, an initial
performance test must be performed on all stacks associated with ore
crushing and handling.
(2) Initial performance tests must be completed no later than 180
calendar days after the compliance date specified in Sec. 63.9583.
Performance tests conducted between October 30, 2003 and no later than
180 days after the corresponding compliance date can be used for initial
compliance demonstration, provided the tests meet the initial
performance testing requirements of this subpart.
(b) For each indurating furnace affected source, you must
demonstrate initial compliance with the emission limits in Table 1 to
this subpart by conducting an initial performance test for particulate
matter as specified in paragraphs (b)(1) and (2) of this section.
[[Page 66]]
(1) An initial performance test must be performed on all stacks
associated with each indurating furnace.
(2) Initial performance tests must be completed no later than 180
calendar days after the compliance date specified in Sec. 63.9583.
Performance tests conducted between October 30, 2003 and no later than
180 days after the corresponding compliance date can be used for initial
compliance demonstration, provided the tests meet the initial
performance testing requirements of this subpart. For indurating
furnaces with multiple stacks, the performance tests for all stacks must
be completed within a reasonable period of time, such that the
indurating furnace operating characteristics remain representative for
the duration of the stack tests.
(c) For each finished pellet handling affected source, you must
demonstrate initial compliance with the emission limits in Table 1 to
this subpart by conducting an initial performance test for particulate
matter as specified in paragraphs (c)(1) and (2) of this section.
(1) Except as provided in paragraph (e) of this section, an initial
performance test must be performed on all stacks associated with
finished pellet handling.
(2) Initial performance tests must be completed no later than 180
calendar days after the compliance date specified in Sec. 63.9583.
Performance tests conducted between October 30, 2003 and no later than
180 days after the corresponding compliance date can be used for initial
compliance demonstration, provided the tests meet the initial compliance
testing requirements of this subpart.
(d) For each ore dryer affected source, you must demonstrate initial
compliance with the emission limits in Table 1 to this subpart by
conducting an initial performance test for particulate matter as
specified in paragraphs (d)(1) and (2) of this section.
(1) An initial performance test must be performed on all stacks
associated with each ore dryer.
(2) Initial performance tests must be completed no later than 180
calendar days after the compliance date specified in Sec. 63.9583.
Performance tests conducted between October 30, 2003 and no later than
180 days after the corresponding compliance date can be used for initial
compliance demonstration, provided the tests meet the initial compliance
testing requirements of this subpart. For ore dryers with multiple
stacks, the performance tests for all stacks must be completed within a
reasonable period of time, such that the ore dryer operating
characteristics remain representative for the duration of the stack
tests.
(e) For ore crushing and handling affected sources and finished
pellet handling affected sources, in lieu of conducting initial
performance tests for particulate matter on all stacks, you may elect to
group a maximum of six similar emission units together and conduct an
initial compliance test on one representative emission unit within each
group of similar emission units. The determination of whether emission
units are similar must meet the criteria in paragraph (f) of this
section. If you decide to test representative emission units, you must
prepare and submit a testing plan as described in paragraph (g) of this
section.
(f) If you elect to test representative emission units as provided
in paragraph (e) of this section, the units that are grouped together as
similar units must meet the criteria in paragraphs (f)(1) through (3) of
this section.
(1) All emission units within a group must be of the same process
type (e.g., primary crushers, secondary crushers, tertiary crushers,
fine crushers, ore conveyors, ore bins, ore screens, grate feed, pellet
loadout, hearth layer, cooling stacks, pellet conveyor, and pellet
screens). You cannot group emission units from different process types
together for the purposes of this section.
(2) All emission units within a group must also have the same type
of air pollution control device (e.g., wet scrubbers, dynamic wet
scrubbers, rotoclones, multiclones, wet and dry electrostatic
precipitators, and baghouses). You cannot group emission units with
different air pollution control device types together for the purposes
of this section.
(3) The site-specific operating limits established for the emission
unit selected as representative of a group of similar emission units
will be used as
[[Page 67]]
the operating limit for each emission unit within the group. The
operating limit established for the representative unit must be met by
each emission unit within the group.
(g) If you plan to conduct initial performance tests on
representative emission units within an ore crushing and handling
affected source or a finished pellet handling affected source, you must
submit a testing plan for initial performance tests. This testing plan
must be submitted to the Administrator or delegated authority no later
than 90 days prior to the first scheduled initial performance test. The
testing plan must contain the information specified in paragraphs (g)(1)
through (3) of this section.
(1) A list of all emission units. This list must clearly identify
all emission units that have been grouped together as similar emission
units. Within each group of emission units, you must identify the
emission unit that will be the representative unit for that group and
subject to initial performance testing.
(2) A list of the process type and type of air pollution control
device on each emission unit.
(3) A schedule indicating when you will conduct an initial
performance test for particulate matter for each representative emission
unit.
(h) For each work practice standard and operation and maintenance
requirement that applies to you where initial compliance is not
demonstrated using a performance test, you must demonstrate initial
compliance within 30 calendar days after the compliance date that is
specified for your affected source in Sec. 63.9583.
(i) If you commenced construction or reconstruction of an affected
source between December 18, 2002 and October 30, 2003 , you must
demonstrate initial compliance with either the proposed emission limit
or the promulgated emission limit no later than 180 calendar days after
October 30, 2003 or no later than 180 calendar days after startup of the
source, whichever is later, according to Sec. 63.7(a)(2)(ix).
(j) If you commenced construction or reconstruction of an affected
source between December 18, 2002 and October 30, 2003, and you chose to
comply with the proposed emission limit when demonstrating initial
compliance, you must conduct a second performance test to demonstrate
compliance with the promulgated emission limit by 3 years and 180
calendar days after October 30, 2003, or after startup of the source,
whichever is later, according to Sec. 63.7(a)(2)(ix).
Sec. 63.9621 What test methods and other procedures must I use to
demonstrate initial compliance with the emission limits for particulate
matter?
(a) You must conduct each performance test that applies to your
affected source according to the requirements in Sec. 63.7(e)(1) and
paragraphs (b) and (c) of this section.
(b) For each ore crushing and handling affected source and each
finished pellet handling affected source, you must determine compliance
with the applicable emission limit for particulate matter in Table 1 to
this subpart by following the test methods and procedures in paragraphs
(b)(1) through (3) of this section.
(1) Except as provided in Sec. 63.9620(e), determine the
concentration of particulate matter in the stack gas for each emission
unit according to the test methods in appendix A to part 60 of this
chapter. The applicable test methods are listed in paragraphs (b)(1)(i)
through (v) of this section.
(i) Method 1 or 1A to select sampling port locations and the number
of traverse points. Sampling ports must be located at the outlet of the
control device and prior to any releases to the atmosphere.
(ii) Method 2, 2A, 2C, 2D, 2F, or 2G, as applicable, to determine
the volumetric flow rate of the stack gas.
(iii) Method 3, 3A, or 3B to determine the dry molecular weight of
the stack gas.
(iv) Method 4 to determine the moisture content of the stack gas.
(v) Method 5, 5D, or 17 to determine the concentration of
particulate matter.
(2) Each Method 5, 5D, or 17 performance test must consist of three
separate runs. Each run must be conducted for a minimum of 2 hours. The
average particulate matter concentration from
[[Page 68]]
the three runs will be used to determine compliance, as shown in
Equation 1 of this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.000
Where:
Ci = Average particulate matter concentration for emission
unit, grains per dry standard cubic foot, (gr/dscf);
C1 = Particulate matter concentration for run 1 corresponding
to emission unit, gr/dscf;
C2 = Particulate matter concentration for run 2 corresponding
to emission unit, gr/dscf; and
C3 = Particulate matter concentration for run 3 corresponding
to emission unit, gr/dscf.
(3) For each ore crushing and handling affected source and each
finished pellet handling affected source, you must determine the flow-
weighted mean concentration of particulate matter emissions from all
emission units in each affected source following the procedure in
paragraph (b)(3)(i) or (ii) of this section.
(i) If an initial performance test is conducted on all emission
units within an affected source, calculate the flow-weighted mean
concentration of particulate matter emissions from the affected source
using Equation 2 of this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.001
Where:
Ca = Flow-weighted mean concentration of particulate matter
for all emission units within affected source, (gr/dscf);
Ci = Average particulate matter concentration measured during
the performance test from emission unit ``i'' in affected source, as
determined using Equation 1 of this section, gr/dscf;
Qi = Average volumetric flow rate of stack gas measured
during the performance test from emission unit ``i'' in affected source,
dscf/hr; and
n = Number of emission units in affected source.
(ii) If you are grouping similar emission units together in
accordance with Sec. 63.9620(e), you must follow the procedures in
paragraphs (b)(3)(ii)(A) through (C) of this section.
(A) Assign the average particulate matter concentration measured
from the representative unit, as determined from Equation 1 of this
section, to each emission unit within the corresponding group of similar
units.
(B) Establish the maximum operating volumetric flow rate of exhaust
gas from each emission unit within each group of similar units.
(C) Using the data from paragraphs (b)(3)(ii)(A) and (B) of this
section, calculate the flow-weighted mean concentration of particulate
matter emissions from the affected source using Equation 3 of this
section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.002
Where:
Ca = Flow-weighted mean concentration of particulate matter
for all emission units within affected source, gr/dscf;
Ck = Average particulate matter concentration measured during
the performance test from the representative emission unit in group
``k'' of affected source ``a,'' as determined using Equation 1 of this
section, gr/dscf;
Qk = Sum of the maximum operating volumetric flow rates of
stack gas from all similar emission units within group ``k'' of affected
source, dscf/hr; and
m = Number of similar emission unit groups in affected source.
(c) For each ore dryer affected source and each indurating furnace
affected source, you must determine compliance with the applicable
emission limit for particulate matter in Table 1 to this subpart by
following the test methods and procedures in paragraphs (c)(1) through
(3) of this section.
(1) Determine the concentration of particulate matter for each stack
according to the test methods in 40 CFR part 60, appendix A. The
applicable test methods are listed in paragraphs (c)(1)(i) through (v)
of this section.
(i) Method 1 or 1A to select sampling port locations and the number
of traverse points. Sampling ports must be
[[Page 69]]
located at the outlet of the control device and prior to any releases to
the atmosphere.
(ii) Method 2, 2A, 2C, 2D, 2F, or 2G, as applicable, to determine
the volumetric flow rate of the stack gas.
(iii) Method 3, 3A, or 3B to determine the dry molecular weight of
the stack gas.
(iv) Method 4 to determine the moisture content of the stack gas.
(v) Method 5, 5D, or 17 to determine the concentration of
particulate matter.
(2) Each Method 5, 5D, or 17 performance test must consist of three
separate runs. Each run must be conducted for a minimum of 2 hours. The
average particulate matter concentration from the three runs will be
used to determine compliance, as shown in Equation 1 of this section.
(3) For each ore dryer and each indurating furnace with multiple
stacks, calculate the flow-weighted mean concentration of particulate
matter emissions using Equation 4 of this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.003
Where:
Cb = Flow-weighted mean concentration of particulate matter
for all stacks associated with affected source, gr/dscf;
Cj = Average particulate matter concentration measured during
the performance test from stack ``j'' in affected source, as determined
using Equation 1 of this section, gr/dscf;
Qj = Average volumetric flow rate of stack gas measured
during the performance test from stack ``j'' in affected source, dscf/
hr;
n = Number of stacks associated with affected source.
Sec. 63.9622 What test methods and other procedures must I use to
establish and demonstrate initial compliance with the operating limits?
(a) For wet scrubbers subject to performance testing in Sec.
63.9620 and operating limits for pressure drop and scrubber water flow
rate in Sec. 63.9590(b)(1), you must establish site-specific operating
limits according to the procedures in paragraphs (a)(1) through (3) of
this section.
(1) Using the CPMS required in Sec. 63.9631(b), measure and record
the pressure drop and scrubber water flow rate every 15 minutes during
each run of the particulate matter performance test.
(2) Calculate and record the average pressure drop and scrubber
water flow rate for each individual test run. Your operating limits are
established as the lowest average pressure drop and the lowest average
scrubber water flow rate corresponding to any of the three test runs.
(3) If a rod-deck venturi scrubber is applied to an indurating
furnace to meet any particulate matter emission limit in Table 1 to this
subpart, you may establish a lower average pressure drop operating limit
by using historical average pressure drop data from a certified
performance test completed on or after December 18, 2002 instead of
using the average pressure drop value determined during the initial
performance test, as specified in paragraph (a)(2) of this section. If
historical average pressure drop data are used to establish an operating
limit (i.e., using data from a certified performance test conducted
prior to the promulgation date of the final rule), then the average
particulate matter concentration corresponding to the historical
performance test must be at or below the applicable indurating furnace
emission limit, as listed in Table 1 to this subpart.
(b) For dynamic wet scrubbers subject to performance testing in
Sec. 63.9620 and operating limits for scrubber water flow rate and
either fan amperage or pressure drop in Sec. 63.9590(b)(2), you must
establish site-specific operating limits according to the procedures in
paragraphs (b)(1) and (2) of this section.
(1) Using the CPMS required in Sec. 63.9631(b), measure and record
the scrubber water flow rate and either the fan amperage or pressure
drop every 15 minutes during each run of the particulate matter
performance test.
(2) Calculate and record the average scrubber water flow rate and
either the average fan amperage or average pressure drop for each
individual test run. Your operating limits are established
[[Page 70]]
as the lowest average scrubber water flow rate and either the lowest
average fan amperage or pressure drop value corresponding to any of the
three test runs.
(c) For a dry electrostatic precipitator subject to performance
testing in Sec. 63.9620 and operating limits in Sec. 63.9590(b)(3),
you must establish a site-specific operating limit according to the
procedures in paragraphs (c)(1) or (2) of this section.
(1) If the operating limit for your dry electrostatic precipitator
is a 6-minute average opacity of emissions value, then you must follow
the requirements in paragraphs (c)(1)(i) through (iii) of this section.
(i) Using the continuous opacity monitoring system (COMS) required
in Sec. 63.9631(d)(1), measure and record the opacity of emissions from
each control device stack during the particulate matter performance
test.
(ii) Compute and record the 6-minute opacity averages from 24 or
more data points equally spaced over each 6-minute period (e.g., at 15-
second intervals) during the test runs.
(iii) Using the opacity measurements from a performance test that
meets the emission limit, determine the opacity value corresponding to
the 99 percent upper confidence level of a normal distribution of the 6-
minute opacity averages.
(2) If the operating limit for your dry electrostatic precipitator
is the daily average secondary voltage and daily average secondary
current for each field, then you must follow the requirements in
paragraphs (c)(2)(i) and (ii) of this section.
(i) Using the CPMS required in Sec. 63.9631(d)(2), measure and
record the secondary voltage and secondary current for each dry
electrostatic precipitator field every 15 minutes during each run of the
particulate matter performance test.
(ii) Calculate and record the average secondary voltage and
secondary current for each dry electrostatic precipitator field for each
individual test run. Your operating limits are established as the lowest
average secondary voltage and secondary current value for each dry
electrostatic precipitator field corresponding to any of the three test
runs.
(d) For a wet electrostatic precipitator subject to performance
testing in Sec. 63.9620 and operating limit in Sec. 63.9590(b)(4), you
must establish a site-specific operating limit according to the
procedures in paragraphs (d)(1) and (2) of this section.
(1) Using the CPMS required in Sec. 63.9631(e), measure and record
the parametric values in paragraphs (d)(1)(i) through (iii) of this
section for each wet electrostatic precipitator field every 15 minutes
during each run of the particulate matter performance test.
(i) Secondary voltage;
(ii) Water flow rate; and
(iii) Stack outlet temperature.
(2) For each individual test run, calculate and record the average
value for each operating parameter in paragraphs (d)(1)(i) through (iii)
of this section for each wet electrostatic precipitator field. Your
operating limits are established as the lowest average value for each
operating parameter corresponding to any of the three test runs.
(e) If you use an air pollution control device other than a wet
scrubber, dynamic wet scrubber, dry electrostatic precipitator, wet
electrostatic precipitator, or baghouse, and it is subject to
performance testing in Sec. 63.9620, you must submit a site-specific
monitoring plan in accordance with Sec. 63.9631(f). The site-specific
monitoring plan must include the site-specific procedures for
demonstrating initial and continuous compliance with the corresponding
operating limits.
(f) You may change the operating limits for any air pollution
control device as long as you meet the requirements in paragraphs (f)(1)
through (3) of this section.
(1) Submit a written notification to the Administrator of your
request to conduct a new performance test to revise the operating limit.
(2) Conduct a performance test to demonstrate compliance with the
applicable emission limitation in Table 1 to this subpart.
(3) Establish revised operating limits according to the applicable
procedures
[[Page 71]]
in paragraphs (a) through (e) of this section.
Sec. 63.9623 How do I demonstrate initial compliance with the emission
limitations that apply to me?
(a) For each affected source subject to an emission limit in Table 1
to this subpart, you must demonstrate initial compliance by meeting the
emission limit requirements in paragraphs (a)(1) through (4) of this
section.
(1) For ore crushing and handling, the flow-weighted mean
concentration of particulate matter, determined according to the
procedures in Sec. Sec. 63.9620(a) and 63.9621(b), must not exceed the
emission limits in Table 1 to this subpart.
(2) For indurating furnaces, the flow-weighted mean concentration of
particulate matter, determined according to the procedures in Sec. Sec.
63.9620(b) and 63.9621(c), must not exceed the emission limits in Table
1 to this subpart.
(3) For finished pellet handling, the flow-weighted mean
concentration of particulate matter, determined according to the
procedures in Sec. Sec. 63.9620(c) and 63.9621(b), must not exceed the
emission limits in Table 1 to this subpart.
(4) For ore dryers, the flow-weighted mean concentration of
particulate matter, determined according to the procedures in Sec. Sec.
63.9620(d) and 63.9621(c), must not exceed the emission limits in Table
1 to this subpart.
(b) For each affected source subject to an emission limit in Table 1
to this subpart, you must demonstrate initial compliance by meeting the
operating limit requirements in paragraphs (b)(1) through (5) of this
section.
(1) For each wet scrubber subject to performance testing in Sec.
63.9620 and operating limits for pressure drop and scrubber water flow
rate in Sec. 63.9590(b)(1), you have established appropriate site-
specific operating limits and have a record of the pressure drop and
scrubber water flow rate measured during the performance test in
accordance with Sec. 63.9622(a).
(2) For each dynamic wet scrubber subject to performance testing in
Sec. 63.9620 and operating limits for scrubber water flow rate and
either fan amperage or pressure drop in Sec. 63.9590(b)(2), you have
established appropriate site-specific operating limits and have a record
of the scrubber water flow rate and either the fan amperage or pressure
drop value, measured during the performance test in accordance with
Sec. 63.9622(b).
(3) For each dry electrostatic precipitator subject to performance
testing in Sec. 63.9620 and one of the operating limits in Sec.
63.9590(b)(3), you must meet the requirements in paragraph (b)(3)(i) or
(ii) of this section.
(i) If you are subject to the operating limit for opacity in Sec.
63.9590(b)(3)(i), you have established appropriate site-specific
operating limits and have a record of the opacity measured during the
performance test in accordance with Sec. 63.9622(c)(1).
(ii) If you are subject to the operating limit for secondary voltage
and secondary current in Sec. 63.9590(b)(3)(ii), you have established
appropriate site-specific operating limits and have a record of the
secondary voltage and secondary current measured during the performance
test in accordance with Sec. 63.9622(c)(2).
(4) For each wet electrostatic precipitator subject to performance
testing in Sec. 63.9620 and operating limits for secondary voltage,
water flow rate, and stack outlet temperature in Sec. 63.9590(b)(4),
you have established appropriate site-specific operating limits and have
a record of the secondary voltage, water flow rate, and stack outlet
temperature measured during the performance test in accordance with
Sec. 63.9622(d).
(5) For other air pollution control devices subject to performance
testing in Sec. 63.9620 and operating limits in accordance with Sec.
63.9590(b)(5), you have submitted a site-specific monitoring plan in
accordance with Sec. 63.9631(f) and have a record of the site-specific
operating limits as measured during the performance test in accordance
with Sec. 63.9622(e).
(c) For each emission limitation and operating limit that applies to
you, you must submit a notification of compliance status according to
Sec. 63.9640(e).
[[Page 72]]
Sec. 63.9624 How do I demonstrate initial compliance with the work
practice standards that apply to me?
You must demonstrate initial compliance with the work practice
standards by meeting the requirements in paragraphs (a) through (c) of
this section.
(a) You must prepare a fugitive dust emissions control plan in
accordance with the requirements in Sec. 63.9591.
(b) You must submit to the Administrator the fugitive dust emissions
control plan in accordance with the requirements in Sec. 63.9591.
(c) You must implement each control practice according to the
procedures specified in your fugitive dust emissions control plan.
Sec. 63.9625 How do I demonstrate initial compliance with the
operation and maintenance requirements that apply to me?
For each air pollution control device subject to operating limits in
Sec. 63.9590(b), you have demonstrated initial compliance if you meet
all of the requirements in paragraphs (a) through (d) of this section.
(a) You have prepared the operation and maintenance plan for air
pollution control devices in accordance with Sec. 63.9600(b).
(b) You have operated each air pollution control device according to
the procedures in the operation and maintenance plan.
(c) You have submitted a notification of compliance status according
to the requirements in Sec. 63.9640(e).
(d) You have prepared a site-specific monitoring plan in accordance
with Sec. 63.9632(b).
Continuous Compliance Requirements
Sec. 63.9630 When must I conduct subsequent performance tests?
(a) You must conduct subsequent performance tests to demonstrate
continued compliance with the ore crushing and handling emission limits
in Table 1 to this subpart according to the schedule developed by your
permitting authority and shown in your title V permit. If a title V
permit has not been issued, you must submit a testing plan and schedule,
containing the information specified in paragraph (e) of this section,
to the permitting authority for approval.
(b) You must conduct subsequent performance tests on all stacks
associated with indurating furnaces to demonstrate continued compliance
with the indurating furnace emission limits in Table 1 to this subpart
according to the schedule developed by your permitting authority and
shown in your title V permit, but no less frequent than twice per 5-year
permit term. If a title V permit has not been issued, you must submit a
testing plan and schedule, containing the information specified in
paragraph (e) of this section, to the permitting authority for approval.
For indurating furnaces with multiple stacks, the performance tests for
all stacks associated with that indurating furnace must be conducted
within a reasonable period of time, such that the indurating furnace
operating characteristics remain representative for the duration of the
stack tests.
(c) You must conduct subsequent performance tests to demonstrate
continued compliance with the finished pellet handling emission limits
in Table 1 to this subpart according to the schedule developed by your
permitting authority and shown in your title V permit. If a title V
permit has not been issued, you must submit a testing plan and schedule,
containing the information specified in paragraph (e) of this section,
to the permitting authority for approval.
(d) You must conduct subsequent performance tests on all stacks
associated with ore dryers to demonstrate continued compliance with the
ore dryer emission limits in Table 1 to this subpart according to the
schedule developed by your permitting authority and shown in your title
V permit. If a title V permit has not been issued, you must submit a
testing plan and schedule, containing the information specified in
paragraph (e) of this section, to the permitting authority for approval.
For ore dryers with multiple stacks, the performance tests for all
stacks associated with an ore dryer must be conducted within a
reasonable period of time, such that the ore dryer operating
characteristics remain representative for the duration of the stack
tests.
[[Page 73]]
(e) If your plant does not have a title V permit, you must submit a
testing plan for subsequent performance tests as required in paragraphs
(a) through (d) of this section. This testing plan must be submitted to
the Administrator on or before the compliance date that is specified in
Sec. 63.9583. The testing plan must contain the information specified
in paragraphs (e)(1) and (2) of this section. You must maintain a
current copy of the testing plan onsite, and it must be available for
inspection upon request. You must keep the plan for the life of the
affected source or until the affected source is no longer subject to the
requirements of this subpart.
(1) A list of all emission units.
(2) A schedule indicating when you will conduct subsequent
performance tests for particulate matter for each of the emission units.
Sec. 63.9631 What are my monitoring requirements?
(a) For each baghouse applied to meet any particulate matter
emission limit in Table 1 to this subpart, you must install, operate,
and maintain a bag leak detection system to monitor the relative change
in particulate matter loadings according to the requirements in Sec.
63.9632(a), and conduct inspections at their specified frequencies
according to the requirements in paragraphs (a)(1) through (8) of this
section.
(1) Monitor the pressure drop across each baghouse cell each day to
ensure pressure drop is within the normal operating range.
(2) Confirm that dust is being removed from hoppers through weekly
visual inspections or other means of ensuring the proper functioning of
removal mechanisms.
(3) Check the compressed air supply of pulse-jet baghouses each day.
(4) Monitor cleaning cycles to ensure proper operation using an
appropriate methodology.
(5) Check bag cleaning mechanisms for proper functioning through
monthly visual inspections or equivalent means.
(6) Make monthly visual checks of bag tension on reverse air and
shaker-type baghouses to ensure that bags are not kinked (kneed or bent)
or lying on their sides. You do not have to make this check for shaker-
type baghouses that have self-tensioning (spring-loaded) devices.
(7) Confirm the physical integrity of the baghouse through quarterly
visual inspections of the baghouse interior for air leaks.
(8) Inspect fans for wear, material buildup, and corrosion through
quarterly visual inspections, vibration detectors, or equivalent means.
(b) Except as provided in paragraph (c) of this section, for each
wet scrubber subject to the operating limits for pressure drop and
scrubber water flow rate in Sec. 63.9590(b)(1), you must install,
operate, and maintain a CPMS according to the requirements in Sec.
63.9632(b) through (e) and monitor the daily average pressure drop and
daily average scrubber water flow rate according to the requirements in
Sec. 63.9633.
(c) For each dynamic wet scrubber subject to the scrubber water flow
rate and either the fan amperage or pressure drop operating limits in
Sec. 63.9590(b)(2), you must install, operate, and maintain a CPMS
according to the requirements in Sec. 63.9632(b) through (e) and
monitor the daily average scrubber water flow rate and either the daily
average fan amperage or the daily average pressure drop according to the
requirements in Sec. 63.9633.
(d) For each dry electrostatic precipitator subject to the operating
limits in Sec. 63.9590(b)(3), you must follow the monitoring
requirements in paragraph (d)(1) or (2) of this section.
(1) If the operating limit you choose to monitor is the 6-minute
average opacity of emissions in accordance with Sec. 63.9590(b)(3)(i),
you must install, operate, and maintain a COMS according to the
requirements in Sec. 63.9632(f) and monitor the 6-minute average
opacity of emissions exiting each control device stack according to the
requirements in Sec. 63.9633.
(2) If the operating limit you choose to monitor is average
secondary voltage and average secondary current for each dry
electrostatic precipitator field in accordance with Sec.
63.9590(b)(3)(ii), you must install, operate, and maintain a CPMS
according to the requirements in Sec. 63.9632(b) through
[[Page 74]]
(e) and monitor the daily average secondary voltage and daily average
secondary current according to the requirements in Sec. 63.9633.
(e) For each wet electrostatic precipitator subject to the operating
limits in Sec. 63.9590(b)(4), you must install, operate, and maintain a
CPMS according to the requirements in Sec. 63.9632(b) through (e) and
monitor the daily average secondary voltage, daily average stack outlet
temperature, and daily average water flow rate according to the
requirements in Sec. 63.9633.
(f) If you use any air pollution control device other than a
baghouse, wet scrubber, dry electrostatic precipitator, or wet
electrostatic precipitator, you must submit a site-specific monitoring
plan that includes the information in paragraphs (f)(1) through (4) of
this section. The monitoring plan is subject to approval by the
Administrator. You must maintain a current copy of the monitoring plan
onsite, and it must be available for inspection upon request. You must
keep the plan for the life of the affected source or until the affected
source is no longer subject to the requirements of this subpart.
(1) A description of the device.
(2) Test results collected in accordance with Sec. 63.9621
verifying the performance of the device for reducing emissions of
particulate matter to the atmosphere to the levels required by this
subpart.
(3) A copy of the operation and maintenance plan required in Sec.
63.9600(b).
(4) Appropriate operating parameters that will be monitored to
maintain continuous compliance with the applicable emission
limitation(s).
Sec. 63.9632 What are the installation, operation, and maintenance
requirements for my monitoring equipment?
(a) For each negative pressure baghouse or positive pressure
baghouse equipped with a stack, applied to meet any particulate emission
limit in Table 1 to this subpart, you must install, operate, and
maintain a bag leak detection system according to the requirements in
paragraphs (a)(1) through (8) of this section.
(1) The system must be certified by the manufacturer to be capable
of detecting emissions of particulate matter at concentrations of 10
milligrams per actual cubic meter (0.0044 grains per actual cubic foot)
or less.
(2) The system must provide output of relative changes in
particulate matter loadings.
(3) The system must be equipped with an alarm that will sound when
an increase in relative particulate loadings is detected over the alarm
level set point established according to paragraph (a)(4) of this
section. The alarm must be located such that it can be heard by the
appropriate plant personnel.
(4) For each bag leak detection system, you must develop and submit
to the Administrator for approval, a site-specific monitoring plan that
addresses the items identified in paragraphs (a)(4)(i) through (v) of
this section. For each bag leak detection system that operates based on
the triboelectric effect, the monitoring plan shall be consistent with
the recommendations contained in the U.S. Environmental Protection
Agency (U.S. EPA) guidance document, ``Fabric Filter Bag Leak Detection
Guidance'' (EPA-454/R-98-015). This document is available on the EPA's
Technology Transfer Network at http://www.epa.gov/ttn/emc/cem/tribo.pdf
(Adobe Acrobat version) or http://www.epa.gov/ttn/emc/cem/tribo.wpd
(WordPerfect version). You must operate and maintain the bag leak
detection system according to the site-specific monitoring plan at all
times. The plan shall describe all of the items in paragraphs (a)(4)(i)
through (v) of this section.
(i) Installation of the bag leak detection system.
(ii) Initial and periodic adjustment of the bag leak detection
system including how the alarm set-point will be established.
(iii) Operation of the bag leak detection system including quality
assurance procedures.
(iv) How the bag leak detection system will be maintained including
a routine maintenance schedule and spare parts inventory list.
[[Page 75]]
(v) How the bag leak detection system output shall be recorded and
stored.
(5) To make the initial adjustment of the system, establish the
baseline output by adjusting the sensitivity (range) and the averaging
period of the device. Then, establish the alarm set points and the alarm
delay time (if applicable).
(6) Following initial adjustment, do not adjust averaging period,
alarm set point, or alarm delay time, without approval from the
Administrator except as provided for in paragraph (a)(6)(i) of this
section.
(i) Once per quarter, you may adjust the sensitivity of the bag leak
detection system to account for seasonal effects, including temperature
and humidity, according to the procedures identified in the site-
specific monitoring plan required under paragraph (a)(4) of this
section.
(ii) [Reserved]
(7) Where multiple detectors are required, the system's
instrumentation and alarm may be shared among detectors.
(8) The bag leak detector sensor must be installed downstream of the
baghouse and upstream of any wet scrubber.
(b) For each CPMS required in Sec. 63.9631, you must develop and
make available for inspection upon request by the permitting authority a
site-specific monitoring plan that addresses the requirements in
paragraphs (b)(1) through (7) of this section.
(1) Installation of the CPMS sampling probe or other interface at a
measurement location relative to each affected emission unit such that
the measurement is representative of control of the exhaust emissions
(e.g., on or downstream of the last control device).
(2) Performance and equipment specifications for the sample
interface, the parametric signal analyzer, and the data collection and
reduction system.
(3) Performance evaluation procedures and acceptance criteria (e.g.,
calibrations).
(4) Ongoing operation and maintenance procedures in accordance with
the general requirements of Sec. 63.8(c)(1), (3), (4)(ii), (7), and
(8).
(5) Ongoing data quality assurance procedures in accordance with the
general requirements of Sec. 63.8(d).
(6) Ongoing recordkeeping and reporting procedures in accordance
with the general requirements of Sec. 63.10(c), (e)(1), and (e)(2)(i).
(7) Corrective action procedures that you will follow in the event
an air pollution control device, except for a baghouse, exceeds an
established operating limit as required in Sec. 63.9600(b)(3).
(c) Unless otherwise specified, each CPMS must meet the requirements
in paragraphs (c)(1) and (2) of this section.
(1) Each CPMS must complete a minimum of one cycle of operation for
each successive 15-minute period and must have valid data for at least
95 percent of every daily averaging period.
(2) Each CPMS must determine and record the daily average of all
recorded readings.
(d) You must conduct a performance evaluation of each CPMS in
accordance with your site-specific monitoring plan.
(e) You must operate and maintain the CPMS in continuous operation
according to the site-specific monitoring plan.
(f) For each dry electrostatic precipitator subject to the opacity
operating limit in Sec. 63.9590(b)(3)(i), you must install, operate,
and maintain each COMS according to the requirements in paragraphs
(f)(1) through (4) of this section.
(1) You must install each COMS and conduct a performance evaluation
of each COMS according to Sec. 63.8 and Performance Specification 1 in
appendix B to 40 CFR part 60.
(2) You must develop and implement a quality control program for
operating and maintaining each COMS according to Sec. 63.8. At a
minimum, the quality control program must include a daily calibration
drift assessment, quarterly performance audit, and annual zero alignment
of each COMS.
(3) You must operate and maintain each COMS according to Sec.
63.8(e) and your quality control program. You must also identify periods
the COMS is out of control, including any periods that the COMS fails to
pass a daily calibration drift assessment, quarterly
[[Page 76]]
performance audit, or annual zero alignment audit.
(4) You must determine and record the 6-minute average opacity for
periods during which the COMS is not out of control.
Sec. 63.9633 How do I monitor and collect data to demonstrate continuous
compliance?
(a) Except for monitoring malfunctions, associated repairs, and
required quality assurance or control activities (including as
applicable, calibration checks and required zero and span adjustments),
you must monitor continuously (or collect data at all required
intervals) at all times an affected source is operating.
(b) You may not use data recorded during monitoring malfunctions,
associated repairs, and required quality assurance or control activities
in data averages and calculations used to report emission or operating
levels, or to fulfill a minimum data availability requirement. You must
use all the data collected during all other periods in assessing
compliance.
(c) A monitoring malfunction is any sudden, infrequent, not
reasonably preventable failure of the monitoring system to provide valid
data. Monitoring failures that are caused in part by poor maintenance or
careless operation are not considered malfunctions.
Sec. 63.9634 How do I demonstrate continuous compliance with the emission
limitations that apply to me?
(a) For each affected source subject to an emission limit in Table 1
to this subpart, you must demonstrate continuous compliance by meeting
the requirements in paragraphs (b) through (f) of this section.
(b) For ore crushing and handling affected sources and finished
pellet handling affected sources, you must demonstrate continuous
compliance by meeting the requirements in paragraphs (b)(1) through (3)
of this section.
(1) The flow-weighted mean concentration of particulate matter for
all ore crushing and handling emission units and for all finished pellet
handling emission units must be maintained at or below the emission
limits in Table 1 to this subpart.
(2) You must conduct subsequent performance tests for emission units
in the ore crushing and handling and finished pellet handling affected
sources following the schedule in your title V permit. If a title V
permit has not been issued, you must conduct subsequent performance
tests according to a testing plan approved by the Administrator or
delegated authority.
(3) For emission units not selected for initial performance testing
and defined within a group of similar emission units in accordance with
Sec. 63.9620(e), you must calculate the daily average value of each
operating parameter for the similar air pollution control device applied
to each similar emission unit within a defined group using Equation 1 of
this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.004
Where:
Pk = Daily average operating parameter value for all emission
units within group ``k'';
Pi = Daily average parametric monitoring parameter value
corresponding to emission unit ``i'' within group ``k''; and
n = Total number of emission units within group, including emission
units that have been selected for performance tests and those that have
not been selected for performance tests.
(c) For ore dryers and indurating furnaces, you must demonstrate
continuous compliance by meeting the requirements in paragraphs (c)(1)
and (2) of this section.
(1) The flow-weighted mean concentration of particulate matter for
all stacks from the ore dryer or indurating furnace must be maintained
at or below the emission limits in Table 1 to this subpart.
(2) For ore dryers, you must conduct subsequent performance tests
following the schedule in your title V permit. For indurating furnaces,
you must conduct subsequent performance tests following the schedule in
your title V permit, but no less frequent than twice per 5-year permit
term. If a title V permit has not been issued, you must conduct
subsequent performance tests according to a testing plan approved by
[[Page 77]]
the Administrator or delegated authority.
(d) For each baghouse applied to meet any particulate emission limit
in Table 1 to this subpart, you must demonstrate continuous compliance
by completing the requirements in paragraphs (d)(1) and (2) of this
section.
(1) Maintaining records of the time you initiated corrective action
in the event of a bag leak detection system alarm, the corrective
action(s) taken, and the date on which corrective action was completed.
(2) Inspecting and maintaining each baghouse according to the
requirements in Sec. 63.9631(a)(1) through (8) and recording all
information needed to document conformance with these requirements. If
you increase or decrease the sensitivity of the bag leak detection
system beyond the limits specified in your site-specific monitoring
plan, you must include a copy of the required written certification by a
responsible official in the next semiannual compliance report.
(e) Except as provided in paragraph (f) of this section, for each
wet scrubber subject to the operating limits for pressure drop and
scrubber water flow rate in Sec. 63.9590(b)(1), you must demonstrate
continuous compliance by completing the requirements of paragraphs
(e)(1) through (4) of this section.
(1) Maintaining the daily average pressure drop and daily average
scrubber water flow rate at or above the minimum levels established
during the initial or subsequent performance test.
(2) Operating and maintaining each wet scrubber CPMS according to
Sec. 63.9632(b) and recording all information needed to document
conformance with these requirements.
(3) Collecting and reducing monitoring data for pressure drop and
scrubber water flow rate according to Sec. 63.9632(c) and recording all
information needed to document conformance with these requirements.
(4) If the daily average pressure drop or daily average scrubber
water flow rate is below the operating limits established for a
corresponding emission unit or group of similar emission units, you must
then follow the corrective action procedures in paragraph (j) of this
section.
(f) For each dynamic wet scrubber subject to the operating limits
for scrubber water flow rate and either the fan amperage or pressure
drop in Sec. 63.9590(b)(2), you must demonstrate continuous compliance
by completing the requirements of paragraphs (f)(1) through (4) of this
section.
(1) Maintaining the daily average scrubber water flow rate and
either the daily average fan amperage or the daily average pressure drop
at or above the minimum levels established during the initial or
subsequent performance test.
(2) Operating and maintaining each dynamic wet scrubber CPMS
according to Sec. 63.9632(b) and recording all information needed to
document conformance with these requirements.
(3) Collecting and reducing monitoring data for scrubber water flow
rate and either fan amperage or pressure drop according to Sec.
63.9632(c) and recording all information needed to document conformance
with these requirements.
(4) If the daily average scrubber water flow rate, daily average fan
amperage, or daily average pressure drop is below the operating limits
established for a corresponding emission unit or group of similar
emission units, you must then follow the corrective action procedures in
paragraph (j) of this section.
(g) For each dry electrostatic precipitator subject to operating
limits in Sec. 63.9590(b)(3), you must demonstrate continuous
compliance by completing the requirements of paragraph (g)(1) or (2) of
this section.
(1) If the operating limit for your dry electrostatic precipitator
is a 6-minute average opacity of emissions value, then you must follow
the requirements in paragraphs (g)(1)(i) through (iii) of this section.
(i) Maintaining the 6-minute average opacity of emissions at or
below the maximum level established during the initial or subsequent
performance test.
(ii) Operating and maintaining each COMS and reducing the COMS data
according to Sec. 63.9632(f).
(iii) If the 6-minute average opacity of emissions is above the
operating limits established for a corresponding emission unit, you must
then follow
[[Page 78]]
the corrective action procedures in paragraph (j) of this section.
(2) If the operating limit for your dry electrostatic precipitator
is the daily average secondary voltage and daily average secondary
current for each field, then you must follow the requirements in
paragraphs (g)(2)(i) through (iv) of this section.
(i) Maintaining the daily average secondary voltage or daily average
secondary current for each field at or above the minimum levels
established during the initial or subsequent performance test.
(ii) Operating and maintaining each dry electrostatic precipitator
CPMS according to Sec. 63.9632(b) and recording all information needed
to document conformance with these requirements.
(iii) Collecting and reducing monitoring data for secondary voltage
or secondary current for each field according to Sec. 63.9632(c) and
recording all information needed to document conformance with these
requirements.
(iv) If the daily average secondary voltage or daily average
secondary current for each field is below the operating limits
established for a corresponding emission unit, you must then follow the
corrective action procedures in paragraph (j) of this section.
(h) For each wet electrostatic precipitator subject to the operating
limits for secondary voltage, stack outlet temperature, and water flow
rate in Sec. 63.9590(b)(4), you must demonstrate continuous compliance
by completing the requirements of paragraphs (h)(1) through (4) of this
section.
(1) Maintaining the daily average secondary voltage, daily average
secondary current, and daily average scrubber water flow rate for each
field at or above the minimum levels established during the initial or
subsequent performance test. Maintaining the daily average stack outlet
temperature at or below the maximum levels established during the
initial or subsequent performance test.
(2) Operating and maintaining each wet electrostatic precipitator
CPMS according to Sec. 63.9632(b) and recording all information needed
to document conformance with these requirements.
(3) Collecting and reducing monitoring data for secondary voltage,
stack outlet temperature, and water flow rate according to Sec.
63.9632(c) and recording all information needed to document conformance
with these requirements.
(4) If the daily average secondary voltage, stack outlet
temperature, or water flow rate does not meet the operating limits
established for a corresponding emission unit, you must then follow the
corrective action procedures in paragraph (j) of this section.
(i) If you use an air pollution control device other than a wet
scrubber, dynamic wet scrubber, dry electrostatic precipitator, wet
electrostatic precipitator, or baghouse, you must submit a site-specific
monitoring plan in accordance with Sec. 63.9631(f). The site-specific
monitoring plan must include the site-specific procedures for
demonstrating initial and continuous compliance with the corresponding
operating limits.
(j) If the daily average operating parameter value for an emission
unit or group of similar emission units does not meet the corresponding
established operating limit, you must then follow the procedures in
paragraphs (j)(1) through (4) of this section.
(1) You must initiate and complete initial corrective action within
10 calendar days and demonstrate that the initial corrective action was
successful. During any period of corrective action, you must continue to
monitor and record all required operating parameters for equipment that
remains in operation. After 10 calendar days, measure and record the
daily average operating parameter value for the emission unit or group
of similar emission units on which corrective action was taken. After
the initial corrective action, if the daily average operating parameter
value for the emission unit or group of similar emission units meets the
operating limit established for the corresponding unit or group, then
the corrective action was successful and the emission unit or group of
similar emission units is in compliance with the established operating
limits.
(2) If the initial corrective action required in paragraph (j)(1) of
this section was not successful, then you must complete additional
corrective action
[[Page 79]]
within 10 calendar days and demonstrate that the subsequent corrective
action was successful. During any period of corrective action, you must
continue to monitor and record all required operating parameters for
equipment that remains in operation. After the second set of 10 calendar
days allowed to implement corrective action, you must again measure and
record the daily average operating parameter value for the emission unit
or group of similar emission units. If the daily average operating
parameter value for the emission unit or group of similar emission units
meets the operating limit established for the corresponding unit or
group, then the corrective action was successful and the emission unit
or group of similar emission units is in compliance with the established
operating limits.
(3) If the second attempt at corrective action required in paragraph
(j)(2) of this section was not successful, then you must repeat the
procedures of paragraph (j)(2) of this section until the corrective
action is successful. If the third attempt at corrective action is
unsuccessful, you must conduct another performance test in accordance
with the procedures in Sec. 63.9622(f) and report to the Administrator
as a deviation the third unsuccessful attempt at corrective action.
(4) After the third unsuccessful attempt at corrective action, you
must submit to the Administrator the written report required in
paragraph (j)(3) of this section within 5 calendar days after the third
unsuccessful attempt at corrective action. This report must notify the
Administrator that a deviation has occurred and document the types of
corrective measures taken to address the problem that resulted in the
deviation of established operating parameters and the resulting
operating limits.
Sec. 63.9635 How do I demonstrate continuous compliance with the work
practice standards that apply to me?
(a) You must demonstrate continuous compliance with the work
practice standard requirements in Sec. 63.9591 by operating in
accordance with your fugitive dust emissions control plan at all times.
(b) You must maintain a current copy of the fugitive dust emissions
control plan required in Sec. 63.9591 onsite and it must be available
for inspection upon request. You must keep the plan for the life of the
affected source or until the affected source is no longer subject to the
requirements of this subpart.
Sec. 63.9636 How do I demonstrate continuous compliance with the
operation and maintenance requirements that apply to me?
(a) For each control device subject to an operating limit in Sec.
63.9590(b), you must demonstrate continuous compliance with the
operation and maintenance requirements in Sec. 63.9600(b) by completing
the requirements of paragraphs (a)(1) through (4) of this section.
(1) Performing preventative maintenance for each control device in
accordance with Sec. 63.9600(b)(1) and recording all information needed
to document conformance with these requirements;
(2) Initiating and completing corrective action for a bag leak
detection system alarm in accordance with Sec. 63.9600(b)(2) and
recording all information needed to document conformance with these
requirements;
(3) Initiating and completing corrective action for a CPMS when you
exceed an established operating limit for an air pollution control
device except for a baghouse in accordance with Sec. 63.9600(b)(3) and
recording all information needed to document conformance with these
requirements; and
(4) Implementing and maintaining site-specific good combustion
practices for each indurating furnace in accordance with Sec.
63.9600(b)(4) and recording all information needed to document
conformance with these requirements.
(b) You must maintain a current copy of the operation and
maintenance plan required in Sec. 63.9600(b) onsite, and it must be
available for inspection upon request. You must keep the plan for the
life of the affected source or until the affected source is no longer
subject to the requirements of this subpart.
[[Page 80]]
Sec. 63.9637 What other requirements must I meet to demonstrate
continuous compliance?
(a) Deviations. You must report each instance in which you did not
meet each emission limitation in Table 1 to this subpart that applies to
you. This includes periods of startup, shutdown, and malfunction in
accordance with paragraph (b) of this section. You also must report each
instance in which you did not meet the work practice standards in Sec.
63.9591 and each instance in which you did not meet each operation and
maintenance requirement in Sec. 63.9600 that applies to you. These
instances are deviations from the emission limitations, work practice
standards, and operation and maintenance requirements in this subpart.
These deviations must be reported in accordance with the requirements in
Sec. 63.9641.
(b) Startups, shutdowns, and malfunctions. (1) Consistent with
Sec. Sec. 63.6(e) and 63.7(e)(1), deviations that occur during a period
of startup, shutdown, or malfunction are not violations if you
demonstrate to the Administrator's satisfaction that you were operating
in accordance with Sec. 63.6(e)(1).
(2) The Administrator will determine whether deviations that occur
during a period of startup, shutdown, or malfunction are violations,
according to the provisions in Sec. 63.6(e).
[68 FR 61888, Oct. 30, 2003, as amended at 71 FR 20471, Apr. 20, 2006]
Notifications, Reports, and Records
Sec. 63.9640 What notifications must I submit and when?
(a) You must submit all of the notifications in Sec. Sec. 63.7(b)
and (c), 63.8(f)(4), and 63.9(b) through (h) that apply to you by the
specified dates.
(b) As specified in Sec. 63.9(b)(2), if you start up your affected
source before October 30, 2003, you must submit your initial
notification no later than 120 calendar days after October 30, 2003.
(c) As specified in Sec. 63.9(b)(3), if you start up your new
affected source on or after October 30, 2003, you must submit your
initial notification no later than 120 calendar days after you become
subject to this subpart.
(d) If you are required to conduct a performance test, you must
submit a notification of intent to conduct a performance test at least
60 calendar days before the performance test is scheduled to begin, as
required in Sec. 63.7(b)(1).
(e) If you are required to conduct a performance test or other
initial compliance demonstration, you must submit a notification of
compliance status according to Sec. 63.9(h)(2)(ii). The initial
notification of compliance status must be submitted by the dates
specified in paragraphs (e)(1) and (2) of this section.
(1) For each initial compliance demonstration that does not include
a performance test, you must submit the notification of compliance
status before the close of business on the 30th calendar day following
completion of the initial compliance demonstration.
(2) For each initial compliance demonstration that does include a
performance test, you must submit the notification of compliance status,
including the performance test results, before the close of business on
the 60th calendar day following the completion of the performance test
according to Sec. 63.10(d)(2).
Sec. 63.9641 What reports must I submit and when?
(a) Compliance report due dates. Unless the Administrator has
approved a different schedule, you must submit a semiannual compliance
report to your permitting authority according to the requirements in
paragraphs (a)(1) through (5) of this section.
(1) The first compliance report must cover the period beginning on
the compliance date that is specified for your affected source in Sec.
63.9583 and ending on June 30 or December 31, whichever date comes first
after the compliance date that is specified for your source in Sec.
63.9583.
(2) The first compliance report must be postmarked or delivered no
later than July 31 or January 31, whichever date comes first after your
first compliance report is due.
(3) Each subsequent compliance report must cover the semiannual
reporting period from January 1 through June 30 or the semiannual
reporting period from July 1 through December 31.
(4) Each subsequent compliance report must be postmarked or
delivered
[[Page 81]]
no later than July 31 or January 31, whichever date comes first after
the end of the semiannual reporting period.
(5) For each affected source that is subject to permitting
regulations pursuant to 40 CFR part 70 or 40 CFR part 71, and if the
permitting authority has established dates for submitting semiannual
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance
reports according to the dates the permitting authority has established
instead of according to the dates in paragraphs (a)(1) through (4) of
this section.
(b) Compliance report contents. Each compliance report must include
the information in paragraphs (b)(1) through (3) of this section and, as
applicable, in paragraphs (b)(4) through (8) of this section.
(1) Company name and address.
(2) Statement by a responsible official, with the official's name,
title, and signature, certifying the truth, accuracy, and completeness
of the content of the report.
(3) Date of report and beginning and ending dates of the reporting
period.
(4) If you had a startup, shutdown, or malfunction during the
reporting period and you took actions consistent with your startup,
shutdown, and malfunction plan, the compliance report must include the
information in Sec. 63.10(d)(5)(i).
(5) If there were no deviations from the continuous compliance
requirements in Sec. Sec. 63.9634 through 63.9636 that apply to you,
then provide a statement that there were no deviations from the emission
limitations, work practice standards, or operation and maintenance
requirements during the reporting period.
(6) If there were no periods during which a continuous monitoring
system (including a CPMS or COMS) was out-of-control as specified in
Sec. 63.8(c)(7), then provide a statement that there were no periods
during which a continuous monitoring system was out-of-control during
the reporting period.
(7) For each deviation from an emission limitation in Table 1 to
this subpart that occurs at an affected source where you are not using a
continuous monitoring system (including a CPMS or COMS) to comply with
an emission limitation in this subpart, the compliance report must
contain the information in paragraphs (b)(1) through (4) of this section
and the information in paragraphs (b)(7)(i) and (ii) of this section.
This includes periods of startup, shutdown, and malfunction.
(i) The total operating time of each affected source during the
reporting period.
(ii) Information on the number, duration, and cause of deviations
(including unknown cause) as applicable, and the corrective action
taken.
(8) For each deviation from an emission limitation occurring at an
affected source where you are using a continuous monitoring system
(including a CPMS or COMS) to comply with the emission limitation in
this subpart, you must include the information in paragraphs (b)(1)
through (4) of this section and the information in paragraphs (b)(8)(i)
through (xi) of this section. This includes periods of startup,
shutdown, and malfunction.
(i) The date and time that each malfunction started and stopped.
(ii) The date and time that each continuous monitoring system was
inoperative, except for zero (low-level) and high-level checks.
(iii) The date, time, and duration that each continuous monitoring
system was out-of-control, including the information in Sec.
63.8(c)(8).
(iv) The date and time that each deviation started and stopped, and
whether each deviation occurred during a period of startup, shutdown, or
malfunction or during another period.
(v) A summary of the total duration of the deviation during the
reporting period and the total duration as a percent of the total source
operating time during that reporting period.
(vi) A breakdown of the total duration of the deviations during the
reporting period including those that are due to startup, shutdown,
control equipment problems, process problems, other known causes, and
other unknown causes.
(vii) A summary of the total duration of continuous monitoring
system downtime during the reporting period and the total duration of
continuous
[[Page 82]]
monitoring system downtime as a percent of the total source operating
time during the reporting period.
(viii) A brief description of the process units.
(ix) A brief description of the continuous monitoring system.
(x) The date of the latest continuous monitoring system
certification or audit.
(xi) A description of any changes in continuous monitoring systems,
processes, or controls since the last reporting period.
(c) Immediate startup, shutdown, and malfunction report. If you had
a startup, shutdown, or malfunction during the semiannual reporting
period that was not consistent with your startup, shutdown, and
malfunction plan, you must submit an immediate startup, shutdown, and
malfunction report according to the requirements in Sec.
63.10(d)(5)(ii).
(d) Part 70 monitoring report. If you have obtained a title V
operating permit for an affected source pursuant to 40 CFR part 70 or 40
CFR part 71, you must report all deviations as defined in this subpart
in the semiannual monitoring report required by 40 CFR
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A). If you submit a
compliance report for an affected source along with, or as part of, the
semiannual monitoring report required by 40 CFR 70.6(a)(3)(iii)(A) or 40
CFR 71.6(a)(3)(iii)(A), and the compliance report includes all the
required information concerning deviations from any emission limitation
or operation and maintenance requirement in this subpart, submission of
the compliance report satisfies any obligation to report the same
deviations in the semiannual monitoring report. However, submission of a
compliance report does not otherwise affect any obligation you may have
to report deviations from permit requirements for an affected source to
your permitting authority.
(e) Immediate corrective action report. If you had three
unsuccessful attempts of applying corrective action as described in
Sec. 63.9634(j) on an emission unit or group of emission units, then
you must submit an immediate corrective action report. Within 5 calendar
days after the third unsuccessful attempt at corrective action, you must
submit to the Administrator a written report in accordance with Sec.
63.9634(j)(3) and (4). This report must notify the Administrator that a
deviation has occurred and document the types of corrective measures
taken to address the problem that resulted in the deviation of
established operating parameters and the resulting operating limits.
Sec. 63.9642 What records must I keep?
(a) You must keep the records listed in paragraphs (a)(1) through
(3) of this section.
(1) A copy of each notification and report that you submitted to
comply with this subpart, including all documentation supporting any
initial notification or notification of compliance status that you
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
(2) The records in Sec. 63.6(e)(3)(iii) through (v) related to
startup, shutdown, and malfunction.
(3) Records of performance tests and performance evaluations as
required in Sec. 63.10(b)(2)(viii).
(b) For each COMS, you must keep the records specified in paragraphs
(b)(1) through (4) of this section.
(1) Records described in Sec. 63.10(b)(2)(vi) through (xi).
(2) Monitoring data for COMS during a performance evaluation as
required in Sec. 63.6(h)(7)(i) and (ii).
(3) Previous (that is, superceded) versions of the performance
evaluation plan as required in Sec. 63.8(d)(3).
(4) Records of the date and time that each deviation started and
stopped, and whether the deviation occurred during a period of startup,
shutdown, or malfunction or during another period.
(c) You must keep the records required in Sec. Sec. 63.9634 through
63.9636 to show continuous compliance with each emission limitation,
work practice standard, and operation and maintenance requirement that
applies to you.
Sec. 63.9643 In what form and how long must I keep my records?
(a) Your records must be in a form suitable and readily available
for expeditious review, according to Sec. 63.10(b)(1).
[[Page 83]]
(b) As specified in Sec. 63.10(b)(1), you must keep each record for
5 years following the date of each occurrence, measurement, maintenance,
corrective action, report, or record.
(c) You must keep each record on site for at least 2 years after the
date of each occurrence, measurement, maintenance, corrective action,
report, or record according to Sec. 63.10(b)(1). You can keep the
records offsite for the remaining 3 years.
Other Requirements and Information
Sec. 63.9650 What parts of the General Provisions apply to me?
Table 2 to this subpart shows which parts of the General Provisions
in Sec. Sec. 63.1 through 63.15 apply to you.
Sec. 63.9651 Who implements and enforces this subpart?
(a) This subpart can be implemented and enforced by us, the EPA, or
a delegated authority such as your State, local, or tribal agency. If
the EPA Administrator has delegated authority to your State, local, or
tribal agency, then that agency has the authority to implement and
enforce this subpart. You should contact your EPA Regional Office to
find out if this subpart is delegated to your State, local, or tribal
agency.
(b) In delegating implementation and enforcement authority of this
subpart to a State, local, or tribal agency under subpart E of this
part, the authorities contained in paragraph (c) of this section are
retained by the Administrator of the EPA and are not transferred to the
State, local, or tribal agency.
(c) The authorities that will not be delegated to State, local, or
tribal agencies are specified in paragraphs (c)(1) through (4) of this
section.
(1) Approval of non-opacity emission limitations and work practice
standards under Sec. 63.6(h)(9) and as defined in Sec. 63.90.
(2) Approval of major alternatives to test methods under Sec.
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
(3) Approval of major alternatives to monitoring under Sec. 63.8(f)
and as defined in Sec. 63.90.
(4) Approval of major alternatives to recordkeeping and reporting
under Sec. 63.10(f) and as defined in Sec. 63.90.
Sec. 63.9652 What definitions apply to this subpart?
Terms used in this subpart are defined in the Clean Air Act, in
Sec. 63.2, and in this section as follows.
Affected source means each new or existing ore crushing and handling
operation, ore dryer, indurating furnace, or finished pellet handling
operation, at your taconite iron ore processing plant.
Bag leak detection system means a system that is capable of
continuously monitoring relative particulate matter (dust) loadings in
the exhaust of a baghouse to detect bag leaks and other upset
conditions. A bag leak detection system includes, but is not limited to,
an instrument that operates on triboelectric, light scattering, light
transmittance, or other effect to continuously monitor relative
particulate matter loadings.
Conveyor belt transfer point means a point in the conveying
operation where the taconite ore or taconite pellets are transferred to
or from a conveyor belt, except where the taconite ore or taconite
pellets are being transferred to a bin or stockpile.
Crusher means a machine used to crush taconite ore and includes
feeders or conveyors located immediately below the crushing surfaces.
Crushers include, but are not limited to, gyratory crushers and cone
crushers.
Deviation means any instance in which an affected source subject to
this subpart, or an owner or operator of such a source:
(1) Fails to meet any requirement or obligation established by this
subpart, including but not limited to any emission limitation (including
operating limits) or operation and maintenance requirement;
(2) Fails to meet any term or condition that is adopted to implement
an applicable requirement in this subpart and that is included in the
operating permit for any affected source required to obtain such a
permit; or
(3) Fails to meet any emission limitation in this subpart during
startup, shutdown, or malfunction, regardless
[[Page 84]]
of whether or not such failure is permitted by this subpart.
Dynamic wet scrubber means an air emissions control device which
utilizes a mechanically powered fan to cause contact between the process
exhaust gas stream and the scrubbing liquid which are introduced
concurrently into the fan inlet.
Emission limitation means any emission limit, opacity limit, or
operating limit.
Finished pellet handling means the transfer of fired taconite
pellets from the indurating furnace to the finished pellet stockpiles at
the plant. Finished pellet handling includes, but is not limited to,
furnace discharge or grate discharge, and finished pellet screening,
transfer, and storage. The atmospheric pellet cooler vent stack and
gravity conveyor gallery vents designed to remove heat and water vapor
from the structure are not included as a part of the finished pellet
handling affected source.
Fugitive dust emission source means a stationary source from which
particles are discharged to the atmosphere due to wind or mechanical
inducement such as vehicle traffic. Fugitive dust sources include, but
are not limited to:
(1) Stockpiles (includes, but is not limited to, stockpiles of
uncrushed ore, crushed ore, or finished pellets);
(2) Material transfer points;
(3) Plant roadways;
(4) Tailings basins;
(5) Pellet loading areas; and
(6) Yard areas.
Grate feed means the transfer of unfired taconite pellets from the
pelletizer into the indurating furnace.
Grate kiln indurating furnace means a furnace system that consists
of a traveling grate, a rotary kiln, and an annular cooler. The grate
kiln indurating furnace begins at the point where the grate feed
conveyor discharges the green balls onto the furnace traveling grate and
ends where the hardened pellets exit the cooler. The atmospheric pellet
cooler vent stack is not included as part of the grate kiln indurating
furnace.
Indurating means the process whereby unfired taconite pellets,
called green balls, are hardened at high temperature in an indurating
furnace. Types of indurating furnaces include straight grate indurating
furnaces and grate kiln indurating furnaces.
Ore crushing and handling means the process whereby dry taconite ore
is crushed and screened. Ore crushing and handling includes, but is not
limited to, all dry crushing operations (e.g., primary, secondary, and
tertiary crushing), dry ore conveyance and transfer points, dry ore
classification and screening, dry ore storage and stockpiling, dry
milling, dry cobbing (i.e., dry magnetic separation), and the grate
feed. Ore crushing and handling specifically excludes any operations
where the dry crushed ore is saturated with water, such as wet milling
and wet magnetic separation.
Ore dryer means a rotary dryer that repeatedly tumbles wet taconite
ore concentrate through a heated air stream to reduce the amount of
entrained moisture in the taconite ore concentrate.
Pellet cooler vent stacks means atmospheric vents in the cooler
section of the grate kiln indurating furnace that exhaust cooling air
that is not returned for recuperation. Pellet cooler vent stacks are not
to be confused with the cooler discharge stack, which is in the pellet
loadout or dumping area.
Pellet loading area means that portion of a taconite iron ore
processing plant where taconite pellets are loaded into trucks or
railcars.
Responsible official means responsible official as defined in Sec.
63.2.
Rod-deck venturi scrubber means a wet scrubber emission control
device in which the inlet air flows through a bed of parallel metal
pipes spaced apart to produce a series of parallel venturi throats.
Screen means a device for separating material according to size by
passing undersize material through one or more mesh surfaces (screens)
in series and retaining oversize material on the mesh surfaces
(screens).
Storage bin means a facility for storage (including surge bins and
hoppers) of taconite ore or taconite pellets prior to further processing
or loading.
Straight grate indurating furnace means a furnace system that
consists of a traveling grate that carries the
[[Page 85]]
taconite pellets through different furnace temperature zones. In the
straight grate indurating furnace a layer of fired pellets, called the
hearth layer, is placed on the traveling grate prior to the addition of
unfired pellets. The straight grate indurating furnace begins at the
point where the grate feed conveyor discharges the green balls onto the
furnace traveling grate and ends where the hardened pellets drop off of
the traveling grate.
Taconite iron ore processing means the separation and concentration
of iron ore from taconite, a low-grade iron ore, to produce taconite
pellets.
Taconite ore means a low-grade iron ore suitable for concentration
of magnetite or hematite by fine grinding and magnetic or flotation
treatment, from which pellets containing iron can be produced.
Tailings basin means a natural or artificial impoundment in which
gangue or other refuse material resulting from the washing,
concentration or treatment of ground taconite iron ore is confined.
Wet grinding and milling means the process whereby wet taconite ore
is finely ground using rod and/or ball mills.
Table 1 to Subpart RRRRR of Part 63--Emission Limits
As required in Sec. 63.9590(a), you must comply with each
applicable emission limit in the following table:
----------------------------------------------------------------------------------------------------------------
then you must comply with the
flow-weighted mean
concentration of particulate
matter discharged to the
If your affected source is . . . and the affected source is categorized as atmosphere from the affected
. . . source, as determined using
the procedures in Sec.
63.9621(b), such that you
must not exceed . . .
----------------------------------------------------------------------------------------------------------------
1. Ore crushing and handling emission Existing.................................. 0.008 grains per dry standard
units. cubic foot (gr/dscf).
New....................................... 0.005 gr/dscf.
2. Straight grate indurating furnace Existing.................................. 0.01 gr/dscf.
processing magnetite. New....................................... 0.006 gr/dscf.
3. Grate kiln indurating furnace Existing.................................. 0.01 gr/dscf.
processing magnetite. New....................................... 0.006 gr/dscf.
4. Grate kiln indurating furnace Existing.................................. 0.03 gr/dscf.
processing hematite. New....................................... 0.018 gr/dscf.
5. Finished pellet handling emission Existing.................................. 0.008 gr/dscf.
units. New....................................... 0.005 gr/dscf.
6. Ore dryer......................... Existing.................................. 0.052 gr/dscf.
New....................................... 0.025 gr/dscf.
----------------------------------------------------------------------------------------------------------------
Table 2 to Subpart RRRRR of Part 63--Applicability of General Provisions
to Subpart RRRRR of Part 63
As required in Sec. 63.9650, you must comply with the requirements
of the NESHAP General Provisions (40 CFR part 63, subpart A) shown in
the following table:
----------------------------------------------------------------------------------------------------------------
Citation Subject Applies to Subpart RRRRR Explanation
----------------------------------------------------------------------------------------------------------------
Sec. 63.1....................... Applicability......... Yes.
Sec. 63.2....................... Definitions........... Yes.
Sec. 63.3....................... Units and Yes.
Abbreviations.
Sec. 63.4....................... Prohibited Activities. Yes.
Sec. 63.5....................... Construction/ Yes.
Reconstruction.
Sec. 63.6(a)-(g)................ Compliance With Yes.
Standards and
Maintenance
Requirements.
Sec. 63.6(h).................... Compliance With No........................... Subpart RRRRR does
Opacity and Visible not contain opacity
Emission (VE) and VE standards.
Standards.
Sec. 63.6(i), (j)............... Extension of Yes.
Compliance and
Presidential
Compliance Extension.
Sec. 63.7(a)(1)-(2)............. Applicability and No........................... Subpart RRRRR
Performance Test specifies
Dates. performance test
applicability and
dates.
[[Page 86]]
Sec. 63.7(a)(3), (b)-(h)........ Performance Testing Yes.
Requirements.
Sec. 63.8(a)(1)-(a)(3), (b), Monitoring Yes.......................... Continuous monitoring
(c)(1)-(3), (c)(5)-(8), (d), (e), Requirements. system (CMS)
(f)(1)-(5), (g)(1)-(4). requirements in Sec.
63.8(c)(5) and (6)
apply only to COMS
for dry
electrostatic
precipitators.
Sec. 63.8(a)(4)................. Additional Monitoring No........................... Subpart RRRRR does
Requirements for not require flares.
Control Devices in
Sec. 63.11.
Sec. 63.8(c)(4)................. Continuous Monitoring No........................... Subpart RRRRR
System Requirements. specifies
requirements for
operation of CMS.
Sec. 63.8(f)(6)................. Relative Accuracy Test No........................... Subpart RRRRR does
Alternative (RATA). not require
continuous emission
monitoring systems.
Sec. 63.8(g)(5)................. Data Reduction........ No........................... Subpart RRRRR
specifies data
reduction
requirements.
Sec. 63.9....................... Notification Yes.......................... Additional
Requirements. notifications for
CMS in Sec.
63.9(g) apply to
COMS for dry
electrostatic
precipitators.
Sec. 63.10(a), (b)(1)-(2)(xii), Recordkeeping and Yes.......................... Additional records
(b)(2)(xiv), (b)(3), (c)(1)-(6), Reporting for CMS in Sec.
(c)(9)-(15), (d)(1)-(2), (d)(4)- Requirements. 63.10(c)(1)-(6), (9)-
(5), (e), (f). (15), and reports in
Sec. 63.10(d)(1)-
(2) apply only to
COMS for dry
electrostatic
precipitators.
Sec. 63.10(b)(2)(xiii).......... CMS Records for RATA No........................... Subpart RRRRR doesn't
Alternative. require continuous
emission monitoring
systems.
Sec. 63.10(c)(7)-(8)............ Records of Excess No........................... Subpart RRRRR
Emissions and specifies record
Parameter Monitoring requirements.
Exceedances for CMS.
Sec. 63.10(d)(3)................ Reporting opacity or No........................... Subpart RRRRR does
VE observations. not have opacity and
VE standards.
Sec. 63.11...................... Control Device No........................... Subpart RRRRR does
Requirements. not require flares.
Sec. 63.12...................... State Authority and Yes.
Delegations.
Sec. 63.13-Sec. 63.15......... Addresses, Yes.
Incorporation by
Reference,
Availability of
Information.
----------------------------------------------------------------------------------------------------------------
Subpart SSSSS_National Emission Standards for Hazardous Air Pollutants
for Refractory Products Manufacturing
Source: 68 FR 18747, Apr. 16, 2003, unless otherwise noted.
What This Subpart Covers
Sec. 63.9780 What is the purpose of this subpart?
This subpart establishes national emission standards for hazardous
air pollutants (NESHAP) for refractory products manufacturing
facilities. This subpart also establishes requirements to demonstrate
initial and continuous compliance with the emission limitations.
Sec. 63.9782 Am I subject to this subpart?
You are subject to this subpart if you own or operate a refractory
products manufacturing facility that is, is located at, or is part of, a
major source of hazardous air pollutant (HAP) emissions according to the
criteria in paragraphs (a) and (b) of this section.
(a) A refractory products manufacturing facility is a plant site
that manufactures refractory products (refractory bricks, refractory
shapes, monolithics, kiln furniture, crucibles, and other materials used
for lining furnaces and other high temperature process units), as
defined in Sec. 63.9824. Refractory products manufacturing facilities
typically process raw material by crushing, grinding, and screening;
mixing the processed raw materials with binders and other additives;
forming
[[Page 87]]
the refractory mix into shapes; and drying and firing the shapes.
(b) A major source of HAP is a plant site that emits or has the
potential to emit any single HAP at a rate of 9.07 megagrams (10 tons)
or more per year or any combination of HAP at a rate of 22.68 megagrams
(25 tons) or more per year.
Sec. 63.9784 What parts of my plant does this subpart cover?
(a) This subpart applies to each new, reconstructed, or existing
affected source at a refractory products manufacturing facility.
(b) The existing affected sources are shape dryers, curing ovens,
and kilns that are used to manufacture refractory products that use
organic HAP; shape preheaters, pitch working tanks, defumers, and coking
ovens that are used to produce pitch-impregnated refractory products;
kilns that are used to manufacture chromium refractory products; and
kilns that are used to manufacture clay refractory products.
(c) The new or reconstructed affected sources are shape dryers,
curing ovens, and kilns that are used to manufacture refractory products
that use organic HAP; shape preheaters, pitch working tanks, defumers,
and coking ovens used to produce pitch-impregnated refractory products;
kilns that are used to manufacture chromium refractory products; and
kilns that are used to manufacture clay refractory products.
(d) Shape dryers, curing ovens, kilns, coking ovens, defumers, shape
preheaters, and pitch working tanks that are research and development
(R&D) process units are not subject to the requirements of this subpart.
(See definition of research and development process unit in Sec.
63.9824).
(e) A source is a new affected source if you began construction of
the affected source after June 20, 2002, and you met the applicability
criteria at the time you began construction.
(f) An affected source is reconstructed if you meet the criteria as
defined in Sec. 63.2.
(g) An affected source is existing if it is not new or
reconstructed.
Sec. 63.9786 When do I have to comply with this subpart?
(a) If you have a new or reconstructed affected source, you must
comply with this subpart according to paragraphs (a)(1) and (2) of this
section.
(1) If the initial startup of your affected source is before April
16, 2003, then you must comply with the emission limitations for new and
reconstructed sources in this subpart no later than April 16, 2003.
(2) If the initial startup of your affected source is after April
16, 2003, then you must comply with the emission limitations for new and
reconstructed sources in this subpart upon initial startup of your
affected source.
(b) If you have an existing affected source, you must comply with
the emission limitations for existing sources no later than April 17,
2006.
(c) You must be in compliance with this subpart when you conduct a
performance test on an affected source.
(d) If you have an existing area source that increases its emissions
or its potential to emit such that it becomes a major source of HAP, you
must be in compliance with this subpart according to paragraphs (d)(1)
and (2) of this section.
(1) Any portion of the existing facility that is a new affected
source or a new reconstructed source must be in compliance with this
subpart upon startup.
(2) All other parts of the existing facility must be in compliance
with this subpart by 3 years after the date the area source becomes a
major source.
(e) If you have a new area source (i.e., an area source for which
construction or reconstruction was commenced after June 20, 2002) that
increases its emissions or its potential to emit such that it becomes a
major source of HAP, you must be in compliance with this subpart upon
initial startup of your affected source as a major source.
(f) You must meet the notification requirements in Sec. 63.9812
according to the schedule in Sec. 63.9812 and in 40 CFR part 63,
subpart A. Some of the notifications must be submitted before you are
required to comply with the emission limitations in this subpart.
[[Page 88]]
Emission Limitations and Work Practice Standards
Sec. 63.9788 What emission limits, operating limits, and work practice
standards must I meet?
(a) You must meet each emission limit in Table 1 to this subpart
that applies to you.
(b) You must meet each operating limit in Table 2 to this subpart
that applies to you.
(c) You must meet each work practice standard in Table 3 to this
subpart that applies to you.
Sec. 63.9790 What are my options for meeting the emission limits?
To meet the emission limits in Table 1 to this subpart, you must use
one or both of the options listed in paragraphs (a) and (b) of this
section.
(a) Emissions control system. Use an emissions capture and
collection system and an add-on air pollution control device (APCD) and
demonstrate that the resulting emissions or emissions reductions meet
the applicable emission limits in Table 1 to this subpart, and
demonstrate that the capture and collection system and APCD meet the
applicable operating limits in Table 2 to this subpart.
(b) Process changes. Use raw materials that have little or no
potential to emit HAP during the refractory products manufacturing
process or implement manufacturing process changes and demonstrate that
the resulting emissions or emissions reductions meet the applicable
emission limits in Table 1 to this subpart without an add-on APCD.
General Compliance Requirements
Sec. 63.9792 What are my general requirements for complying with this
subpart?
(a) You must be in compliance with the emission limitations
(including operating limits and work practice standards) in this subpart
at all times, except during periods specified in paragraphs (a)(1) and
(2) of this section.
(1) Periods of startup, shutdown, and malfunction.
(2) Periods of scheduled maintenance on a control device that is
used on an affected continuous kiln, as specified in paragraph (e) of
this section.
(b) Except as specified in paragraph (e) of this section, you must
always operate and maintain your affected source, including air
pollution control and monitoring equipment, according to the provisions
in Sec. 63.6(e)(1)(i). During the period between the compliance date
specified for your affected source in Sec. 63.9786 and the date upon
which continuous monitoring systems have been installed and validated
and any applicable operating limits have been established, you must
maintain a log detailing the operation and maintenance of the process
and emissions control equipment.
(c) You must develop a written startup, shutdown, and malfunction
plan (SSMP) according to the provisions in Sec. 63.6(e)(3).
(d) You must prepare and implement a written operation, maintenance,
and monitoring (OM&M) plan according to the requirements in Sec.
63.9794.
(e) If you own or operate an affected continuous kiln and must
perform scheduled maintenance on the control device for that kiln, you
may bypass the kiln control device and continue operating the kiln upon
approval by the Administrator, provided you satisfy the conditions
listed in paragraphs (e)(1) through (3) of this section.
(1) You must request approval from the Administrator to bypass the
control device while the scheduled maintenance is performed. You must
submit a separate request each time you plan to bypass the control
device, and your request must include the information specified in
paragraphs (e)(1)(i) through (vi) of this section.
(i) Reason for the scheduled maintenance.
(ii) Explanation for why the maintenance cannot be performed when
the kiln is shut down.
(iii) Detailed description of the maintenance activities.
(iv) Time required to complete the maintenance.
(v) How you will minimize HAP emissions from the kiln during the
period when the control device is out of service.
(vi) How you will minimize the time when the kiln is operating and
the control device is out of service for scheduled maintenance.
[[Page 89]]
(2) You must minimize HAP emissions during the period when the kiln
is operating and the control device is out of service.
(3) You must minimize the time period during which the kiln is
operating and the control device is out of service.
(f) You must be in compliance with the provisions of subpart A of
this part, except as noted in Table 11 to this subpart.
[68 FR 18747, Apr. 16, 2003, as amended at 71 FR 20471, Apr. 20, 2006]
Sec. 63.9794 What do I need to know about operation, maintenance, and
monitoring plans?
(a) For each continuous parameter monitoring system (CPMS) required
by this subpart, you must develop, implement, make available for
inspection, and revise, as necessary, an OM&M plan that includes the
information in paragraphs (a)(1) through (13) of this section.
(1) A list and identification of each process and add-on APCD that
is required by this subpart to be monitored, the type of monitoring
device that will be used, and the operating parameters that will be
monitored.
(2) Specifications for the sensor, signal analyzer, and data
collection system.
(3) A monitoring schedule that specifies the frequency that the
parameter values will be determined and recorded.
(4) The operating limits for each parameter that represent
continuous compliance with the emission limitations in Sec. 63.9788,
based on values of the monitored parameters recorded during performance
tests.
(5) Procedures for installing the CPMS at a measurement location
relative to each process unit or APCD such that measurement is
representative of control of emissions.
(6) Procedures for the proper operation and routine and long-term
maintenance of each process unit and APCD, including a maintenance and
inspection schedule that is consistent with the manufacturer's
recommendations.
(7) Procedures for the proper operation and maintenance of
monitoring equipment consistent with the requirements in Sec. Sec.
63.8(c)(1), (3), (4)(ii), (7), and (8), and 63.9804.
(8) Ongoing data quality assurance procedures in accordance with the
general requirements of Sec. 63.8(d).
(9) Procedures for evaluating the performance of each CPMS.
(10) Procedures for responding to operating parameter deviations,
including the procedures in paragraphs (a)(10)(i) through (iii) of this
section:
(i) Procedures for determining the cause of the operating parameter
deviation.
(ii) Actions for correcting the deviation and returning the
operating parameters to the allowable limits.
(iii) Procedures for recording the times that the deviation began
and ended, and when corrective actions were initiated and completed.
(11) Procedures for keeping records to document compliance and
reporting in accordance with the requirements of Sec. 63.10(c), (e)(1),
and (e)(2)(i).
(12) If you operate a kiln that is subject to the limits on the type
of fuel used, as specified in items 3 and 4 of Table 3 to subpart SSSSS,
procedures for using alternative fuels.
(13) If you operate an affected continuous kiln and you plan to take
the kiln control device out of service for scheduled maintenance, as
specified in Sec. 63.9792(e), the procedures specified in paragraphs
(a)(13)(i) and (ii) of this section.
(i) Procedures for minimizing HAP emissions from the kiln during
periods of scheduled maintenance of the kiln control device when the
kiln is operating and the control device is out of service.
(ii) Procedures for minimizing any period of scheduled maintenance
on the kiln control device when the kiln is operating and the control
device is out of service.
(b) Changes to the operating limits in your OM&M plan require a new
performance test. If you are revising an operating limit parameter
value, you must meet the requirements in paragraphs (b)(1) and (2) of
this section.
(1) Submit a Notification of Performance Test to the Administrator
as specified in Sec. 63.7(b).
(2) After completing the performance tests to demonstrate that
compliance
[[Page 90]]
with the emission limits can be achieved at the revised operating limit
parameter value, you must submit the performance test results and the
revised operating limits as part of the Notification of Compliance
Status required under Sec. 63.9(h).
(c) If you are revising the inspection and maintenance procedures in
your OM&M plan, you do not need to conduct a new performance test.
Testing and Initial Compliance Requirements
Sec. 63.9796 By what date must I conduct performance tests?
You must conduct performance tests within 180 calendar days after
the compliance date that is specified for your source in Sec. 63.9786
and according to the provisions in Sec. 63.7(a)(2).
Sec. 63.9798 When must I conduct subsequent performance tests?
(a) You must conduct a performance test every 5 years following the
initial performance test, as part of renewing your 40 CFR part 70 or 40
CFR part 71 operating permit.
(b) You must conduct a performance test when you want to change the
parameter value for any operating limit specified in your OM&M plan.
(c) If you own or operate a source that is subject to the emission
limits specified in items 2 through 9 of Table 1 to this subpart, you
must conduct a performance test on the source(s) listed in paragraphs
(c)(1) and (2) of this section before you start production of any
refractory product for which the organic HAP processing rate is likely
to exceed by more than 10 percent the maximum organic HAP processing
rate established during the most recent performance test on that same
source.
(1) Each affected shape dryer or curing oven that is used to process
the refractory product with the higher organic HAP processing rate.
(2) Each affected kiln that follows an affected shape dryer or
curing oven and is used to process the refractory product with the
higher organic HAP processing rate.
(d) If you own or operate a kiln that is subject to the emission
limits specified in item 5 or 9 of Table 1 to this subpart, you must
conduct a performance test on the affected kiln following any process
changes that are likely to increase organic HAP emissions from the kiln
(e.g., a decrease in the curing cycle time for a curing oven that
precedes the affected kiln in the process line).
(e) If you own or operate a clay refractory products kiln that is
subject to the emission limits specified in item 10 or 11 of Table 1 to
this subpart and is controlled with a dry limestone adsorber (DLA), you
must conduct a performance test on the affected kiln following any
change in the source of limestone used in the DLA.
Sec. 63.9800 How do I conduct performance tests and establish operating
limits?
(a) You must conduct each performance test in Table 4 to this
subpart that applies to you.
(b) Before conducting the performance test, you must install and
validate all monitoring equipment.
(c) Each performance test must be conducted according to the
requirements in Sec. 63.7 and under the specific conditions in Table 4
to this subpart.
(d) You may not conduct performance tests during periods of startup,
shutdown, or malfunction, as specified in Sec. 63.7(e)(1).
(e) You must conduct separate test runs for at least the duration
specified for each performance test required in this section, as
specified in Sec. 63.7(e)(3) and Table 4 to this subpart.
(f) For batch process sources, you must satisfy the requirements
specified in paragraphs (f)(1) through (5) of this section.
(1) You must conduct at least two test runs.
(2) Each test run must last an entire batch cycle unless you develop
an emissions profile, as specified in items 8(a)(i)(4) and 17(b)(i)(4)
of Table 4 to this subpart, or you satisfy the conditions for
terminating a test run prior to the completion of a batch cycle as
specified in item 8(a)(i)(5) of Table 4 to this subpart.
(3) Each test run must be performed over a separate batch cycle
unless you satisfy the conditions for conducting both test runs over a
single batch
[[Page 91]]
cycle, as described in paragraphs (f)(3)(i) and (ii) of this section.
(i) You do not produce the product that corresponds to the maximum
organic HAP processing rate for that batch process source in consecutive
batch cycles.
(ii) To produce that product in two consecutive batch cycles would
disrupt production of other refractory products.
(4) If you want to conduct a performance test over a single batch
cycle, you must include in your Notification of Performance Test the
rationale for testing over a single batch cycle.
(5) If you are granted approval to conduct a performance test over a
single batch cycle, you must use paired sampling trains and collect two
sets of emissions data. Each set of data can be considered a separate
test run.
(g) You must use the data gathered during the performance test and
the equations in paragraphs (g)(1) through (3) of this section to
determine compliance with the emission limitations.
(1) To determine compliance with the total hydrocarbon (THC)
emission concentration limit listed in Table 1 to this subpart, you must
calculate your emission concentration corrected to 18 percent oxygen for
each test run using Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR16AP03.000
Where:
C THC-C=THC concentration, corrected to 18 percent oxygen,
parts per million by volume, dry basis (ppmvd)
C THC=THC concentration (uncorrected), ppmvd
CO2=oxygen concentration, percent.
(2) To determine compliance with any of the emission limits based on
percentage reduction across an emissions control system specified in
Table 1 to this subpart, you must calculate the percentage reduction for
each test run using Equation 2 of this section:
[GRAPHIC] [TIFF OMITTED] TR16AP03.001
Where:
PR=percentage reduction, percent
ERi=mass emissions rate of specific HAP or pollutant (THC,
HF, or HCl) entering the control device, kilograms (pounds) per hour
ERo=mass emissions rate of specific HAP or pollutant (THC,
HF, or HCl) exiting the control device, kilograms (pounds) per hour.
(3) To determine compliance with production-based hydrogen fluoride
(HF) and hydrogen chloride (HCl) emission limits in Table 1 to this
subpart, you must calculate your mass emissions per unit of uncalcined
clay processed for each test run using Equation 3 of this section:
[GRAPHIC] [TIFF OMITTED] TR16AP03.002
Where:
MP=mass per unit of production, kilograms of pollutant per megagram
(pounds per ton) of uncalcined clay processed
ER=mass emissions rate of specific HAP (HF or HCl) during each
performance test run, kilograms (pounds) per hour
P=average uncalcined clay processing rate for the performance test,
megagrams (tons) of uncalcined clay processed per hour.
(h) You must establish each site-specific operating limit in Table 2
to this subpart that applies to you, as specified in Table 4 to this
subpart.
(i) For each affected source that is equipped with an add-on APCD
that is not addressed in Table 2 to this subpart or that is using
process changes as a means of meeting the emission limits in Table 1 to
this subpart, you must meet the requirements in Sec. 63.8(f) and
paragraphs (i)(1) through (3) of this section.
(1) For sources subject to the THC concentration limit specified in
item 3 or 7 of Table 1 to this subpart, you must satisfy the
requirements specified in paragraphs (i)(1)(i) through (iii) of this
section.
(i) You must install a THC continuous emissions monitoring system
(CEMS) at the outlet of the control device or in the stack of the
affected source.
(ii) You must meet the requirements specified in Performance
Specification (PS) 8 of 40 CFR part 60, appendix B.
(iii) You must meet the requirements specified in Procedure 1 of 40
CFR part 60, appendix F.
[[Page 92]]
(2) For sources subject to the emission limits specified in item 3,
4, 7, or 8 of Table 1 to this subpart, you must submit a request for
approval of alternative monitoring methods to the Administrator no later
than the submittal date for the Notification of Performance Test, as
specified in Sec. 63.9812(d). The request must contain the information
specified in paragraphs (i)(2)(i) through (v) of this section.
(i) Description of the alternative add-on APCD or process changes.
(ii) Type of monitoring device or method that will be used,
including the sensor type, location, inspection procedures, quality
assurance and quality control measures, and data recording device.
(iii) Operating parameters that will be monitored.
(iv) Frequency that the operating parameter values will be
determined and recorded to establish continuous compliance with the
operating limits.
(v) Averaging time.
(3) You must establish site-specific operating limits during the
performance test based on the information included in the approved
alternative monitoring methods request and, as applicable, as specified
in Table 4 to this subpart.
Sec. 63.9802 How do I develop an emissions profile?
If you decide to develop an emissions profile for an affected batch
process source; as indicated in item 8(a)(i)(4) or 17(b)(i)(4) of Table
4 to this subpart, you must measure and record mass emissions of the
applicable pollutant throughout a complete batch cycle of the affected
batch process source according to the procedures described in paragraph
(a) or (b) of this section.
(a) If your affected batch process source is subject to the THC
concentration limit specified in item 6(a), 7(a), 8, or 9 of Table 1 to
this subpart or the THC percentage reduction limit specified in item
6(b) or 7(b) of Table 1 to this subpart, you must measure and record the
THC mass emissions rate at the inlet to the control device using the
test methods, averaging periods, and procedures specified in items 10(a)
and (b) of Table 4 to this subpart for each complete hour of the batch
process cycle.
(b) If your affected batch process source is subject to the HF and
HCl percentage reduction emission limits in item 11 of Table 1 to this
subpart, you must measure and record the HF mass emissions rate at the
inlet to the control device through a series of 1-hour test runs
according to the test method specified in item 14(a) of Table 4 to this
subpart for each complete hour of the batch process cycle.
Sec. 63.9804 What are my monitoring system installation, operation, and
maintenance requirements?
(a) You must install, operate, and maintain each CPMS required by
this subpart according to your OM&M plan and the requirements in
paragraphs (a)(1) through (15) of this section.
(1) You must satisfy all applicable requirements of performance
specifications for CPMS specified in 40 CFR part 60, appendix B, upon
promulgation of such performance specifications.
(2) You must satisfy all applicable requirements of quality
assurance (QA) procedures for CPMS specified in 40 CFR part 60, appendix
F, upon promulgation of such QA procedures.
(3) You must install each sensor of your CPMS in a location that
provides representative measurement of the appropriate parameter over
all operating conditions, taking into account the manufacturer's
guidelines.
(4) You must use a CPMS that is capable of measuring the appropriate
parameter over a range that extends from a value of at least 20 percent
less than the lowest value that you expect your CPMS to measure, to a
value of at least 20 percent greater than the highest value that you
expect your CPMS to measure.
(5) You must use a data acquisition and recording system that is
capable of recording values over the entire range specified in paragraph
(a)(4) of this section.
(6) You must use a signal conditioner, wiring, power supply, and
data acquisition and recording system that are compatible with the
output signal of the sensors used in your CPMS.
[[Page 93]]
(7) You must perform an initial calibration of your CPMS based on
the procedures specified in the manufacturer's owner's manual.
(8) You must use a CPMS that is designed to complete a minimum of
one cycle of operation for each successive 15-minute period. To have a
valid hour of data, you must have at least three of four equally-spaced
data values (or at least 75 percent of the total number of values if you
collect more than four data values per hour) for that hour (not
including startup, shutdown, malfunction, or out-of-control periods).
(9) You must record valid data from at least 90 percent of the hours
during which the affected source or process operates.
(10) You must determine and record the 15-minute block averages of
all measurements, calculated after every 15 minutes of operation as the
average of the previous 15 operating minutes (not including periods of
startup, shutdown, or malfunction).
(11) You must determine and record the 3-hour block averages of all
15-minute recorded measurements, calculated after every 3 hours of
operation as the average of the previous 3 operating hours (not
including periods of startup, shutdown, or malfunction).
(12) You must record the results of each inspection, calibration,
initial validation, and accuracy audit.
(13) At all times, you must maintain your CPMS including, but not
limited to, maintaining necessary parts for routine repairs of the CPMS.
(14) You must perform an initial validation of your CPMS under the
conditions specified in paragraphs (14)(i) and (ii) of this section.
(i) Prior to the initial performance test on the affected source for
which the CPMS is required.
(ii) Within 180 days of your replacing or relocating one or more of
the sensors of your CPMS.
(15) Except for redundant sensors, as defined in Sec. 63.9824, any
device that you use to conduct an initial validation or accuracy audit
of your CPMS must meet the accuracy requirements specified in paragraphs
(15)(i) and (ii) of this section.
(i) The device must have an accuracy that is traceable to National
Institute of Standards and Technology (NIST) standards.
(ii) The device must be at least three times as accurate as the
required accuracy for the CPMS.
(b) For each temperature CPMS that is used to monitor the combustion
chamber temperature of a thermal oxidizer or the catalyst bed inlet
temperature of a catalytic oxidizer, you must meet the requirements in
paragraphs (a) and (b)(1) through (6) of this section.
(1) Use a temperature CPMS with a minimum accuracy of 1.0 percent of the temperature value or 2.8 degrees
Celsius ([deg]C) (5 degrees Fahrenheit ([deg]F)), whichever is greater.
(2) Use a data recording system with a minimum resolution of one-
half or better of the required CPMS accuracy specified in paragraph
(b)(1) of this section.
(3) Perform an initial validation of your CPMS according to the
requirements in paragraph (3)(i) or (ii) of this section.
(i) Place the sensor of a calibrated temperature measurement device
adjacent to the sensor of your temperature CPMS in a location that is
subject to the same environment as the sensor of your temperature CPMS.
The calibrated temperature measurement device must satisfy the accuracy
requirements of paragraph (a)(15) of this section. While the process and
control device that is monitored by your CPMS are operating normally,
record concurrently and compare the temperatures measured by your
temperature CPMS and the calibrated temperature measurement device.
Using the calibrated temperature measurement device as the reference,
the temperature measured by your CPMS must be within the accuracy
specified in paragraph (b)(1) of this section.
(ii) Perform any of the initial validation methods for temperature
CPMS specified in performance specifications for CPMS established in 40
CFR part 60, appendix B.
(4) Perform an accuracy audit of your temperature CPMS at least
quarterly, according to the requirements in paragraph (b)(4)(i), (ii),
or (iii) of this section.
[[Page 94]]
(i) If your temperature CPMS includes a redundant temperature
sensor, record three pairs of concurrent temperature measurements within
a 24-hour period. Each pair of concurrent measurements must consist of a
temperature measurement by each of the two temperature sensors. The
minimum time interval between any two such pairs of consecutive
temperature measurements is 1 hour. The measurements must be taken
during periods when the process and control device that is monitored by
your temperature CPMS are operating normally. Calculate the mean of the
three values for each temperature sensor. The mean values must agree
within the required overall accuracy of the CPMS, as specified in
paragraph (b)(1) of this section.
(ii) If your temperature CPMS does not include a redundant
temperature sensor, place the sensor of a calibrated temperature
measurement device adjacent to the sensor of your temperature CPMS in a
location that is subject to the same environment as the sensor of your
temperature CPMS. The calibrated temperature measurement device must
satisfy the accuracy requirements of paragraph (a)(15) of this section.
While the process and control device that is monitored by your
temperature CPMS are operating normally, record concurrently and compare
the temperatures measured by your CPMS and the calibrated temperature
measurement device. Using the calibrated temperature measurement device
as the reference, the temperature measured by your CPMS must be within
the accuracy specified in paragraph (b)(1) of this section.
(iii) Perform any of the accuracy audit methods for temperature CPMS
specified in QA procedures for CPMS established in 40 CFR part 60,
appendix F.
(5) Conduct an accuracy audit of your CPMS following any 24-hour
period throughout which the temperature measured by your CPMS exceeds
the manufacturer's specified maximum operating temperature range, or
install a new temperature sensor.
(6) If your CPMS is not equipped with a redundant temperature
sensor, perform at least quarterly a visual inspection of all components
of the CPMS for integrity, oxidation, and galvanic corrosion.
(c) For each pressure CPMS that is used to monitor the pressure drop
across a DLA or wet scrubber, you must meet the requirements in
paragraphs (a) and (c)(1) through (7) of this section.
(1) Use a pressure CPMS with a minimum accuracy of 5.0 percent or 0.12 kilopascals (kPa) (0.5 inches of
water column (in. w.c.)), whichever is greater.
(2) Use a data recording system with a minimum resolution of one-
half the required CPMS accuracy specified in paragraph (c)(1) of this
section, or better.
(3) Perform an initial validation of your pressure CPMS according to
the requirements in paragraph (c)(3)(i) or (ii) of this section.
(i) Place the sensor of a calibrated pressure measurement device
adjacent to the sensor of your pressure CPMS in a location that is
subject to the same environment as the sensor of your pressure CPMS. The
calibrated pressure measurement device must satisfy the accuracy
requirements of paragraph (a)(15) of this section. While the process and
control device that is monitored by your CPMS are operating normally,
record concurrently and compare the pressure measured by your CPMS and
the calibrated pressure measurement device. Using the calibrated
pressure measurement device as the reference, the pressure measured by
your CPMS must be within the accuracy specified in paragraph (c)(1) of
this section.
(ii) Perform any of the initial validation methods for pressure CPMS
specified in performance specifications for CPMS established in 40 CFR
part 60, appendix B.
(4) Perform an accuracy audit of your pressure CPMS at least
quarterly, according to the requirements in paragraph (c)(4)(i), (ii),
or (iii) of this section.
(i) If your pressure CPMS includes a redundant pressure sensor,
record three pairs of concurrent pressure measurements within a 24-hour
period. Each pair of concurrent measurements must consist of a pressure
measurement by each of the two pressure sensors. The minimum time
interval between any two such pairs of consecutive pressure
[[Page 95]]
measurements is 1 hour. The measurements must be taken during periods
when the process and control device that is monitored by your CPMS are
operating normally. Calculate the mean of the three pressure measurement
values for each pressure sensor. The mean values must agree within the
required overall accuracy of the CPMS, as specified in paragraph (c)(1)
of this section.
(ii) If your pressure CPMS does not include a redundant pressure
sensor, place the sensor of a calibrated pressure measurement device
adjacent to the sensor of your pressure CPMS in a location that is
subject to the same environment as the sensor of your pressure CPMS. The
calibrated pressure measurement device must satisfy the accuracy
requirements of paragraph (a)(15) of this section. While the process and
control device that is monitored by your pressure CPMS are operating
normally, record concurrently and compare the pressure measured by your
CPMS and the calibrated pressure measurement device. Using the
calibrated pressure measurement device as the reference, the pressure
measured by your CPMS must be within the accuracy specified in paragraph
(c)(1) of this section.
(iii) Perform any of the accuracy audit methods for pressure CPMS
specified in QA procedures for CPMS established in 40 CFR part 60,
appendix F.
(5) Conduct an accuracy audit of your CPMS following any 24-hour
period throughout which the pressure measured by your CPMS exceeds the
manufacturer's specified maximum operating pressure range, or install a
new pressure sensor.
(6) At least monthly, check all mechanical connections on your CPMS
for leakage.
(7) If your CPMS is not equipped with a redundant pressure sensor,
perform at least quarterly a visual inspection of all components of the
CPMS for integrity, oxidation, and galvanic corrosion.
(d) For each liquid flow rate CPMS that is used to monitor the
liquid flow rate in a wet scrubber, you must meet the requirements in
paragraphs (a) and (d)(1) through (7) of this section.
(1) Use a flow rate CPMS with a minimum accuracy of 5.0 percent or 1.9 liters per minute (L/min) (0.5
gallons per minute (gal/min)), whichever is greater.
(2) Use a data recording system with a minimum resolution of one-
half the required CPMS accuracy specified in paragraph (d)(1) of this
section, or better.
(3) Perform an initial validation of your CPMS according to the
requirements in paragraph (3)(i) or (ii) of this section.
(i) Use a calibrated flow rate measurement system to measure the
liquid flow rate in a location that is adjacent to the measurement
location for your flow rate CPMS and is subject to the same environment
as your flow rate CPMS. The calibrated flow rate measurement device must
satisfy the accuracy requirements of paragraph (a)(15) of this section.
While the process and control device that is monitored by your flow rate
CPMS are operating normally, record concurrently and compare the flow
rates measured by your flow rate CPMS and the calibrated flow rate
measurement device. Using the calibrated flow rate measurement device as
the reference, the flow rate measured by your CPMS must be within the
accuracy specified in paragraph (d)(1) of this section.
(ii) Perform any of the initial validation methods for liquid flow
rate CPMS specified in performance specifications for CPMS established
in 40 CFR part 60, appendix B.
(4) Perform an accuracy audit of your flow rate CPMS at least
quarterly, according to the requirements in paragraph (d)(4)(i), (ii),
or (iii) of this section.
(i) If your flow rate CPMS includes a redundant sensor, record three
pairs of concurrent flow rate measurements within a 24-hour period. Each
pair of concurrent measurements must consist of a flow rate measurement
by each of the two flow rate sensors. The minimum time interval between
any two such pairs of consecutive flow rate measurements is 1 hour. The
measurements must be taken during periods when the process and control
device that is monitored by your flow rate CPMS are operating normally.
Calculate the mean of the three flow rate measurement values for each
flow rate
[[Page 96]]
sensor. The mean values must agree within the required overall accuracy
of the CPMS, as specified in paragraph (d)(1) of this section.
(ii) If your flow rate CPMS does not include a redundant flow rate
sensor, place the sensor of a calibrated flow rate measurement device
adjacent to the sensor of your flow rate CPMS in a location that is
subject to the same environment as the sensor of your flow rate CPMS.
The calibrated flow rate measurement device must satisfy the accuracy
requirements of paragraph (a)(15) of this section. While the process and
control device that is monitored by your flow rate CPMS are operating
normally, record concurrently and compare the flow rate measured by your
pressure CPMS and the calibrated flow rate measurement device. Using the
calibrated flow rate measurement device as the reference, the flow rate
measured by your CPMS must be within the accuracy specified in paragraph
(d)(1) of this section.
(iii) Perform any of the accuracy audit methods for liquid flow rate
CPMS specified in QA procedures for CPMS established in 40 CFR part 60,
appendix F.
(5) Conduct an accuracy audit of your flow rate CPMS following any
24-hour period throughout which the flow rate measured by your CPMS
exceeds the manufacturer's specified maximum operating range, or install
a new flow rate sensor.
(6) At least monthly, check all mechanical connections on your CPMS
for leakage.
(7) If your CPMS is not equipped with a redundant flow rate sensor,
perform at least quarterly a visual inspection of all components of the
CPMS for integrity, oxidation, and galvanic corrosion.
(e) For each pH CPMS that is used to monitor the pH of a wet
scrubber liquid, you must meet the requirements in paragraphs (a) and
(e)(1) through (5) of this section.
(1) Use a pH CPMS with a minium accuracy of 0.2 pH units.
(2) Use a data recording system with a minimum resolution of 0.1 pH
units, or better.
(3) Perform an initial validation of your pH CPMS according to the
requirements in paragraph (e)(3)(i) or (ii) of this section.
(i) Perform a single-point calibration using an NIST-certified
buffer solution that is accurate to within 0.02 pH
units at 25 [deg]C (77 [deg]F). If the expected pH of the liquid that is
monitored lies in the acidic range (less than 7 pH), use a buffer
solution with a pH value of 4.00. If the expected pH of the liquid that
is monitored is neutral or lies in the basic range (equal to or greater
than 7 pH), use a buffer solution with a pH value of 10.00. Place the
electrode of your pH CPMS in the container of buffer solution. Record
the pH measured by your CPMS. Using the certified buffer solution as the
reference, the pH measured by your CPMS must be within the accuracy
specified in paragraph (e)(1) of this section.
(ii) Perform any of the initial validation methods for pH CPMS
specified in performance specifications for CPMS established in 40 CFR
part 60, appendix B.
(4) Perform an accuracy audit of your pH CPMS at least weekly,
according to the requirements in paragraph (e)(4)(i), (ii), or (iii) of
this section.
(i) If your pH CPMS includes a redundant pH sensor, record the pH
measured by each of the two pH sensors. The measurements must be taken
during periods when the process and control device that is monitored by
your pH CPMS are operating normally. The two pH values must agree within
the required overall accuracy of the CPMS, as specified in paragraph
(e)(1) of this section.
(ii) If your pH CPMS does not include a redundant pH sensor, perform
a single point calibration using an NIST-certified buffer solution that
is accurate to within 0.02 pH units at 25 [deg]C
(77 [deg]F). If the expected pH of the liquid that is monitored lies in
the acidic range (less than 7 pH), use a buffer solution with a pH value
of 4.00. If the expected pH of the liquid that is monitored is neutral
or lies in the basic range (equal to or greater than 7 pH), use a buffer
solution with a pH value of 10.00. Place the electrode of the pH CPMS in
the container of buffer solution. Record the pH measured by your CPMS.
Using the certified buffer solution as the reference, the pH measured
[[Page 97]]
by your CPMS must be within the accuracy specified in paragraph (e)(1)
of this section.
(iii) Perform any of the accuracy audit methods for pH CPMS
specified in QA procedures for CPMS established in 40 CFR part 60,
appendix F.
(5) If your CPMS is not equipped with a redundant pH sensor, perform
at least monthly a visual inspection of all components of the CPMS for
integrity, oxidation, and galvanic corrosion.
(f) For each bag leak detection system, you must meet the
requirements in paragraphs (f)(1) through (11) of this section.
(1) Each triboelectric bag leak detection system must be installed,
calibrated, operated, and maintained according to the ``Fabric Filter
Bag Leak Detection Guidance'' (EPA-454/R-98-015, September 1997). That
document is available from the U.S. EPA; Office of Air Quality Planning
and Standards; Emissions, Monitoring and Analysis Division; Emission
Measurement Center (D205-02), Research Triangle Park, NC 27711. It is
also available on the Technology Transfer Network (TTN) at the following
address: http://www.epa.gov/ttn/emc/cem.html. Other types of bag leak
detection systems must be installed, operated, calibrated, and
maintained in a manner consistent with the manufacturer's written
specifications and recommendations.
(2) The bag leak detection system must be certified by the
manufacturer to be capable of detecting particulate matter (PM)
emissions at concentrations of 10 milligrams per actual cubic meter
(0.0044 grains per actual cubic foot) or less.
(3) The bag leak detection system sensor must provide an output of
relative PM loadings.
(4) The bag leak detection system must be equipped with a device to
continuously record the output signal from the sensor.
(5) The bag leak detection system must be equipped with an alarm
system that will be engaged automatically when an increase in relative
PM emissions over a preset level is detected. The alarm must be located
where it is easily recognized by plant operating personnel.
(6) For positive pressure fabric filter systems, a bag leak detector
must be installed in each baghouse compartment or cell.
(7) For negative pressure or induced air fabric filters, the bag
leak detector must be installed downstream of the fabric filter.
(8) Where multiple detectors are required, the system's
instrumentation and alarm may be shared among detectors.
(9) The baseline output must be established by adjusting the range
and the averaging period of the device and establishing the alarm set
points and the alarm delay time according to section 5.0 of the ``Fabric
Filter Bag Leak Detection Guidance.''
(10) Following initial adjustment of the system, the owner or
operator must not adjust the sensitivity or range, averaging period,
alarm set points, or alarm delay time except as detailed in the OM&M
plan. In no case may the sensitivity be increased by more than 100
percent or decreased by more than 50 percent over a 365-day period
unless such adjustment follows a complete fabric filter inspection that
demonstrates that the fabric filter is in good operating condition. You
must record each adjustment of your bag leak detection system.
(11) Record the results of each inspection, calibration, and
validation check.
(g) For each lime feed rate measurement device that is used to
monitor the lime feed rate of a dry injection fabric filter (DIFF) or
dry lime scrubber/fabric filter (DLS/FF), or the chemical feed rate of a
wet scrubber, you must meet the requirements in paragraph (a) of this
section.
(h) For each affected source that is subject to the emission limit
specified in item 3, 4, 7, or 8 of Table 1 to this subpart, you must
satisfy the requirements of paragraphs (h)(1) through (3) of this
section.
(1) Install a THC CEMS at the outlet of the control device or in the
stack of the affected source.
(2) Meet the requirements of PS-8 of 40 CFR part 60, appendix B.
(3) Meet the requirements of Procedure 1 of 40 CFR part 60, appendix
F.
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(i) Requests for approval of alternate monitoring methods must meet
the requirements in Sec. Sec. 63.9800(i)(2) and 63.8(f).
Sec. 63.9806 How do I demonstrate initial compliance with the emission
limits, operating limits, and work practice standards?
(a) You must demonstrate initial compliance with each emission limit
that applies to you according to the requirements specified in Table 5
to this subpart.
(b) You must establish each site-specific operating limit in Table 2
to this subpart that applies to you according to the requirements
specified in Sec. 63.9800 and Table 4 to this subpart.
(c) You must demonstrate initial compliance with each work practice
standard that applies to you according to the requirements specified in
Table 6 to this subpart.
(d) You must submit the Notification of Compliance Status containing
the results of the initial compliance demonstration according to the
requirements in Sec. 63.9812(e).
Continuous Compliance Requirements
Sec. 63.9808 How do I monitor and collect data to demonstrate continuous
compliance?
(a) You must monitor and collect data according to this section.
(b) At all times, you must maintain your monitoring systems
including, but not limited to, maintaining necessary parts for routine
repairs of the monitoring equipment.
(c) Except for, as applicable, monitoring system malfunctions,
associated repairs, and required quality assurance or quality control
activities, you must monitor continuously whenever your affected process
unit is operating. For purposes of calculating data averages, you must
not use data recorded during monitoring system malfunctions, associated
repairs, and required quality assurance or quality control activities.
You must use all the data collected during all other periods in
assessing compliance. A monitoring system malfunction is any sudden,
infrequent, not reasonably preventable failure of the monitoring system
to provide valid data. Monitoring system malfunctions include out of
control continuous monitoring systems (CMS), such as a CPMS. Any
averaging period for which you do not have valid monitoring data as a
result of a monitoring system malfunction and for which such data are
required constitutes a deviation, and you must notify the Administrator
in accordance with Sec. 63.9814(e). Monitoring system failures are
different from monitoring system malfunctions in that they are caused in
part by poor maintenance or careless operation. Any period for which
there is a monitoring system failure and data are not available for
required calculations constitutes a deviation and you must notify the
Administrator in accordance with Sec. 63.9814(e).
Sec. 63.9810 How do I demonstrate continuous compliance with the
emission limits, operating limits, and work practice standards?
(a) You must demonstrate continuous compliance with each emission
limit specified in Table 1 to this subpart that applies to you according
to the requirements specified in Table 7 to this subpart.
(b) You must demonstrate continuous compliance with each operating
limit specified in Table 2 to this subpart that applies to you according
to the requirements specified in Table 8 to this subpart.
(c) You must demonstrate continuous compliance with each work
practice standard specified in Table 3 to this subpart that applies to
you according to the requirements specified in Table 9 to this subpart.
(d) For each affected source that is equipped with an add-on APCD
that is not addressed in Table 2 to this subpart or that is using
process changes as a means of meeting the emission limits in Table 1 to
this subpart, you must demonstrate continuous compliance with each
emission limit in Table 1 to this subpart and each operating limit
established as required in Sec. 63.9800(i)(3) according to the methods
specified in your approved alternative monitoring methods request as
described in Sec. 63.9800(i)(2).
(e) You must report each instance in which you did not meet each
emission limit and each operating limit in this
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subpart that applies to you. This includes periods of startup, shutdown,
and malfunction. These instances are deviations from the emission
limitations in this subpart. These deviations must be reported according
to the requirements in Sec. 63.9814.
(1) [Reserved]
(2) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations
that occur during a period of startup, shutdown, or malfunction are not
violations if you demonstrate to the Administrator's satisfaction that
you were operating in accordance with Sec. 63.6(e)(1) and your OM&M
plan. The Administrator will determine whether deviations that occur
during a period of startup, shutdown, or malfunction are violations,
according to the provisions in Sec. 63.6(e).
[68 FR 18747, Apr. 16, 2003, as amended at 71 FR 20471, Apr. 20, 2006]
Notifications, Reports, and Records
Sec. 63.9812 What notifications must I submit and when?
(a) You must submit all of the notifications in Sec. Sec. 63.7(b)
and (c), 63.8(f)(4), and 63.9 (b) through (e) and (h) that apply to you
by the dates specified.
(b) As specified in Sec. 63.9(b)(2) and (3), if you start up your
affected source before April 16, 2003, you must submit an Initial
Notification not later than 120 calendar days after April 16, 2003.
(c) As specified in Sec. 63.9(b)(3), if you start up your new or
reconstructed affected source on or after April 16, 2003, you must
submit an Initial Notification not later than 120 calendar days after
you become subject to this subpart.
(d) If you are required to conduct a performance test, you must
submit a Notification of Performance Test at least 60 calendar days
before the performance test is scheduled to begin, as required in Sec.
63.7(b)(1).
(e) If you are required to conduct a performance test, you must
submit a Notification of Compliance Status as specified in Sec. 63.9(h)
and paragraphs (e)(1) and (2) of this section.
(1) For each compliance demonstration that includes a performance
test conducted according to the requirements in Table 4 to this subpart,
you must submit the Notification of Compliance Status, including the
performance test results, before the close of business on the 60th
calendar day following the completion of the performance test, according
to Sec. 63.10(d)(2).
(2) In addition to the requirements in Sec. 63.9(h)(2)(i), you must
include the information in paragraphs (e)(2)(i) through (iv) of this
section in your Notification of Compliance Status.
(i) The operating limit parameter values established for each
affected source with supporting documentation and a description of the
procedure used to establish the values.
(ii) Design information and analysis with supporting documentation
demonstrating conformance with requirements for capture/collection
systems in Table 2 to this subpart.
(iii) A description of the methods used to comply with any
applicable work practice standard.
(iv) For each APCD that includes a fabric filter, analysis and
supporting documentation demonstrating conformance with EPA guidance and
specifications for bag leak detection systems in Sec. 63.9804(f).
(f) If you operate a clay refractory products kiln or a chromium
refractory products kiln that is subject to the work practice standard
specified in item 3 or 4 of Table 3 to this subpart, and you intend to
use a fuel other than natural gas or equivalent to fire the affected
kiln, you must submit a notification of alternative fuel use within 48
hours of the declaration of a period of natural gas curtailment or
supply interruption, as defined in Sec. 63.9824. The notification must
include the information specified in paragraphs (f)(1) through (5) of
this section.
(1) Company name and address.
(2) Identification of the affected kiln.
(3) Reason you are unable to use natural gas or equivalent fuel,
including the date when the natural gas curtailment was declared or the
natural gas supply interruption began.
(4) Type of alternative fuel that you intend to use.
(5) Dates when the alternative fuel use is expected to begin and
end.
(g) If you own or operate an affected continuous kiln and must
perform scheduled maintenance on the control device for that kiln, you
must request
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approval from the Administrator before bypassing the control device, as
specified in Sec. 63.9792(e). You must submit a separate request for
approval each time you plan to bypass the kiln control device.
Sec. 63.9814 What reports must I submit and when?
(a) You must submit each report in Table 10 to this subpart that
applies to you.
(b) Unless the Administrator has approved a different schedule for
submission of reports under Sec. 63.10(a), you must submit each report
by the date in Table 10 to this subpart and as specified in paragraphs
(b)(1) through (5) of this section.
(1) The first compliance report must cover the period beginning on
the compliance date that is specified for your affected source in Sec.
63.9786 and ending on June 30 or December 31 and lasting at least 6
months but less than 12 months. For example, if your compliance date is
March 1, then the first semiannual reporting period would begin on March
1 and end on December 31.
(2) The first compliance report must be postmarked or delivered no
later than July 31 or January 31 for compliance periods ending on June
30 and December 31, respectively.
(3) Each subsequent compliance report must cover the semiannual
reporting period from January 1 through June 30 or the semiannual
reporting period from July 1 through December 31.
(4) Each subsequent compliance report must be postmarked or
delivered no later than July 31 or January 31 for compliance periods
ending on June 30 and December 31, respectively.
(5) For each affected source that is subject to permitting
regulations pursuant to 40 CFR part 70 or 40 CFR part 71 and, if the
permitting authority has established dates for submitting semiannual
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance
reports according to the dates the permitting authority has established
instead of according to the dates in paragraphs (b)(1) through (4) of
this section. In such cases, you must notify the Administrator of this
change.
(c) The compliance report must contain the information in paragraphs
(c)(1) through (6) of this section.
(1) Company name and address.
(2) Statement by a responsible official with that official's name,
title, and signature, certifying that, based on information and belief
formed after reasonable inquiry, the statements and information in the
report are true, accurate, and complete.
(3) Date of report and beginning and ending dates of the reporting
period.
(4) If you had a startup, shutdown, or malfunction during the
reporting period, and you took actions consistent with your SSMP and
OM&M plan, the compliance report must include the information specified
in Sec. 63.10(d)(5)(i).
(5) If there are no deviations from any emission limitations
(emission limit, operating limit, or work practice standard) that apply
to you, the compliance report must include a statement that there were
no deviations from the emission limitations during the reporting period.
(6) If there were no periods during which any affected CPMS was out
of control as specified in Sec. 63.8(c)(7), the compliance report must
include a statement that there were no periods during which the CPMS was
out of control during the reporting period.
(d) For each deviation from an emission limitation (emission limit,
operating limit, or work practice standard) that occurs at an affected
source where you are not using a CPMS to comply with the emission
limitations in this subpart, the compliance report must contain the
information in paragraphs (c)(1) through (4) and (d)(1) and (2) of this
section. This includes periods of startup, shutdown, and malfunction.
(1) The compliance report must include the total operating time of
each affected source during the reporting period.
(2) The compliance report must include information on the number,
duration, and cause of deviations (including unknown cause, if
applicable) and the corrective action taken.
(e) For each deviation from an emission limitation (emission limit,
operating limit, or work practice standard)
[[Page 101]]
occurring at an affected source where you are using a CPMS to comply
with the emission limitation in this subpart, the compliance report must
include the information in paragraphs (c)(1) through (4) and (e)(1)
through (13) of this section. This includes periods of startup,
shutdown, and malfunction.
(1) The total operating time of each affected source during the
reporting period.
(2) The date and time that each startup, shutdown, or malfunction
started and stopped.
(3) The date, time, and duration that each CPMS was inoperative.
(4) The date, time and duration that each CPMS was out of control,
including the information in Sec. 63.8(c)(8), as required by your OM&M
plan.
(5) The date and time that each deviation from an emission
limitation (emission limit, operating limit, or work practice standard)
started and stopped, and whether each deviation occurred during a period
of startup, shutdown, or malfunction.
(6) A description of corrective action taken in response to a
deviation.
(7) A summary of the total duration of the deviations during the
reporting period and the total duration as a percentage of the total
source operating time during that reporting period.
(8) A breakdown of the total duration of the deviations during the
reporting period into those that are due to startup, shutdown, control
equipment problems, process problems, other known causes, and other
unknown causes.
(9) A summary of the total duration of CPMS downtime during the
reporting period and the total duration of CPMS downtime as a percentage
of the total source operating time during that reporting period.
(10) A brief description of the process units.
(11) A brief description of the CPMS.
(12) The date of the latest CPMS initial validation or accuracy
audit.
(13) A description of any changes in CPMS, processes, or controls
since the last reporting period.
(f) If you have obtained a title V operating permit pursuant to 40
CFR part 70 or 40 CFR part 71, you must report all deviations as defined
in this subpart in the semiannual monitoring report required by 40 CFR
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A). If you submit a
compliance report according to Table 10 to this subpart along with, or
as part of, the semiannual monitoring report required by 40 CFR
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A), and the compliance
report includes all required information concerning deviations from any
emission limitation (including any operating limit), then submitting the
compliance report will satisfy any obligation to report the same
deviations in the semiannual monitoring report. However, submitting a
compliance report will not otherwise affect any obligation you may have
to report deviations from permit requirements to the permit authority.
(g) If you operate a clay refractory products kiln or a chromium
refractory products kiln that is subject to the work practice standard
specified in item 3 or 4 of Table 3 to this subpart, and you use a fuel
other than natural gas or equivalent to fire the affected kiln, you must
submit a report of alternative fuel use within 10 working days after
terminating the use of the alternative fuel. The report must include the
information in paragraphs (g)(1) through (6) of this section.
(1) Company name and address.
(2) Identification of the affected kiln.
(3) Reason for using the alternative fuel.
(4) Type of alternative fuel used to fire the affected kiln.
(5) Dates that the use of the alternative fuel started and ended.
(6) Amount of alternative fuel used.
Sec. 63.9816 What records must I keep?
(a) You must keep the records listed in paragraphs (a)(1) through
(3) of this section.
(1) A copy of each notification and report that you submitted to
comply with this subpart, including all documentation supporting any
Initial Notification or Notification of Compliance Status that you
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
(2) The records in Sec. 63.6(e)(3)(iii) through (v) related to
startup, shutdown, and malfunction.
(3) Records of performance tests as required in Sec.
63.10(b)(2)(viii).
[[Page 102]]
(b) You must keep the records required in Tables 7 through 9 to this
subpart to show continuous compliance with each emission limitation that
applies to you.
(c) You must also maintain the records listed in paragraphs (c)(1)
through (10) of this section.
(1) Records of emission data used to develop an emissions profile,
as indicated in items 8(a)(i)(4) and 17(b)(i)(4) of Table 4 to this
subpart.
(2) Records that document how you comply with any applicable work
practice standard.
(3) For each bag leak detection system, records of each alarm, the
time of the alarm, the time corrective action was initiated and
completed, and a brief description of the cause of the alarm and the
corrective action taken.
(4) For each kiln controlled with a DLA, records that document the
source of limestone used.
(5) For each deviation of an operating limit parameter value, the
date, time, and duration of the deviation, a brief explanation of the
cause of the deviation and the corrective action taken, and whether the
deviation occurred during a period of startup, shutdown, or malfunction.
(6) For each affected source, records of production rate on a
process throughput basis (either feed rate to the process unit or
discharge rate from the process unit).
(7) Records of any approved alternative monitoring method(s) or test
procedure(s).
(8) Records of maintenance activities and inspections performed on
control devices, including all records associated with the scheduled
maintenance of continuous kiln control devices, as specified in Sec.
63.9792(e).
(9) If you operate a source that is subject to the THC emission
limits specified in item 2, 3, 6, or 7 of Table 1 to this subpart and is
controlled with a catalytic oxidizer, records of annual checks of
catalyst activity levels and subsequent corrective actions.
(10) Current copies of the SSMP and the OM&M plan, including any
revisions and records documenting conformance with those revisions.
Sec. 63.9818 In what form and how long must I keep my records?
(a) Your records must be in a form suitable and readily available
for expeditious review, according to Sec. 63.10(b)(1).
(b) As specified in Sec. 63.10(b)(1), you must keep each record for
5 years following the date of each occurrence, measurement, maintenance,
corrective action, report, or record.
(c) You must keep each record onsite for at least 2 years after the
date of each occurrence, measurement, maintenance, corrective action,
report, or record, according to Sec. 63.10(b)(1). You may keep the
records offsite for the remaining 3 years.
Other Requirements and Information
Sec. 63.9820 What parts of the General Provisions apply to me?
Table 11 to this subpart shows which parts of the General Provisions
specified in Sec. Sec. 63.1 through 63.15 apply to you.
Sec. 63.9822 Who implements and enforces this subpart?
(a) This subpart can be implemented and enforced by us, the U.S.
Environmental Protection Agency (U.S. EPA), or a delegated authority
such as your State, local, or tribal agency. If the U.S. EPA
Administrator has delegated authority to your State, local, or tribal
agency, then that agency, in addition to the U.S. EPA, has the authority
to implement and enforce this subpart. You should contact your U.S. EPA
Regional Office to find out if implementation and enforcement to this
subpart is delegated to your State, local, or tribal agency.
(b) In delegating implementation and enforcement authority to this
subpart to a State, local, or tribal agency under 40 CFR part 63,
subpart E, the authorities contained in paragraph (c) of this section
are retained by the Administrator of the U.S. EPA and are not
transferred to the State, local, or tribal agency.
(c) The authorities that cannot be delegated to State, local, or
tribal agencies are as specified in paragraphs (c)(1) through (4) of
this section.
[[Page 103]]
(1) Approval of alternatives to the applicability requirements in
Sec. Sec. 63.9782 and 63.9784, the compliance date requirements in
Sec. 63.9786, and the emission limitations in Sec. 63.9788.
(2) Approval of major changes to test methods under Sec.
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
(3) Approval of major changes to monitoring under Sec. 63.8(f) and
as defined in Sec. 63.90.
(4) Approval of major changes to recordkeeping and reporting under
Sec. 63.10(f) and as defined in Sec. 63.90.
Sec. 63.9824 What definitions apply to this subpart?
Terms used in this subpart are defined in the Clean Air Act, in 40
CFR 63.2, the General Provisions of this part, and in this section as
follows:
Additive means a minor addition of a chemical, mineral, or metallic
substance that is added to a refractory mixture to facilitate processing
or impart specific properties to the final refractory product.
Add-on air pollution control device (APCD) means equipment installed
on a process vent that reduces the quantity of a pollutant that is
emitted to the air.
Autoclave means a vessel that is used to impregnate fired and/or
unfired refractory shapes with pitch to form pitch-impregnated
refractory products. Autoclaves also can be used as defumers following
the impregnation process.
Bag leak detection system means an instrument that is capable of
monitoring particulate matter loadings in the exhaust of a fabric filter
in order to detect bag failures. A bag leak detection system includes,
but is not limited to, an instrument that operates on triboelectric,
light-scattering, light-transmittance, or other effects to monitor
relative PM loadings.
Basket means the metal container used to hold refractory shapes for
pitch impregnation during the shape preheating, impregnation, defuming,
and, if applicable, coking processes.
Batch process means a process in which a set of refractory shapes is
acted upon as a single unit according to a predetermined schedule,
during which none of the refractory shapes being processed are added or
removed. A batch process does not operate continuously.
Binder means a substance added to a granular material to give it
workability and green or dry strength.
Catalytic oxidizer means an add-on air pollution control device that
is designed specifically to destroy organic compounds in a process
exhaust gas stream by catalytic incineration. A catalytic oxidizer
includes a bed of catalyst media through which the process exhaust
stream passes to promote combustion and incineration at a lower
temperature than would be possible without the catalyst.
Chromium refractory product means a refractory product that contains
at least 1 percent chromium by weight.
Clay refractory product means a refractory product that contains at
least 10 percent uncalcined clay by weight prior to firing in a kiln. In
this definition, the term ``clay'' means any of the following six
classifications of clay defined by the U.S. Geologic Survey: ball clay,
bentonite, common clay and shale, fire clay, fuller's earth, and kaolin.
Coking oven means a thermal process unit that operates at a peak
temperature typically between 540[deg] and 870 [deg]C (1000[deg] and
1600 [deg]F) and is used to drive off the volatile constituents of
pitch-impregnated refractory shapes under a reducing or oxygen-deprived
atmosphere.
Continuous parameter monitoring system (CPMS) means the total
equipment that is used to measure and record temperature, pressure,
liquid flow rate, gas flow rate, or pH on a continuous basis in one or
more locations. ``Total equipment'' includes the sensor, mechanical
components, electronic components, data acquisition system, data
recording system, electrical wiring, and other components of a CPMS.
Continuous process means a process that operates continuously. In a
continuous process unit, the materials or shapes that are processed are
either continuously charged (fed) to and discharged from the process
unit, or are charged and discharged at regular time intervals without
the process unit being shut down. Continuous thermal process units, such
as tunnel kilns,
[[Page 104]]
generally include temperature zones that are maintained at relatively
constant temperature and through which the materials or shapes being
processed are conveyed continuously or at regular time intervals.
Curing oven means a thermal process unit that operates at a peak
temperature typically between 90[deg] and 340 [deg]C (200[deg] and 650
[deg]F) and is used to activate a thermosetting resin, pitch, or other
binder in refractory shapes. Curing ovens also perform the same function
as shape dryers in removing the free moisture from refractory shapes.
Defumer means a process unit that is used for holding pitch-
impregnated refractory shapes as the shapes defume or cool immediately
following the impregnation process. This definition includes autoclaves
that are opened and exhausted to the atmosphere following an
impregnation cycle and used for holding pitch-impregnated refractory
shapes while the shapes defume or cool.
Deviation means any instance in which an affected source subject to
this subpart, or an owner or operator of such a source:
(1) Fails to meet any requirement or obligation established by this
subpart including, but not limited to, any emission limitation (emission
limit, operating limit, or work practice standard);
(2) Fails to meet any term or condition that is adopted to implement
an applicable requirement in this subpart for any affected source
required to obtain such a permit; or
(3) Fails to meet any emission limitation (emission limit, operating
limit, or work practice standard) in this subpart during startup,
shutdown, or malfunction, regardless of whether or not such failure is
permitted by this subpart.
Dry injection fabric filter (DIFF) means an add-on air pollution
control device that includes continuous injection of hydrated lime or
other sorbent into a duct or reaction chamber followed by a fabric
filter.
Dry lime scrubber/fabric filter (DLS/FF) means an add-on air
pollution control device that includes continuous injection of
humidified hydrated lime or other sorbent into a reaction chamber
followed by a fabric filter. These systems may include recirculation of
some of the sorbent.
Dry limestone adsorber (DLA) means an air pollution control device
that includes a limestone storage bin, a reaction chamber that is
essentially a packed-tower filled with limestone, and may or may not
include a peeling drum that mechanically scrapes reacted limestone to
regenerate the stone for reuse.
Emission limitation means any restriction on the emissions a process
unit may discharge.
Fabric filter means an add-on air pollution control device used to
capture particulate matter by filtering a process exhaust stream through
a filter or filter media; a fabric filter is also known as a baghouse.
Fired refractory shape means a refractory shape that has been fired
in a kiln.
HAP means any hazardous air pollutant that appears in section 112(b)
of the Clean Air Act.
Kiln means a thermal process unit that operates at a peak
temperature greater than 820 [deg]C (1500 [deg]F) and is used for firing
or sintering refractory, ceramic, or other shapes.
Kiln furniture means any refractory shape that is used to hold,
support, or position ceramic or refractory products in a kiln during the
firing process.
Maximum organic HAP processing rate means the combination of process
and refractory product formulation that has the greatest potential to
emit organic HAP. The maximum organic HAP processing rate is a function
of the organic HAP processing rate, process operating temperature, and
other process operating parameters that affect emissions of organic HAP.
(See also the definition of organic HAP processing rate.)
Organic HAP processing rate means the rate at which the mass of
organic HAP materials contained in refractory shapes are processed in an
affected thermal process unit. The organic HAP processing rate is a
function of the amount of organic HAP contained in the resins, binders,
and additives used in a refractory mix; the amounts of those resins,
binders, and additives in the refractory mix; and the rate at which the
refractory shapes formed
[[Page 105]]
from the refractory mix are processed in an affected thermal process
unit. For continuous process units, the organic HAP processing rate is
expressed in units of mass of organic HAP per unit of time (e.g., pounds
per hour). For batch process units, the organic HAP processing rate is
expressed in units of mass of organic HAP per unit mass of refractory
shapes processed during the batch process cycle (e.g., pounds per ton).
Particulate matter (PM) means, for the purposes of this subpart,
emissions of particulate matter that serve as a measure of total
particulate emissions as measured by EPA Method 5 of 40 CFR part 60,
appendix A.
Peak emissions period means the period of consecutive hourly mass
emissions of the applicable pollutant that is greater than any other
period of consecutive hourly mass emissions for the same pollutant over
the course of a specified batch process cycle, as defined in paragraphs
(1) and (2) of this definition. The peak emissions period is a function
of the rate at which the temperature of the refractory shapes is
increased, the mass and loading configuration of the shapes in the
process unit, the constituents of the refractory mix, and the type of
pollutants emitted.
(1) The 3-hour peak THC emissions period is the period of 3
consecutive hours over which the sum of the hourly THC mass emissions
rates is greater than the sum of the hourly THC mass emissions rates for
any other period of 3 consecutive hours during the same batch process
cycle.
(2) The 3-hour peak HF emissions period is the period of 3
consecutive hours over which the sum of the hourly HF mass emissions
rates is greater than the sum of the hourly HF mass emissions rates for
any other period of 3 consecutive hours during the same batch process
cycle.
Period of natural gas curtailment or supply interruption means a
period of time during which the supply of natural gas to an affected
facility is halted for reasons beyond the control of the facility. An
increase in the cost or unit price of natural gas does not constitute a
period of natural gas curtailment or supply interruption.
Pitch means the residue from the distillation of petroleum or coal
tar.
Pitch-bonded refractory product means a formed refractory product
that is manufactured using pitch as a bonding agent. Pitch-bonded
refractory products are manufactured by mixing pitch with magnesium
oxide, graphite, alumina, silicon carbide, silica, or other refractory
raw materials, and forming the mix into shapes. After forming, pitch-
bonded refractory products are cured in a curing oven and may be
subsequently fired in a kiln.
Pitch-impregnated refractory product means a refractory shape that
has been fired in a kiln, then impregnated with heated coal tar or
petroleum pitch under pressure. After impregnation, pitch-impregnated
refractory shapes may undergo the coking process in a coking oven. The
total carbon content of a pitch-impregnated refractory product is less
than 50 percent.
Pitch working tank means a tank that is used for heating pitch to
the impregnation temperature, typically between 150[deg] and 260 [deg]C
(300[deg] and 500 [deg]F); temporarily storing heated pitch between
impregnation cycles; and transferring pitch to and from the autoclave
during the impregnation step in manufacturing pitch-impregnated
refractory products.
Plant site means all contiguous or adjoining property that is under
common control, including properties that are separated only by a road
or other public right-of-way. Common control includes properties that
are owned, leased, or operated by the same entity, parent entity,
subsidiary, or any combination thereof.
Redundant sensor means a second sensor or a back-up sensor that is
integrated into a CPMS and is used to check the parameter value (e.g.,
temperature, pressure) measured by the primary sensor of the CPMS.
Refractory product means nonmetallic materials containing less than
50 percent carbon by weight and having those chemical and physical
properties that make them applicable for structures, or as components of
systems, that are exposed to environments above 538 [deg]C (1000
[deg]F). This definition includes, but is not limited to: refractory
bricks, kiln furniture, crucibles,
[[Page 106]]
refractory ceramic fiber, and other materials used as linings for
boilers, kilns, and other processing units and equipment where extremes
of temperature, corrosion, and abrasion would destroy other materials.
Refractory products that use organic HAP means resin-bonded
refractory products, pitch-bonded refractory products, and other
refractory products that are produced using a substance that is an
organic HAP, that releases an organic HAP during production of the
refractory product, or that contains an organic HAP, such as methanol or
ethylene glycol.
Refractory shape means any refractory piece forming a stable mass
with specific dimensions.
Research and development process unit means any process unit whose
purpose is to conduct research and development for new processes and
products and is not engaged in the manufacture of products for
commercial sale, except in a de minimis manner.
Resin-bonded refractory product means a formed refractory product
that is manufactured using a phenolic resin or other type of
thermosetting resin as a bonding agent. Resin-bonded refractory products
are manufactured by mixing resin with alumina, magnesium oxide,
graphite, silica, zirconia, or other refractory raw materials, and
forming the mix into shapes. After forming, resin-bonded refractory
products are cured in a curing oven and may be subsequently fired in a
kiln.
Responsible official means one of the following:
(1) For a corporation: a president, secretary, treasurer, or vice-
president of the corporation in charge of a principal business function,
or any other person who performs similar policy or decisionmaking
functions for the corporation, or a duly authorized representative of
such person if the representative is responsible for the overall
operation of one or more manufacturing, production, or operating
facilities applying for or subject to a permit and either:
(i) The facilities employ more than 250 persons or have gross annual
sales or expenditures exceeding $25 million (in second quarter 1980
dollars); or
(ii) The delegation of authority to such representatives is approved
in advance by the Administrator;
(2) For a partnership or sole proprietorship: a general partner or
the proprietor, respectively;
(3) For a municipality, State, Federal, or other public agency:
either a principal executive officer or ranking elected official. For
the purposes of this part, a principal executive officer of a Federal
agency includes the chief executive officer having responsibility for
the overall operations of a principal geographic unit of the agency
(e.g., a Regional Administrator of EPA); or
(4) For affected sources (as defined in this subpart) applying for
or subject to a title V permit: ``responsible official'' shall have the
same meaning as defined in part 70 or Federal title V regulations in
this chapter (42 U.S.C. 7661), whichever is applicable.
Shape dryer means a thermal process unit that operates at a peak
temperature typically between 40[deg] and 700 [deg]C (100[deg] and 1300
[deg]F) and is used exclusively to reduce the free moisture content of a
refractory shape. Shape dryers generally are the initial thermal process
step following the forming step in refractory products manufacturing.
(See also the definition of a curing oven.)
Shape preheater means a thermal process unit that operates at a peak
temperature typically between 180[deg] and 320 [deg]C (350[deg] and 600
[deg]F) and is used to heat fired refractory shapes prior to the
impregnation step in manufacturing pitch-impregnated refractory
products.
Thermal oxidizer means an add-on air pollution control device that
includes one or more combustion chambers and is designed specifically to
destroy organic compounds in a process exhaust gas stream by
incineration.
Uncalcined clay means clay that has not undergone thermal processing
in a calciner.
Wet scrubber means an add-on air pollution control device that
removes pollutants from a gas stream by bringing them into contact with
a liquid, typically water.
Work practice standard means any design, equipment, work practice,
or operational standard, or combination
[[Page 107]]
thereof, that is promulgated pursuant to section 112(h) of the Clean Air
Act.
Table 1 to Subpart SSSSS of Part 63--Emission Limits
As stated in Sec. 63.9788, you must comply with the emission limits
for affected sources in the following table:
------------------------------------------------------------------------
You must meet the following
For . . . emission limits . . .
------------------------------------------------------------------------
1. Each new or existing curing oven, As specified in items 2 through
shape dryer, and kiln that is used to 9 of this table.
process refractory products that use
organic HAP; each new or existing
coking oven and defumer that is used
to produce pitch-impregnated
refractory products; each new shape
preheater that is used to produce
pitch-impregnated refractory products;
AND each new or existing process unit
that is exhausted to a thermal or
catalytic oxidizer that also controls
emissions from an affected shape
preheater or pitch working tank.
2. Continuous process units that are a. The 3-hour block average THC
controlled with a thermal or catalytic concentration must not exceed
oxidizer. 20 parts per million by
volume, dry basis (ppmvd),
corrected to 18 percent
oxygen, at the outlet of the
control device; or
b. The 3-hour block average THC
mass emissions rate must be
reduced by at least 95
percent.
3. Continuous process units that are a. The 3-hour block average THC
equipped with a control device other concentration must not exceed
than a thermal or catalytic oxidizer. 20 ppmvd, corrected to 18
percent oxygen, at the outlet
of the control device; or
b. The 3-hour block average THC
mass emissions rate must be
reduced by at least 95
percent.
4. Continuous process units that use The 3-hour block average THC
process changes to reduce organic HAP concentration must not exceed
emissions. 20 ppmvd, corrected to 18
percent oxygen, at the outlet
of the process gas stream.
5. Continuous kilns that are not The 3-hour block average THC
equipped with a control device. concentration must not exceed
20 ppmvd, corrected to 18
percent oxygen, at the outlet
of the process gas stream.
6. Batch process units that are a. The 2-run block average THC
controlled with a thermal or catalytic concentration for the 3-hour
oxidizer. peak emissions period must not
exceed 20 ppmvd, corrected to
18 percent oxygen, at the
outlet of the control device;
or
b. The 2-run block average THC
mass emissions rate for the 3-
hour peak emissions period
must be reduced by at least 95
percent.
7. Batch process units that are a. The 2-run block average THC
equipped with a control device other concentration for the 3-hour
than a thermal or catalytic oxidizer. peak emissions period must not
exceed 20 ppmvd, corrected to
18 percent oxygen, at the
outlet of the control device;
or
b. The 2-run block average THC
mass emissions rate for the 3-
hour peak emissions period
must be reduced by at least 95
percent.
8. Batch process units that use process The 2-run block average THC
changes to reduce organic HAP concentration for the 3-hour
emissions. peak emissions period must not
exceed 20 ppmvd, corrected to
18 percent oxygen, at the
outlet of the process gas
stream.
9. Batch process kilns that are not The 2-run block average THC
equipped with a control device. concentration for the 3-hour
peak emissions period must not
exceed 20 ppmvd, corrected to
18 percent oxygen, at the
outlet of the process gas
stream.
10. Each new continuous kiln that is a. The 3-hour block average HF
used to produce clay refractory emissions must not exceed
products. 0.019 kilograms per megagram
(kg/Mg) (0.038 pounds per ton
(lb/ton)) of uncalcined clay
processed, OR the 3-hour block
average HF mass emissions rate
must be reduced by at least 90
percent; and
b. The 3-hour block average HCl
emissions must not exceed
0.091 kg/Mg (0.18 lb/ton) of
uncalcined clay processed, OR
the 3-hour block average HCl
mass emissions rate must be
reduced by at least 30
percent.
11. Each new batch process kiln that is a. The 2-run block average HF
used to produce clay refractory mass emissions rate for the 3-
products. hour peak emissions period
must be reduced by at least 90
percent; and
b. The 2-run block average HCl
mass emissions rate for the 3-
hour peak emissions period
must be reduced by at least 30
percent.
------------------------------------------------------------------------
[[Page 108]]
Table 2 to Subpart SSSSS of Part 63--Operating Limits
As stated in Sec. 63.9788, you must comply with the operating
limits for affected sources in the following table:
------------------------------------------------------------------------
For . . . You must . . .
------------------------------------------------------------------------
1. Each affected source listed in Table a. Operate all affected sources
1 to this subpart. according to the requirements
to this subpart on and after
the date on which the initial
performance test is conducted
or required to be conducted,
whichever date is earlier; and
b. Capture emissions and vent
them through a closed system;
and
c. Operate each control device
that is required to comply
with this subpart on each
affected source during all
periods that the source is
operating, except where
specified in Sec.
63.9792(e), item 2 of this
table, and item 13 of Table 4
to this subpart; and
d. Record all operating
parameters specified in Table
8 to this subpart for the
affected source; and
e. Prepare and implement a
written OM&M plan as specified
in Sec. 63.9792(d).
2. Each affected continuous kiln that a. Receive approval from the
is equipped with an emission control Administrator before taking
device. the control device on the
affected kiln out of service
for scheduled maintenance, as
specified in Sec.
63.9792(e); and
b. Minimize HAP emissions from
the affected kiln during all
periods of scheduled
maintenance of the kiln
control device when the kiln
is operating and the control
device is out of service; and
c. Minimize the duration of all
periods of scheduled
maintenance of the kiln
control device when the kiln
is operating and the control
device is out of service.
3. Each new or existing curing oven, Satisfy the applicable
shape dryer, and kiln that is used to operating limits specified in
process refractory products that use items 4 through 9 of this
organic HAP; each new or existing table.
coking oven and defumer that is used
to produce pitch-impregnated
refractory products; each new shape
preheater that is used to produce
pitch-impregnated refractory products;
AND each new or existing process unit
that is exhausted to a thermal or
catalytic oxidizer that also controls
emissions from an affected shape
preheater or pitch working tank.
4. Each affected continuous process Maintain the 3-hour block
unit. average organic HAP processing
rate (pounds per hour) at or
below the maximum organic HAP
processing rate established
during the most recent
performance test.
5. Continuous process units that are Maintain the 3-hour block
equipped with a thermal oxidizer. average operating temperature
in the thermal oxidizer
combustion chamber at or above
the minimum allowable
operating temperature for the
oxidizer established during
the most recent performance
test.
6. Continuous process units that are a. Maintain the 3-hour block
equipped with a catalytic oxidizer. average operating temperature
at the inlet of the catalyst
bed of the oxidizer at or
above the minimum allowable
operating temperature for the
oxidizer established during
the most recent performance
test; and
b. Check the activity level of
the catalyst at least every 12
months.
7. Each affected batch process unit.... For each batch cycle, maintain
the organic HAP processing
rate (pounds per batch) at or
below the maximum organic HAP
processing rate established
during the most recent
performance test.
8. Batch process units that are a. From the start of each batch
equipped with a thermal oxidizer. cycle until 3 hours have
passed since the process unit
reached maximum temperature,
maintain the hourly average
operating temperature in the
thermal oxidizer combustion
chamber at or above the
minimum allowable operating
temperature established for
the corresponding period
during the most recent
performance test, as
determined according to item
11 of Table 4 to this subpart;
and
b. For each subsequent hour of
the batch cycle, maintain the
hourly average operating
temperature in the thermal
oxidizer combustion chamber at
or above the minimum allowable
operating temperature
established for the
corresponding hour during the
most recent performance test,
as specified in item 13 of
Table 4 to this subpart.
[[Page 109]]
9. Batch process units that are a. From the start of each batch
equipped with a catalytic oxidizer. cycle until 3 hours have
passed since the process unit
reached maximum temperature,
maintain the hourly average
operating temperature at the
inlet of the catalyst bed at
or above the minimum allowable
operating temperature
established for the
corresponding period during
the most recent performance
test, as determined according
to item 12 of Table 4 to this
subpart; and
b. For each subsequent hour of
the batch cycle, maintain the
hourly average operating
temperature at the inlet of
the catalyst bed at or above
the minimum allowable
operating temperature
established for the
corresponding hour during the
most recent performance test,
as specified in item 13 of
Table 4 to this subpart; and
c. Check the activity level of
the catalyst at least every 12
months.
10. Each new kiln that is used to Satisfy the applicable
process clay refractory products. operating limits specified in
items 11 through 13 of this
table.
11. Each affected kiln that is equipped a. Maintain the 3-hour block
with a DLA. average pressure drop across
the DLA at or above the
minimum levels established
during the most recent
performance test; and
b. Maintain free-flowing
limestone in the feed hopper,
silo, and DLA at all times;
and
c. Maintain the limestone
feeder at or above the level
established during the most
recent performance test; and
d. Use the same grade of
limestone from the same source
as was used during the most
recent performance test and
maintain records of the source
and type of limestone used.
12. Each affected kiln that is equipped a. Initiate corrective action
with a DIFF or DLS/FF. within 1 hour of a bag leak
detection system alarm and
complete corrective actions in
accordance with the OM&M plan;
and
b. Verify at least once each 8-
hour shift that lime is free-
flowing by means of a visual
check, checking the output of
a load cell, carrier gas/lime
flow indicator, or carrier gas
pressure drop measurement
system; and
c. Record the lime feeder
setting daily to verify that
the feeder setting is at or
above the level established
during the most recent
performance test.
13. Each affected kiln that is equipped a. Maintain the 3-hour block
with a wet scrubber. average pressure drop across
the scrubber, liquid pH, and
liquid flow rate at or above
the minimum levels established
during the most recent
performance test; and
b. If chemicals are added to
the scrubber liquid, maintain
the 3-hour block average
chemical feed rate at or above
the minimum chemical feed rate
established during the most
recent performance test.
------------------------------------------------------------------------
Table 3 to Subpart SSSSS of Part 63--Work Practice Standards
As stated in Sec. 63.9788, you must comply with the work practice
standards for affected sources in the following table:
[[Page 110]]
------------------------------------------------------------------------
According to one
For . . . You must . . . of the following
requirements . . .
------------------------------------------------------------------------
1. Each basket or container that a. Control POM i. At least every
is used for holding fired emissions from 10 preheating
refractory shapes in an any affected cycles, clean the
existing shape preheater and shape preheater. residual pitch
autoclave during the pitch from the surfaces
impregnation process. of the basket or
container by
abrasive blasting
prior to placing
the basket or
container in the
affected shape
preheater; or
ii. At least every
10 preheating
cycles, subject
the basket or
container to a
thermal process
cycle that meets
or exceeds the
operating
temperature and
cycle time of the
affected
preheater, AND is
conducted in a
process unit that
is exhausted to a
thermal or
catalytic
oxidizer that is
comparable to the
control device
used on an
affected defumer
or coking oven;
or
iii. Capture
emissions from
the affected
shape preheater
and vent them to
the control
device that is
used to control
emissions from an
affected defumer
or coking oven,
or to a
comparable
thermal or
catalytic
oxidizer.
2. Each new or existing pitch Control POM Capture emissions
working tank. emissions. from the affected
pitch working
tank and vent
them to the
control device
that is used to
control emissions
from an affected
defumer or coking
oven, OR to a
comparable
thermal or
catalytic
oxidizer.
3. Each new or existing chromium Minimize fuel- Use natural gas,
refractory products kiln. based HAP or equivalent, as
emissions. the kiln fuel,
except during
periods of
natural gas
curtailment or
supply
interruption, as
defined in Sec.
63.9824.
4. Each existing clay refractory Minimize fuel- Use natural gas,
products kiln. based HAP or equivalent, as
emissions. the kiln fuel,
except during
periods of
natural gas
curtailment or
supply
interruption, as
defined in Sec.
63.9824.
------------------------------------------------------------------------
Table 4 to Subpart SSSSS to Part 63--Requirements for Performance Tests
As stated in Sec. 63.9800, you must comply with the requirements
for performance tests for affected sources in the following table:
----------------------------------------------------------------------------------------------------------------
According to the
For . . . You must . . . Using . . . following requirements
. . .
----------------------------------------------------------------------------------------------------------------
1. Each affected source listed in a. Conduct performance i. The requirements of (1) Record the date of
Table 1 to this subpart. tests. the general provisions the test; and
in subpart A of this (2) Identify the
part and the emission source that
requirements to this is tested; and
subpart. (3) Collect and record
the corresponding
operating parameter
and emission test data
listed in this table
for each run of the
performance test; and
(4) Repeat the
performance test at
least every 5 years;
and
(5) Repeat the
performance test
before changing the
parameter value for
any operating limit
specified in your OM&M
plan; and
(6) If complying with
the THC concentration
or THC percentage
reduction limits
specified in items 2
through 9 of Table 1
to this subpart,
repeat the performance
test under the
conditions specified
in items 2.a.2. and
2.a.3. of this table;
and
[[Page 111]]
(7) If complying with
the emission limits
for new clay
refractory products
kilns specified in
items 10 and 11 of
Table 1 to this
subpart, repeat the
performance test under
the conditions
specified in items
14.a.i.4. and
17.a.i.4. of this
table.
b. Select the locations i. Method 1 or 1A of 40 (1) To demonstrate
of sampling ports and CFR part 60, appendix compliance with the
the number of traverse A. percentage reduction
points. limits specified in
items 2.b., 3.b.,
6.b., 7.b., 10, and 11
of Table 1 to this
subpart, locate
sampling sites at the
inlet of the control
device and at either
the outlet of the
control device or at
the stack prior to any
releases to the
atmosphere; and
(2) To demonstrate
compliance with any
other emission limit
specified in Table 1
to this subpart,
locate all sampling
sites at the outlet of
the control device or
at the stack prior to
any releases to the
atmosphere.
c. Determine gas Method 2, 2A, 2C, 2D, Measure gas velocities
velocity and volumetric 2F, or 2G of 40 CFR and volumetric flow
flow rate. part 60, appendix A. rates at 1-hour
intervals throughout
each test run.
d. Conduct gas molecular (i) Method 3, 3A, or 3B As specified in the
weight analysis. of 40 CFR part 60, applicable test
appendix A; or method.
(ii) ASME PTC 19.10- You may use ASME PTC
1981-Part 10. 19.10-1981-Part 10
(available for
purchase from Three
Park Avenue, New York,
NY 10016-5990) as an
alternative to EPA
Method 3B.
e. Measure gas moisture Method 4 of 40 CFR part As specified in the
content. 60, appendix A. applicable test
method.
[[Page 112]]
2. Each new or existing curing oven, a. Conduct performance ....................... (1) Conduct the
shape dryer, and kiln that is used tests. performance test while
to process refractory products that the source is
use organic HAP; each new or operating at the
existing coking oven and defumer maximum organic HAP
that is used to produce pitch- processing rate, as
impregnated refractory products; defined in Sec.
each new shape preheater that is 63.9824, reasonably
used to produce pitch-impregnated expected to occur; and
refractory products; AND each new (2) Repeat the
or existing process unit that is performance test
exhausted to a thermal or catalytic before starting
oxidizer that also controls production of any
emissions from an affected shape product for which the
preheater or pitch working tank. organic HAP processing
rate is likely to
exceed the maximum
organic HAP processing
rate established
during the most recent
performance test by
more than 10 percent,
as specified in Sec.
63.9798(c); and
(3) Repeat the
performance test on
any affected
uncontrolled kiln
following process
changes (e.g., shorter
curing oven cycle
time) that could
increase organic HAP
emissions from the
affected kiln, as
specified in Sec.
63.9798(d).
b. Satisfy the
applicable requirements
listed in items 3
through 13 of this
table.
3. Each affected continuous process a. Perform a minimum of The appropriate test Each test run must be
unit. 3 test runs. methods specified in at least 1 hour in
items 1, 4, and 5 of duration.
this table.
b. Establish the i. Method 311 of 40 CFR (1) Calculate and
operating limit for the part 63, appendix A, record the organic HAP
maximum organic HAP OR material safety content of all
processing rate. data sheets (MSDS), OR refractory shapes that
product labels to are processed during
determine the mass the performance test,
fraction of organic based on the mass
HAP in each resin, fraction of organic
binder, or additive; HAP in the resins,
and binders, or additives;
the mass fraction of
each resin, binder, or
additive, in the
product; and the
process feed rate; and
ii. Product formulation (2) Calculate and
data that specify the record the organic HAP
mass fraction of each processing rate
resin, binder, and (pounds per hour) for
additive in the each test run; and
products that are
processed during the
performance test; and
iii. Process feed rate (3) Calculate and
data (tons per hour). record the maximum
organic HAP processing
rate as the average of
the organic HAP
processing rates for
the three test runs.
c. Record the operating Process data........... During each test run
temperature of the and at least once per
affected source. hour, record the
operating temperature
in the highest
temperature zone of
the affected source.
[[Page 113]]
4. Each continuous process unit that a. Measure THC i. Method 25A of 40 CFR (1) Each minute,
is subject to the THC emission concentrations at the part 60, appendix A. measure and record the
limit listed in item 2.a., 3.a., 4, outlet of the control concentrations of THC
or 5 of Table 1 to this subpart. device or in the stack. in the exhaust stream;
and
(2) Provide at least 50
1-minute measurements
for each valid hourly
average THC
concentration.
b. Measure oxygen i. Method 3A of 40 CFR (1) Each minute,
concentrations at the part 60, appendix A. measure and record the
outlet of the control concentrations of
device or in the stack. oxygen in the exhaust
stream; and
(2) Provide at least 50
1-minute measurements
for each valid hourly
average THC
concentration.
c. Determine the hourly i. Equation 1 of Sec. (1) Calculate the
average THC 63.9800(g)(1); and. hourly average THC
concentration, ii. The 1-minute THC concentration for each
corrected to 18 percent and oxygen hour of the
oxygen. concentration data. performance test as
the average of the 1-
minute THC
measurements; and
(2) Calculate the
hourly average oxygen
concentration for each
hour of the
performance test as
the average of the 1-
minute oxygen
measurements; and
(3) Correct the hourly
average THC
concentrations to 18
percent oxygen using
Equation 1 of Sec.
63.9800(g)(1).
d. Determine the 3-hour The hourly average Calculate the 3-hour
block average THC concentration of THC, block average THC
emission concentration, corrected to 18 emission
corrected to 18 percent percent oxygen, for concentration,
oxygen. each test run. corrected to 18
percent oxygen, as the
average of the hourly
average THC emission
concentrations,
corrected to 18
percent oxygen.
5. Each continuous process unit that a. Measure THC i. Method 25A of 40 CFR (1) Each minute,
is subject to the THC percentage concentrations at the part 60, appendix A. measure and record the
reduction limit listed in item 2.b. inlet and outlet of the concentrations of THC
or 3.b. of Table 1 to this subpart. control device. at the inlet and
outlet of the control
device; and
(2) Provide at least 50
1-minute measurements
for each valid hourly
average THC
concentration at the
control device inlet
and outlet.
b. Determine the hourly i. The 1-minute THC Calculate the hourly
THC mass emissions concentration data at THC mass emissions
rates at the inlet and the control device rates at the control
outlet of the control inlet and outlet; and device inlet and
device. ii. The volumetric flow outlet for each hour
rates at the control of the performance
device inlet and test.
outlet.
c. Determine the 3-hour i. The hourly THC mass (1) Calculate the
block average THC emissions rates at the hourly THC percentage
percentage reduction. inlet and outlet of reduction for each
the control device. hour of the
performance test using
Equation 2 of Sec.
63.9800(g)(1); and
(2) Calculate the 3-
hour block average THC
percentage reduction.
[[Page 114]]
6. Each continous process unit that a. Establish the i. Continuous recording (1) At least every 15
is equipped with a thermal oxidizer. operating limit for the of the output of the minutes, measure and
minimum allowable combustion chamber record the thermal
thermal oxidizer temperature oxidizer combustion
combustion chamber measurement device. chamber temperature;
temperature. and
(2) Provide at least
one measurement during
at least three 15-
minute periods per
hour of testing; and
(3) Calculate the
hourly average thermal
oxidizer combustion
chamber temperature
for each hour of the
performance test; and
(4) Calculate the
minimum allowable
combustion chamber
temperature as the
average of the
combustion chamber
temperatures for the
three test runs, minus
14 [deg]C (25 [deg]F).
7. Each continuous process unit that a. Establish the i. Continuous recording (1) At least every 15
is equipped with a catalytic operating limit for the of the output of the minutes, measure and
oxidizer. minimum allowable temperature record the temperature
temperature at the measurement device. at the inlet of the
inlet of the catalyst catalyst bed; and
bed. (2) Provide at least
one catalyst bed inlet
temperature
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average
catalyst bed inlet
temperature for each
hour of the
performance test; and
(4) Calculate the
minimum allowable
catalyst bed inlet
temperature as the
average of the
catalyst bed inlet
temperatures for the
three test runs, minus
14 [deg]C (25 [deg]F).
8. Each affected batch process unit. a. Perform a minimum of i. The appropriate test (1) Each test run must
two test runs. methods specified in be conducted over a
items 1, 9, and 10 of separate batch cycle
this table. unless you satisfy the
requirements of Sec.
63.9800(f)(3) and (4);
and
(2) Each test run must
begin with the start
of a batch cycle,
except as specified in
item 8.a.i.4. of this
table; and
(3) Each test run must
continue until the end
of the batch cycle,
except as specified in
items 8.a.i.4. and
8.a.i.5. of this
table; and
(4) If you develop an
emissions profile, as
described in Sec.
63.9802(a), AND for
sources equipped with
a thermal or catalytic
oxidizer, you do not
reduce the oxidizer
operating temperature,
as specified in item
13 of this table, you
can limit each test
run to the 3-hour peak
THC emissions period;
and
[[Page 115]]
(5) If you do not
develop an emissions
profile, a test run
can be stopped, and
the results of that
run considered
complete, if you
measure emissions
continuously until at
least 3 hours after
the affected process
unit has reached
maximum temperature,
AND the hourly average
THC mass emissions
rate has not increased
during the 3-hour
period since maximum
process temperature
was reached, and the
hourly average
concentrations of THC
at the inlet of the
control device have
not exceeded 20 ppmvd,
corrected to 18
percent oxygen, during
the 3-hour period
since maximum process
temperature was
reached or the hourly
average THC percentage
reduction has been at
least 95 percent
during the 3-hour
period since maximum
process temperature
was reached, AND, for
sources equipped with
a thermal or catalytic
oxidizer, at least 1
hour has passed since
any reduction in the
operating temperature
of the oxidizer, as
specified in item 13
of this table.
b. Establish the i. Method 311 of 40 CFR (1) Calculate and
operating limit for the part 63, appendix A, record the organic HAP
maximum organic HAP OR MSDS, OR product content of all
processing rate. labels to determine refractory shapes that
the mass fraction of are processed during
organic HAP in each the performance test,
resin, binder, or based on the mass
additive; and fraction of HAP in the
resins, binders, or
additives; the mass
fraction of each
resin, binder, or
additive, in the
product, and the batch
weight prior to
processing; and
ii. Product formulation (2) Calculate and
data that specify the record the organic HAP
mass fraction of each processing rate
resin, binder, and (pounds per batch) for
additive in the each test run; and
products that are (3) Calculate and
processed during the record the maximum
performance test; and organic HAP processing
iii. Batch weight rate as the average of
(tons). the organic HAP
processing rates for
the two test runs.
c. Record the batch Process data........... Record the total
cycle time. elapsed time from the
start to the
completion of the
batch cycle.
d. Record the operating Process data........... Record the operating
temperature of the temperature of the
affected source. affected source at
least once every hour
from the start to the
completion of the
batch cycle.
9. Each batch process unit that is a. Measure THC i. Method 25A of 40 CFR (1) Each minute,
subject to the THC emission limit concentrations at the part 60, appendix A. measure and record the
listed in item 6.a., 7.a., 8, or 9 outlet of the control concentrations of THC
of Table 1 to this subpart. device or in the stack. in the exhaust stream;
and
(2) Provide at least 50
1-minute measurements
for each valid hourly
average THC
concentration.
[[Page 116]]
b. Measure oxygen i. Method 3A of 40 CFR (1) Each minute,
concentrations at the part 60, appendix A. measure and record the
outlet of the control concentrations of
device or in the stack. oxygen in the exhaust
stream; and
(2) Provide at least 50
1-minute measurements
for each valid hourly
average oxygen
concentration.
c. Determine the hourly i. Equation 1 of Sec. (1) Calculate the
average THC 63.9800(g)(1); and. hourly average THC
concentration, ii. The 1-minute THC concentration for each
corrected to 18 percent and oxygen hour of the
oxygen. concentration data. performance test as
the average of the 1-
minute THC
measurements; and
(2) Calculate the
hourly average oxygen
concentration for each
hour of the
performance test as
the average of the 1-
minute oxygen
measurements; and
(3) Correct the hourly
average THC
concentrations to 18
percent oxygen using
Equation 1 of Sec.
63.9800(g)(1).
d. Determine the 3-hour The hourly average THC Select the period of 3
peak THC emissions concentrations, consecutive hours over
period for each test corrected to 18 which the sum of the
run. percent oxygen. hourly average THC
concentrations,
corrected to 18
percent oxygen, is
greater than the sum
of the hourly average
THC emission
concentrations,
corrected to 18
percent oxygen, for
any other period of 3
consecutive hours
during the test run.
e. Determine the average The hourly average THC Calculate the average
THC concentration, emission of the hourly average
corrected to 18 percent concentrations, THC concentrations,
oxygen, for each test corrected to 18 corrected to 18
run. percent oxygen, for percent oxygen, for
the 3-hour peak THC the 3 hours of the
emissions period. peak emissions period
for each test run.
f. Determine the 2-run The average THC Calculate the average
block average THC concentration, of the average THC
concentration, corrected to 18 concentrations,
corrected to 18 percent percent oxygen, for corrected to 18
oxygen, for the each test run. percent oxygen, for
emission test. each run.
10. Each batch process unit that is a. Measure THC i. Method 25A of 40 CFR (1) Each minute,
subject to the THC percentage concentrations at the part 60, appendix A. measure and record the
reduction limit listed in item 6.b. inlet and outlet of the concentrations of THC
or 7.b. of Table 1 to this subpart. control device. at the control device
inlet and outlet; and
(2) Provide at least 50
1-minute measurements
for each valid hourly
average THC
concentration at the
control device inlet
and outlet.
b. Determine the hourly i. The 1-minute THC (1) Calculate the
THC mass emissions concentration data at hourly mass emissions
rates at the control the control device rates at the control
device inlet and outlet. inlet and outlet; and device inlet and
ii. The volumetric flow outlet for each hour
rates at the control of the performance
device inlet and test.
outlet.
c. Determine the 3-hour The hourly THC mass Select the period of 3
peak THC emissions emissions rates at the consecutive hours over
period for each test control device inlet. which the sum of the
run. hourly THC mass
emissions rates at the
control device inlet
is greater than the
sum of the hourly THC
mass emissions rates
at the control device
inlet for any other
period of 3
consecutive hours
during the test run.
d. Determine the average i. Equation 2 of Sec. Calculate the average
THC percentage 63.9800(g)(2); and. THC percentage
reduction for each test ii. The hourly THC mass reduction for each
run. emissions rates at the test run using
control device inlet Equation 2 of Sec.
and outlet for the 3- 63.9800(g)(2).
hour peak THC
emissions period.
[[Page 117]]
e. Determine the 2-run The average THC Calculate the average
block average THC percentage reduction of the average THC
percentage reduction for each test run. percentage reductions
for the emission test. for each test run.
11. Each batch process unit that is a. Establish the i. Continuous recording (1) At least every 15
equipped with a thermal oxidizer. operating limit for the of the output of the minutes, measure and
minimum thermal combustion chamber record the thermal
oxidizer combustion temperature oxidizer combustion
chamber temperature. measurement device. chamber temperature;
and
(2) Provide at least
one temperature
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average
combustion chamber
temperature for each
hour of the 3-hour
peak emissions period,
as defined in item
9.d. or 10.c. of this
table, whichever
applies; and
(4) Calculate the
minimum allowable
thermal oxidizer
combustion chamber
operating temperature
as the average of the
hourly combustion
chamber temperatures
for the 3-hour peak
emissions period,
minus 14 [deg]C (25
[deg]F).
12. Each batch process unit that is a. Establish the i. Continuous recording (1) At least every 15
equipped with a catalytic oxidizer. operating limit for the of the output of the minutes, measure and
minimum temperature at temperature record the temperature
the inlet of the measurement device. at the inlet of the
catalyst bed. catalyst bed; and
(2) Provide at least
one catalyst bed inlet
temperature
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average
catalyst bed inlet
temperature for each
hour of the 3-hour
peak emissions period,
as defined in item
9.d. or 10.c. of this
table, whichever
applies; and
(4) Calculate the
minimum allowable
catalytic oxidizer
catalyst bed inlet
temperature as the
average of the hourly
catalyst bed inlet
temperatures for the 3-
hour peak emissions
period, minus 14
[deg]C (25 [deg]F).
13. Each batch process unit that is a. During each test run, (1) The oxidizer can be
equipped with a thermal or maintain the applicable shut off or the
catalytic oxidizer. operating temperature oxidizer operating
of the oxidizer until temperature can be
emission levels allow reduced if you do not
the oxidizer to be shut use an emission
off or the operating profile to limit
temperature of the testing to the 3-hour
oxidizer to be reduced. peak emissions period,
as specified in item
8.a.i.4. of this
table; and
(2) At least 3 hours
have passed since the
affected process unit
reached maximum
temperature; and
(3) The applicable
emission limit
specified in item 6.a.
or 6.b. of Table 1 to
this subpart was met
during each of the
previous three 1-hour
periods; and
(4) The hourly average
THC mass emissions
rate did not increase
during the 3-hour
period since maximum
process temperature
was reached; and
[[Page 118]]
(5) The applicable
emission limit
specified in item 6.a.
and 6.b. of Table 1 to
this subpart was met
during each of the
four 15-minute periods
immediately following
the oxidizer
temperature reduction;
and
(6) If the applicable
emission limit
specified in item 6.a.
or 6.b. of Table 1 to
this subpart was not
met during any of the
four 15-minute periods
immediately following
the oxidizer
temperature reduction,
you must return the
oxidizer to its normal
operating temperature
as soon as possible
and maintain that
temperature for at
least 1 hour; and
(7) Continue the test
run until the
applicable emission
limit specified in
items 6.a. and 6.b. of
Table 1 to this
subpart is met for at
least four consecutive
15-minute periods that
immediately follow the
temperature reduction;
and
(8) Calculate the
hourly average
oxidizer operating
temperature for each
hour of the
performance test since
the affected process
unit reached maximum
temperature.
14. Each new continuous kiln that is a. Measure emissions of i. Method 26A of 40 CFR (1) Conduct the test
used to process clay refractory HF and HCl. part 60, appendix A; while the kiln is
products. or operating at the
ii. Method 26 of 40 CFR maximum production
part 60, appendix A; level; and
or. (2) You may use Method
iii. Method 320 of 40 26 of 40 CFR part 60,
CFR part 63, appendix appendix A, only if no
A. acid PM (e.g., HF or
HCl dissolved in water
droplets emitted by
sources controlled by
a wet scrubber) is
present; and
(3) If you use Method
320 of 40 CFR part 63,
appendix A, you must
follow the analyte
spiking procedures of
Section 13 of Method
320 unless you can
demonstrate that the
complete spiking
procedure has been
conducted at a similar
source; and
(4) Repeat the
performance test if
the affected source is
controlled with a DLA
and you change the
source of the
limestone used in the
DLA.
b. Perform a minimum of The appropriate test Each test run must be
3 test runs. methods specified in at least 1 hour in
items 1 and 14.a. of duration.
this table.
15. Each new continuous kiln that is a. Record the uncalcined i. Production data; and (1) Record the
subject to the production-based HF clay processing rate. ii. Product formulation production rate (tons
and HCl emission limits specified data that specify the per hour of fired
in items 10.a. and 10.b. of Table 1 mass fraction of product); and
to this subpart. uncalcined clay in the (2) Calculate and
products that are record the average
processed during the rate at which
performance test. uncalcined clay is
processed (tons per
hour) for each test
run; and
(3) Calculate and
record the 3-run
average uncalcined
clay processing rate
as the average of the
average uncalcined
clay processing rates
for each test run.
[[Page 119]]
b. Determine the HF mass i. Method 26A of 40 CFR Calculate the HF mass
emissions rate at the part 60, appendix A; emissions rate for
outlet of the control or each test.
device or in the stack. ii. Method 26 of 40 CFR
part 60, appendix A;
or.
iii. Method 320 of 40
CFR part 63, appendix
A.
c. Determine the 3-hour i. The HF mass (1) Calculate the
block average emissions rate for hourly production-
production-based HF each test run; and based HF emissions
emissions rate. ii. The average rate for each test run
uncalcined clay using Equation 3 of
processing rate. Sec. 63.9800(g)(3);
and
(2) Calculate the 3-
hour block average
production-based HF
emissions rate as the
average of the hourly
production-based HF
emissions rates for
each test run.
d. Determine the HCl i. Method 26A of 40 CFR Calculate the HCl mass
mass emissions rate at part 60, appendix A; emissions rate for
the outlet of the or each test run.
control device or in ii. Method 26 of 40 CFR
the stack. part 60, appendix A;
or.
iii. Method 320 of 40
CFR part 63, appendix
A.
e. Determine the 3-hour i. The HCl mass (1) Calculate the
block average emissions rate for hourly production-
production-based HCl each test run; and based HCl emissions
emissions rate. ii. The average rate for each test run
uncalcined clay using Equation 3 of
processing rate. Sec. 63.9800(g)(3);
and
(2) Calculate the 3-
hour block average
production-based HCl
emissions rate as the
average of the
production-based HCl
emissions rates for
each test run.
16. Each new continuous kiln that is a. Measure the HF mass i. Method 26A of 40 CFR Calculate the HF mass
subject to the HF and HCl emissions rates at the part 60, appendix A; emissions rates at the
percentage reduction limits inlet and outlet of the or control device inlet
specified in items 10.a. and 10.b. control device. ii. Method 26 of 40 CFR and outlet for each
of Table 1 to this subpart. part 60, appendix A; test run.
or.
iii. Method 320 of 40
CFR part 63, appendix
A.
b. Determine the 3-hour i. The HF mass (1) Calculate the
block average HF emissions rates at the hourly HF percentage
percentage reduction. inlet and outlet of reduction using
the control device for Equation 2 of Sec.
each test run 63.9800(g)(2); and
(2) Calculate the 3-
hour block average HF
percentage reduction
as the average of the
HF percentage
reductions for each
test run.
c. Measure the HCl mass i. Method 26A of 40 CFR Calculate the HCl mass
emissions rates at the part 60, appendix A; emissions rates at the
inlet and outlet of the or control device inlet
control device. ii. Method 26 of 40 CFR and outlet for each
part 60, appendix A; test run.
or.
iii. Method 320 of 40
CFR part 63, appendix
A.
d. Determine the 3-hour i. The HCl mass (1) Calculate the
block average HCl emissions rates at the hourly HCl percentage
percentage reduction. inlet and outlet of reduction using
the control device for Equation 2 of Sec.
each test run. 63.9800(g)(2); and
(2) Calculate the 3-
hour block average HCl
percentage reduction
as the average of HCl
percentage reductions
for each test run.
[[Page 120]]
17. Each new batch process kiln that a. Measure emissions of i. Method 26A of 40 CFR (1) Conduct the test
is used to process clay refractory HF and HCl at the inlet part 60, appendix A; while the kiln is
products. and outlet of the or operating at the
control device. ii. Method 26 of 40 CFR maximum production
part 60, appendix A; level; and
or. (2) You may use Method
iii. Method 320 of 40 26 of 40 CFR part 60,
CFR part 63, appendix appendix A, only if no
A. acid PM (e.g., HF or
HCl dissolved in water
droplets emitted by
sources controlled by
a wet scrubber) is
present; and
(3) If you use Method
320 of 40 CFR part 63,
you must follow the
analyte spiking
procedures of Section
13 of Method 320
unless you can
demonstrate that the
complete spiking
procedure has been
conducted at a similar
source; and
(4) Repeat the
performance test if
the affected source is
controlled with a DLA
and you change the
source of the
limestone used in the
DLA.
b. Perform a minimum of i. The appropriate test (1) Each test run must
2 test runs. methods specified in be conducted over a
items 1 and 17.a. of separate batch cycle
this table. unless you satisfy the
requirements of Sec.
63.9800(f)(3) and (4);
and
(2) Each test run must
consist of a series of
1-hour runs at the
inlet and outlet of
the control device,
beginning with the
start of a batch
cycle, except as
specified in item
17.b.i.4. of this
table; and
(3) Each test run must
continue until the end
of the batch cycle,
except as specified in
item 17.b.i.4. of this
table; and
(4) If you develop an
emissions profile, as
described in Sec.
63.9802(b), you can
limit each test run to
the 3-hour peak HF
emissions period.
c. Determine the hourly i. The appropriate test Determine the hourly
HF and HCl mass methods specified in mass HF and HCl
emissions rates at the items 1 and 17.a. of emissions rates at the
inlet and outlet of the this table. inlet and outlet of
control device. the control device for
each hour of each test
run.
d. Determine the 3-hour The hourly HF mass Select the period of 3
peak HF emissions emissions rates at the consecutive hours over
period. inlet of the control which the sum of the
device. hourly HF mass
emissions rates at the
control device inlet
is greater than the
sum of the hourly HF
mass emissions rates
at the control device
inlet for any other
period of 3
consecutive hours
during the test run.
e. Determine the 2-run i. The hourly average (1) Calculate the HF
block average HF HF emissions rates at percentage reduction
percentage reduction the inlet and outlet for each hour of the 3-
for the emissions test. of the control device. hour peak HF emissions
period using Equation
2 of Sec.
63.9800(g)(2); and
(2) Calculate the
average HF percentage
reduction for each
test run as the
average of the hourly
HF percentage
reductions for the 3-
hour peak HF emissions
period for that run;
and
[[Page 121]]
(3) Calculate the 2-run
block average HF
percentage reduction
for the emission test
as the average of the
average HF percentage
reductions for the two
test runs.
f. Determine the 2-run i. The hourly average (1) Calculate the HCl
block average HCl HCl emissions rates at percentage reduction
percentage reduction the inlet and outlet for each hour of the 3-
for the emission test. of the control device. hour peak HF emissions
period using Equation
2 Sec.
63.9800(g)(2); and
(2) Calculate the
average HCl percentage
reduction for each
test run as the
average of the hourly
HCl percentage
reductions for the 3-
hour peak HF emissions
period for that run;
and
(3) Calculate the 2-run
block average HCl
percentage reduction
for the emission test
as the average of the
average HCl percentage
reductions for the two
test runs.
18. Each new kiln that is used to a. Establish the Data from the pressure (1) At least every 15
process clay refractory products operating limit for the drop measurement minutes, measure the
and is equipped with a DLA. minimum pressure drop device during the pressure drop across
across the DLA. performance test. the DLA; and
(2) Provide at least
one pressure drop
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average
pressure drop across
the DLA for each hour
of the performance
test; and
(4) Calculate and
record the minimum
pressure drop as the
average of the hourly
average pressure drops
across the DLA for the
two or three test
runs, whichever
applies.
b. Establish the Data from the limestone (1) Ensure that
operating limit for the feeder during the limestone in the feed
limestone feeder performance test. hopper, silo, and DLA
setting. is free-flowing at all
times during the
performance test; and
(2) Establish the
limestone feeder
setting 1 week prior
to the performance
test; and
(3) Record and maintain
the feeder setting for
the 1-week period that
precedes the
performance test and
during the performance
test.
19. Each new kiln that is used to a. Document conformance Data from the Submit analyses and
process clay refractory products with specifications and installation and supporting
and is equipped with a DIFF or DLS/ requirements of the bag calibration of the bag documentation
FF. leak detection system. leak detection system. demonstrating
conformance with EPA
guidance and
specifications for bag
leak detection systems
as part of the
Notification of
Compliance Status.
b. Establish the i. Data from the lime (1) For continuous lime
operating limit for the feeder during the injection systems,
lime feeder setting. performance test. ensure that lime in
the feed hopper or
silo is free-flowing
at all times during
the performance test;
and
(2) Record the feeder
setting for the three
test runs; and
(3) If the feed rate
setting varies during
the three test runs,
calculate and record
the average feed rate
for the two or three
test runs, whichever
applies.
[[Page 122]]
20. Each new kiln that is used to a. Establish the i. Data from the (1) At least every 15
process clay refractory products operating limit for the pressure drop minutes, measure the
and is equipped with a wet scrubber. minimum scrubber measurement device pressure drop across
pressure drop. during the performance the scrubber; and
test. (2) Provide at least
one pressure drop
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average
pressure drop across
the scrubber for each
hour of the
performance test; and
(4) Calculate and
record the minimum
pressure drop as the
average of the hourly
average pressure drops
across the scrubber
for the two or three
test runs, whichever
applies.
b. Establish the i. Data from the pH (1) At least every 15
operating limit for the measurement device minutes, measure
minimum scrubber liquid during the performance scrubber liquid pH;
pH. test. and
(2) Provide at least
one pH measurement
during at least three
15-minute periods per
hour of testing; and
(3) Calculate the
hourly average pH
values for each hour
of the performance
test; and
(4) Calculate and
record the minimum
liquid pH as the
average of the hourly
average pH
measurements for the
two or three test
runs, whichever
applies.
c. Establish the i. Data from the flow (1) At least every 15
operating limit for the rate measurement minutes, measure the
minimum scrubber liquid device during the scrubber liquid flow
flow rate. performance test. rate; and
(2) Provide at least
one flow rate
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average liquid
flow rate for each
hour of the
performance test; and
(4) Calculate and
record the minimum
liquid flow rate as
the average of the
hourly average liquid
flow rates for the two
or three test runs,
whichever applies.
d. If chemicals are i. Data from the (1) At least every 15
added to the scrubber chemical feed rate minutes, measure the
liquid, establish the measurement device scrubber chemical feed
operating limit for the during the performance rate; and
minimum scrubber test. (2) Provide at least
chemical feed rate. one chemical feed rate
measurement during at
least three 15-minute
periods per hour of
testing; and
(3) Calculate the
hourly average
chemical feed rate for
each hour of the
performance test; and
(4) Calculate and
record the minimum
chemical feed rate as
the average of the
hourly average
chemical feed rates
for the two or three
test runs, whichever
applies.
----------------------------------------------------------------------------------------------------------------
Table 5 to Subpart SSSSS of Part 63--Initial Compliance with Emission
Limits
As stated in Sec. 63.9806, you must show initial compliance with
the emission limits for affected sources according to the following
table:
[[Page 123]]
------------------------------------------------------------------------
You have
For . . . For the following demonstrated
emission limit . . . compliance if . . .
------------------------------------------------------------------------
1. Each affected source a. Each applicable i. Emissions
listed in Table 1 to this emission limit measured using the
subpart. listed in Table 1 test methods
to this subpart. specified in Table
4 to this subpart
satisfy the
applicable emission
limits specified in
Table 1 to this
subpart; and
ii. You establish
and have a record
of the operating
limits listed in
Table 2 to this
subpart over the
performance test
period; and
iii. You report the
results of the
performance test in
the Notification of
Compliance Status,
as specified by
Sec.
63.9812(e)(1) and
(2).
2. Each new or existing As specified in You have satisfied
curing oven, shape dryer, items 3 through 8 the applicable
and kiln that is used to of this table. requirements
process refractory products specified in items
that use organic HAP; each 3 through 8 of this
new or existing coking oven table.
and defumer that is used to
produce pitch-impregnated
refractory products; each
new shape preheater that is
used to produce pitch-
impregnated refractory
products; AND each new or
existing process unit that
is exhausted to a thermal
or catalytic oxidizer that
also controls emissions
from an affected shape
preheater or pitch working
tank.
3. Each affected continuous The average THC The 3-hour block
process unit that is concentration must average THC
subject to the THC emission not exceed 20 emission
concentration limit listed ppmvd, corrected to concentration
in item 2.a., 3.a., 4, or 5 18 percent oxygen. measured during the
of Table 1 to this subpart. performance test
using Methods 25A
and 3A is equal to
or less than 20
ppmvd, corrected to
18 percent oxygen.
4. Each affected continuous The average THC The 3-hour block
process unit that is percentage average THC
subject to the THC reduction must percentage
percentage reduction limit equal or exceed 95 reduction measured
listed in item 2.b. or 3.b. percent. during the
of Table 1 to this subpart. performance test
using Method 25A is
equal to or greater
than 95 percent.
5. Each affected batch The average THC The 2-run block
process unit that is concentration must average THC
subject to the THC emission not exceed 20 emission
concentration limit listed ppmvd, corrected to concentration for
in item 6.a., 7.a., 8, or 9 18 percent oxygen. the 3-hour peak
of Table 1 to this subpart. emissions period
measured during the
performance test
using Methods 25A
and 3A is equal to
or less than 20
ppmvd, corrected to
18 percent oxygen.
6. Each affected batch The average THC The 2-run block
process unit that is percentage average THC
subject to the THC reduction must percentage
percentage reduction limit equal or exceed 95 reduction for the 3-
listed in item 6.b. or 7.b. percent. hour peak emissions
of Table 1 to this subpart. period measured
during the
performance test
using Method 25A is
equal to or exceeds
95 percent.
7. Each affected continuous a. The average THC i. You have
or batch process unit that concentration must installed a THC
is equipped with a control not exceed 20 CEMS at the outlet
device other than a thermal ppmvd, corrected to of the control
or catalytic oxidizer and 18 percent oxygen; device or in the
is subject to the emission or stack of the
limit listed in item 3 or 7 affected source;
of Table 1 to this subpart. and
b. The average THC ii. You have
percentage satisfied the
reduction must requirements of PS-
equal or exceed 95 8 of 40 CFR part
percent. 60, appendix B.
8. Each affected continuous The average THC i. You have
or batch process unit that concentration must installed a THC
uses process changes to not exceed 20 CEMS at the outlet
reduce organic HAP ppmvd, corrected to of the control
emissions and is subject to 18 percent oxygen. device or in the
the emission limit listed stack of the
in item 4 or 8 of Table 1 affected source;
to this subpart. and
ii. You have
satisfied the
requirements of PS-
8 of 40 CFR part
60, appendix B.
9. Each new continuous kiln a. The average HF i. The 3-hour block
that is used to process emissions must not average production-
clay refractory products. exceed 0.019 kg/Mg based HF emissions
(0.038 lb/ton) of rate measured
uncalcined clay during the
processed; OR the performance test
average using one of the
uncontrolled HF methods specified
emissions must be in item 14.a.i. of
reduced by at least Table 4 to this
90 percent. subpart is equal to
or less than 0.019
kg/Mg (0.038 lb/
ton) of uncalcined
clay processed; or
ii. The 3-hour block
average HF
emissions reduction
measured during the
performance test is
equal to or greater
than 90 percent.
[[Page 124]]
b. The average HCl i. The 3-hour block
emissions must not average production-
exceed 0.091 kg/Mg based HCl emissions
(0.18 lb/ton) of rate measured
uncalcined clay during the
processed; OR the performance test
average using one of the
uncontrolled HCl methods specified
emissions must be in item 14.a.i. of
reduced by at least Table 4 to this
30 percent. subpart is equal to
or less than 0.091
kg/Mg (0.18 lb/ton)
of uncalcined clay
processed; or
ii. The 3-hour block
average HCl
emissions reduction
measured during the
performance test is
equal to or greater
than 30 percent.
10. Each new batch process a. The average The 2-run block
kiln that is used to uncontrolled HF average HF emission
process clay refractory emissions must be reduction measured
products. reduced by at least during the
90 percent. performance test is
equal to or greater
than 90 percent.
b. The average The 2-run block
uncontrolled HCl average HCl
emissions must be emissions reduction
reduced by at least measured during the
30 percent. performance test is
equal to or greater
than 30 percent.
------------------------------------------------------------------------
Table 6 to Subpart SSSSS of Part 63--Initial Compliance with Work
Practice Standards
As stated in Sec. 63.9806, you must show initial compliance with
the work practice standards for affected sources according to the
following table:
------------------------------------------------------------------------
You have
For each . . . For the following demonstrated initial
standard . . . compliance if . . .
------------------------------------------------------------------------
1. Each affected source a. Each applicable i. You have selected
listed in Table 3 to this work practice a method for
subpart. standard listed in performing each of
Table 3 to this the applicable work
subpart. practice standards
listed in Table 3
to this subpart;
and
ii. You have
included in your
Initial
Notification a
description of the
method selected for
complying with each
applicable work
practice standard,
as required by Sec.
63.9(b); and
iii. You submit a
signed statement
with the
Notification of
Compliance Status
that you have
implemented the
applicable work
practice standard
listed in Table 3
to this subpart;
and
iv. You have
described in your
OM&M plan the
method for
complying with each
applicable work
practice standard
specified in Table
3 to this subpart.
2. Each basket or container a. Control POM i. You have
that is used for holding emissions from any implemented at
fired refractory shapes in affected shape least one of the
an existing shape preheater preheater. work practice
and autoclave during the standards listed in
pitch impregnation process. item 1 of Table 3
to this subpart;
and
ii. You have
established a
system for
recording the date
and cleaning method
for each time you
clean an affected
basket or
container.
3. Each affected new or Control POM You have captured
existing pitch working tank. emissions. and vented
emissions from the
affected pitch
working tank to the
device that is used
to control
emissions from an
affected defumer or
coking oven, or to
a thermal or
catalytic oxidizer
that is comparable
to the control
device used on an
affected defumer or
coking oven.
4. Each new or existing Minimize fuel-based You use natural gas,
chromium refractory HAP emissions. or equivalent, as
products kiln. the kiln fuel.
5. Each existing clay Minimize fuel-based You use natural gas,
refractory products kiln. HAP emissions. or equivalent, as
the kiln fuel.
------------------------------------------------------------------------
[[Page 125]]
Table 7 to Subpart SSSSS of Part 63--Continuous Compliance with Emission
Limits
As stated in Sec. 63.9810, you must show continuous compliance with
the emission limits for affected sources according to the following
table:
------------------------------------------------------------------------
You must demonstrate
For the following continuous
For . . . emission limit . . . compliance by . . .
------------------------------------------------------------------------
1. Each affected source a. Each applicable i. Collecting and
listed in Table 1 to this emission limit recording the
subpart. listed in Table 1 monitoring and
to this subpart. process data listed
in Table 2
(operating limits)
to this subpart;
and
ii. Reducing the
monitoring and
process data
associated with the
operating limits
specified in Table
2 to this subpart;
and
iii. Recording the
results of any
control device
inspections; and
iv. Reporting, in
accordance with
Sec. 63.9814(e),
any deviation from
the applicable
operating limits
specified in Table
2 to this subpart.
2. Each new or existing As specified in Satisfying the
curing oven, shape dryer, items 3 though 7 of applicable
and kiln that is used to this table. requirements
process refractory products specified in items
that use organic HAP; each 3 through 7 of this
new or existing coking oven table.
and defumer that is used to
produce pitch-impregnated
refractory products; each
new shape preheater that is
used to produce pitch-
impregnated refractory
products; AND each new or
existing process unit that
is exhausted to a thermal
or catalytic oxidizer that
also controls emissions
from an affected shape
preheater or pitch working
tank.
3. Each affected process a. The average THC i. Collecting the
unit that is equipped with concentration must applicable data
a thermal or catalytic not exceed 20 measured by the
oxidizer. ppmvd, corrected to control device
18 percent oxygen; temperature
OR the average THC monitoring system,
percentage as specified in
reduction must items 5, 6, 8, and
equal or exceed 95 9 of Table 8 to
percent. this subpart; and
ii. Reducing the
applicable data
measured by the
control device
temperature
monitoring system,
as specified in
items 5, 6, 8, and
9 of Table 8 to
this subpart; and
iii. Maintaining the
average control
device operating
temperature for the
applicable
averaging period
specified in items
5, 6, 8, and 9 of
Table 2 to this
subpart at or above
the minimum
allowable operating
temperature
established during
the most recent
performance test.
4. Each affected process The average THC Operating and
unit that is equipped with concentration must maintaining a THC
a control device other than not exceed 20 CEMS at the outlet
a thermal or catalytic ppmvd, corrected to of the control
oxidizer. 18 percent oxygen; device or in the
OR the average THC stack of the
performance affected source,
reduction must according to the
equal or exceed 95 requirements of
percent. Procedure 1 of 40
CFR part 60,
appendix F.
5. Each affected process The average THC Operating and
unit that uses process concentration must maintaining a THC
changes to meet the not exceed 20 CEMS at the outlet
applicable emission limit. ppmvd, corrected to of the control
18 percent oxygen. device or in the
stack of the
affected source,
according to the
requirements of
Procedure 1 of 40
CFR part 60,
appendix F.
6. Each affected continuous The average THC Recording the
process unit. concentration must organic HAP
not exceed 20 processing rate
ppmvd, corrected to (pounds per hour)
18 percent oxygen; and the operating
OR the average THC temperature of the
percentage affected source, as
reduction must specified in items
equal or exceed 95 3.b. and 3.c. of
percent. Table 4 to this
subpart.
[[Page 126]]
7. Each affected batch The average THC Recording the
process unit. concentration must organic HAP
not exceed 20 processing rate
ppmvd, corrected to (pounds per batch);
18 percent oxygen; and process cycle
OR the average THC time for each batch
percentage cycle; and hourly
reduction must average operating
equal or exceed 95 temperature of the
percent. affected source, as
specified in items
8.b. through 8.d.
of Table 4 to this
subpart.
8. Each kiln that is used to As specified in Satisfying the
process clay refractory items 9 through 11 applicable
products. of this table. requirements
specified in items
9 through 11 of
this table.
9. Each affected kiln that a. The average HF i. Maintaining the
is equipped with a DLA. emissions must not pressure drop
exceed 0.019 kg/Mg across the DLA at
(0.038 lb/ton) of or above the
uncalcined clay minimum levels
processed, OR the established during
average the most recent
uncontrolled HF performance test;
emissions must be and
reduced by at least ii. Verifying that
90 percent; and the limestone
b. The average HCl hopper contains an
emissions must not adequate amount of
exceed 0.091 kg/Mg free-flowing
(0.18 lb/ton) of limestone by
uncalcined clay performing a daily
processed, or the visual check of the
average limestone in the
uncontrolled HCl feed hopper; and
emissions must be iii. Recording the
reduced by at least limestone feeder
30 percent. setting daily to
verify that the
feeder setting is
at or above the
level established
during the most
recent performance
test; and
iv. Using the same
grade of limestone
as was used during
the most recent
performance test
and maintaining
records of the
source and grade of
limestone.
10. Each affected kiln that a. The average HF i. Verifying at
is equipped with a DIFF or emissions must not least once each 8-
DLS/FF. exceed 0.019 kg/Mg hour shift that
(0.038 lb/ton) of lime is free-
uncalcined clay flowing by means of
processed; OR the a visual check,
average checking the output
uncontrolled HF of a load cell,
emissions must be carrier gas/lime
reduced by at least flow indicator, or
90 percent; and carrier gas
pressure drop
measurement system;
and
b. The average HCl ii. Recording feeder
emissions must not setting daily to
exceed 0.091 kg/Mg verify that the
(0.18 lb/ton) of feeder setting is
uncalcined clay at or above the
processed; OR the level established
average during the most
uncontrolled HCl recent performance
emissions must be test; and
reduced by at least
30 percent.
iii. Initiating
corrective action
within 1 hour of a
bag leak detection
system alarm AND
completing
corrective actions
in accordance with
the OM&M plan, AND
operating and
maintaining the
fabric filter such
that the alarm does
not engage for more
than 5 percent of
the total operating
time in a 6-month
block reporting
period.
11. Each affected kiln that a. The average HF i. Maintaining the
is equipped with a wet emissions must not pressure drop
scrubber. exceed 0.019 kg/Mg across the
(0.038 lb/ton) of scrubber, liquid
uncalcined clay pH, and liquid flow
processed; OR the rate at or above
average the minimum levels
uncontrolled HF established during
emissions must be the most recent
reduced by at least performance test;
90 percent; and and
b. The average HCl ii. If chemicals are
emissions must not added to the
exceed 0.091 kg/Mg scrubber liquid,
(0.18 lb/ton) of maintaining the
uncalcined clay average chemical
processed; OR the feed rate at or
average above the minimum
uncontrolled HCl chemical feed rate
emissions must be established during
reduced by at least the most recent
30 percent. performance test.
------------------------------------------------------------------------
Table 8 to Subpart SSSSS of Part 63--Continuous Compliance with
Operating Limits
As stated in Sec. 63.9810, you must show continuous compliance with
the operating limits for affected sources according to the following
table:
[[Page 127]]
------------------------------------------------------------------------
You must demonstrate
For the following continuous
For . . . operating limit . . compliance by . . .
.
------------------------------------------------------------------------
1. Each affected source a. Each applicable i. Maintaining all
listed in Table 2 to this operating limit applicable process
subpart. listed in Table 2 and control device
to this subpart. operating
parameters within
the limits
established during
the most recent
performance test;
and
ii. Conducting
annually an
inspection of all
duct work, vents,
and capture devices
to verify that no
leaks exist and
that the capture
device is operating
such that all
emissions are
properly vented to
the control device
in accordance with
the OM&M plan.
2. Each affected continuous a. The operating i. Operating the
kiln that is equipped with limits specified in control device on
a control device. items 2.a. through the affected kiln
2.c. of Table 2 to during all times
this subpart. except during
periods of approved
scheduled
maintenance, as
specified in Sec.
63.9792(e); and
ii. Minimizing HAP
emissions from the
affected kiln
during all periods
of scheduled
maintenance of the
kiln control device
when the kiln is
operating and the
control device is
out of service; and
iii. Minimizing the
duration of all
periods of
scheduled
maintenance of the
kiln control device
when the kiln is
operating and the
control device is
out of service.
3. Each new or existing As specified in Satisfying the
curing oven, shape dryer, items 4 through 9 applicable
and kiln that is used to of this table. requirements
process refractory products specified in items
that use organic HAP; each 4 through 9 of this
new or existing coking oven table.
and defumer that is used to
produce pitch-impregnated
refractory products; each
new shape preheater that is
used to produce pitch-
impregnated refractory
products; AND each new or
existing process unit that
is exhausted to a thermal
or catalytic oxidizer that
also controls emissions
from an affected shape
preheater or pitch working
tank.
4. Each affected continuous Maintain process i. Recording the
process unit. operating organic HAP
parameters within processing rate
the limits (pounds per hour);
established during and
the most recent ii. Recording the
performance test. operating
temperature of the
affected source at
least hourly; and
iii. Maintaining the
3-hour block
average organic HAP
processing rate at
or below the
maximum organic HAP
processing rate
established during
the most recent
performance test.
5. Continuous process units Maintain the 3-hour i. Measuring and
that are equipped with a block average recording the
thermal oxidizer. operating thermal oxidizer
temperature in the combustion chamber
thermal oxidizer temperature at
combustion chamber least every 15
at or above the minutes; and
minimum allowable ii. Calculating the
operating hourly average
temperature thermal oxidizer
established during combustion chamber
the most recent temperature; and
performance test. iii. Maintaining the
3-hour block
average thermal
oxidizer combustion
chamber temperature
at or above the
minimum allowable
operating
temperature
established during
the most recent
performance test;
and
iv. Reporting, in
accordance with
Sec. 63.9814(e),
any 3-hour block
average operating
temperature
measurements below
the minimum
allowable thermal
oxidizer combustion
chamber operating
temperature
established during
the most recent
performance test.
[[Page 128]]
6. Continuous process units a. Maintain the 3- i. Measuring and
that are equipped with a hour block average recording the
catalytic oxidizer. temperature at the temperature at the
inlet of the inlet of the
catalyst bed at or catalyst bed at
above the minimum least every 15
allowable catalyst minutes; and
bed inlet ii. Calculating the
temperature hourly average
established during temperature at the
the most recent inlet of the
performance test. catalyst bed; and
iii. Maintaining the
3-hour block
average temperature
at the inlet of the
catalyst bed at or
above the minimum
allowable catalyst
bed inlet
temperature
established during
the most recent
performance test;
and
iv. Reporting, in
accordance with
Sec. 63.9814(e),
any 3-hour block
average catalyst
bed inlet
temperature
measurements below
the minimum
allowable catalyst
bed inlet
temperature
established during
the most recent
performance; and
v. Checking the
activity level of
the catalyst at
least every 12
months and taking
any necessary
corrective action,
such as replacing
the catalyst, to
ensure that the
catalyst is
performing as
designed.
7. Each affected batch Maintain process i. Recording the
process unit. operating organic HAP
parameters within processing rate
the limits (pounds per batch);
established during and
the most recent ii. Recording the
performance test. hourly average
operating
temperature of the
affected source;
and
iii. Recording the
process cycle time
for each batch
cycle; and
iv. Maintaining the
organic HAP
processing rate at
or below the
maximum organic HAP
processing rate
established during
the most recent
performance test.
8. Batch process units that Maintain the hourly i. Measuring and
are equipped with a thermal average temperature recording the
oxidizer. in the thermal thermal oxidizer
oxidizer combustion combustion chamber
chamber at or above temperature at
the hourly average least every 15
temperature minutes; and
established for the ii. Calculating the
corresponding 1- hourly average
hour period of the thermal oxidizer
cycle during the combustion chamber
most recent temperature; and
performance test. iii. From the start
of each batch cycle
until 3 hours have
passed since the
process unit
reached maximum
temperature,
maintaining the
hourly average
operating
temperature in the
thermal oxidizer
combustion chamber
at or above the
minimum allowable
operating
temperature
established for the
corresponding
period during the
most recent
performance test,
as determined
according to item
11 of Table 4 to
this subpart; and
iv. For each
subsequent hour of
the batch cycle,
maintaining the
hourly average
operating
temperature in the
thermal oxidizer
combustion chamber
at or above the
minimum allowable
operating
temperature
established for the
corresponding hour
during the most
recent performance
test, as specified
in item 13 of Table
4 to this subpart;
and
v. Reporting, in
accordance with
Sec. 63.9814(e),
any temperature
measurements below
the minimum
allowable thermal
oxidizer combustion
chamber temperature
measured during the
most recent
performance test.
[[Page 129]]
9. Batch process units that Maintain the hourly i. Measuring and
are equipped with a average temperature recording
catalytic oxidizer. at the inlet of the temperatures at the
catalyst bed at or inlet of the
above the catalyst bed at
corresponding least every 15
hourly average minutes; and
temperature ii. Calculating the
established for the hourly average
corresponding 1- temperature at the
hour period of the inlet of the
cycle during the catalyst bed; and
most recent iii. From the start
performance test. of each batch cycle
until 3 hours have
passed since the
process unit
reached maximum
temperature,
maintaining the
hourly average
operating
temperature at the
inlet of the
catalyst bed at or
above the minimum
allowable bed inlet
temperature
established for the
corresponding
period during the
most recent
performance test,
as determined
according to item
12 of Table 4 to
this subpart; and
iv. For each
subsequent hour of
the batch cycle,
maintaining the
hourly average
operating
temperature at the
inlet of the
catalyst bed at or
above the minimum
allowable bed inlet
temperature
established for the
corresponding hour
during the most
recent performance
test, as specified
in item 13 of Table
4 to this subpart;
and
v. Reporting, in
accordance with
Sec. 63.9814(e),
any catalyst bed
inlet temperature
measurements below
the minimum
allowable bed inlet
temperature
measured during the
most recent
performance test;
and
vi. Checking the
activity level of
the catalyst at
least every 12
months and taking
any necessary
corrective action,
such as replacing
the catalyst, to
ensure that the
catalyst is
performing as
designed.
10. Each new kiln that is As specified in Satisfying the
used to process clay items 11 through 13 applicable
refractory products. of this table. requirements
specified in items
11 through 13 of
this table.
11. Each new kiln that is a. Maintain the i. Collecting the
equipped a DLA. average pressure DLA pressure drop
drop across the DLA data, as specified
for each 3-hour in item 18.a. of
block period at or Table 4 to this
above the minimum subpart; and
pressure drop ii. Reducing the DLA
established during pressure drop data
the most recent to 1-hour and 3-
performance test. hour block
averages; and
iii. Maintaining the
3-hour block
average pressure
drop across the DLA
at or above the
minimum pressure
drop established
during the most
recent performance
test.
b. Maintain free- Verifying that the
flowing limestone limestone hopper
in the feed hopper, has an adequate
silo, and DLA. amount of free-
flowing limestone
by performing a
daily visual check
of the limestone
hopper.
c. Maintain the Recording the
limestone feeder limestone feeder
setting at or above setting at least
the level daily to verify
established during that the feeder
the most recent setting is being
performance test. maintained at or
above the level
established during
the most recent
performance test.
d. Use the same Using the same grade
grade of limestone of limestone as was
from the same used during the
source as was used most recent
during the most performance test
recent performance and maintaining
test. records of the
source and grade of
limestone.
[[Page 130]]
12. Each new kiln that is a. Initiate i. Initiating
equipped with a DIFF or DLS/ corrective action corrective action
FF. within 1 hour of a within 1 hour of a
bag leak detection bag leak detection
system alarm and system alarm and
complete corrective completing
actions in corrective actions
accordance with the in accordance with
OM&M plan; AND the OM&M plan; and
operate and ii. Operating and
maintain the fabric maintaining the
filter such that fabric filter such
the alarm does not that the alarm does
engage for more not engage for more
than 5 percent of than 5 percent of
the total operating the total operating
time in a 6-month time in a 6-month
block reporting block reporting
period. period; in
calculating this
operating time
fraction, if
inspection of the
fabric filter
demonstrates that
no corrective
action is required,
no alarm time is
counted; if
corrective action
is required, each
alarm shall be
counted as a
minimum of 1 hour;
if you take longer
than 1 hour to
initiate corrective
action, the alarm
time shall be
counted as the
actual amount of
time taken by you
to initiate
corrective action.
b. Maintain free- i. Verifying at
flowing lime in the least once each 8-
feed hopper or silo hour shift that
at all times for lime is free-
continuous flowing via a load
injection systems; cell, carrier gas/
AND maintain feeder lime flow
setting at or above indicator, carrier
the level gas pressure drop
established during measurement system,
the most recent or other system;
performance test recording all
for continuous monitor or sensor
injection systems. output, and if lime
is found not to be
free flowing,
promptly initiating
and completing
corrective actions;
and
ii. Recording the
feeder setting once
each day of
operation to verify
that the feeder
setting is being
maintained at or
above the level
established during
the most recent
performance test.
13. Each new kiln that is a. Maintain the i. Collecting the
used to process clay average pressure scrubber pressure
refractory products and is drop across the drop data, as
equipped with a wet scrubber for each 3- specified in item
scrubber. hour block period 20.a. of Table 4 to
at or above the this subpart; and
minimum pressure ii. Reducing the
drop established scrubber pressure
during the most drop data to 1-hour
recent performance and 3-hour block
test. averages; and
iii. Maintaining the
3-hour block
average scrubber
pressure drop at or
above the minimum
pressure drop
established during
the most recent
performance test.
b. Maintain the i. Collecting the
average scrubber scrubber liquid pH
liquid pH for each data, as specified
3-hour block period in item 20.b. of
at or above the Table 4 to this
minimum scrubber subpart; and
liquid pH ii. Reducing the
established during scrubber liquid pH
the most recent data to 1-hour and
performance test. 3-hour block
averages; and
iii. Maintaining the
3-hour block
average scrubber
liquid pH at or
above the minimum
scrubber liquid pH
established during
the most recent
performance test.
c. Maintain the i. Collecting the
average scrubber scrubber liquid
liquid flow rate flow rate data, as
for each 3-hour specified in item
block period at or 20.c. of Table 4 to
above the minimum this subpart; and
scrubber liquid ii. Reducing the
flow rate scrubber liquid
established during flow rate data to 1-
the most recent hour and 3-hour
performance test. block averages; and
iii. Maintaining the
3-hour block
average scrubber
liquid flow rate at
or above the
minimum scrubber
liquid flow rate
established during
the most recent
performance test.
d. If chemicals are i. Collecting the
added to the scrubber chemical
scrubber liquid, feed rate data, as
maintain the specified in item
average scrubber 20.d. of Table 4 to
chemical feed rate this subpart; and
for each 3-hour ii. Reducing the
block period at or scrubber chemical
above the minimum feed rate data to 1-
scrubber chemical hour and 3-hour
feed rate block averages; and
established during
the most recent
performance test.
[[Page 131]]
iii. Maintaining the
3-hour block
average scrubber
chemical feed rate
at or above the
minimum scrubber
chemical feed rate
established during
the most recent
performance test.
------------------------------------------------------------------------
Table 9 to Subpart SSSSS of Part 63--Continuous Compliance with Work
Practice Standards
As stated in Sec. 63.9810, you must show continuous compliance with
the work practice standards for affected sources according to the
following table:
------------------------------------------------------------------------
You must demonstrate
For the following continuous
For . . . work practice compliance by . . .
standard . . .
------------------------------------------------------------------------
1. Each affected source Each applicable work i. Performing each
listed in Table 3 to this practice applicable work
subpart. requirement listed practice standard
in Table 3 to this listed in Table 3
subpart. to this subpart;
and
ii. Maintaining
records that
document the method
and frequency for
complying with each
applicable work
practice standard
listed in Table 3
to this subpart, as
required by Sec.
Sec. 63.10(b) and
63.9816(c)(2).
2. Each basket or container Control POM i. Controlling
that is used for holding emissions from any emissions from the
fired refractory shapes in affected shape volatilization of
an existing shape preheater preheater. residual pitch by
and autoclave during the implementing one of
pitch impregnation process. the work practice
standards listed in
item 1 of Table 3
to this subpart;
and
ii. Recording the
date and cleaning
method each time
you clean an
affected basket or
container.
3. Each new or existing Control POM Capturing and
pitch working tank. emissions. venting emissions
from the affected
pitch working tank
to the control
device that is used
to control
emissions from an
affected defumer or
coking oven, or to
a thermal or
catalytic oxidizer
that is comparable
to the control
device used on an
affected defumer or
coking oven.
4. Each new or existing Minimize fuel-based i. Using natural
chromium refractory HAP emissions. gas, or equivalent,
products kiln. as the kiln fuel at
all times except
during periods of
natural gas
curtailment or
supply
interruption; and
ii. If you intend to
use an alternative
fuel, submitting a
notification of
alternative fuel
use within 48 hours
of the declaration
of a per-iod of
natural gas
curtailment or
supply
interruption, as
defined in Sec.
63.9824; and
iii. Submitting a
report of
alternative fuel
use within 10
working days after
terminating the use
of the alternative
fuel, as specified
in Sec.
63.9814(g).
5. Each existing clay Minimize fuel-based i. Using natural
refractory products kiln. HAP emissions. gas, or equivalent,
as the kiln fuel at
all times except
during periods of
natural gas
curtailment or
supply
interruption; and
ii. If you intend to
use an alternative
fuel, submitting a
notification of
alternative fuel
use within 48 hours
of the declaration
of a per-iod of
natural gas
curtailment or
supply
interruption, as
defined in Sec.
63.9824; and
iii. Submitting a
report of
alternative fuel
use within 10
working days after
terminating the use
of the alternative
fuel, as specified
in Sec.
63.9814(g).
------------------------------------------------------------------------
[[Page 132]]
Table 10 to Subpart SSSSS of Part 63--Requirements for Reports
As stated in Sec. 63.9814, you must comply with the requirements
for reports in the following table:
------------------------------------------------------------------------
The report must You must submit the
You must submit a(n) . . . contain . . . report . . .
------------------------------------------------------------------------
1. Compliance report........ The information in Semiannually
Sec. 63.9814(c) according to the
through (f). requirements in
Sec. 63.9814(a)
through (f).
2. Immediate startup, a. Actions taken for By fax or telephone
shutdown, and malfunction the event. within 2 working
report if you had a days after starting
startup, shutdown, or actions
malfunction during the inconsistent with
reporting period that is the plan.
not consistent with your
SSMP.
b. The information By letter within 7
in Sec. working days after
63.10(d)(5)(ii). the end of the
event unless you
have made
alternative
arrangements with
the permitting
authority.
3. Report of alternative The information in If you are subject
fuel use. Sec. 63.9814(g) to the work
and items 4 and 5 practice standard
of Table 9 to this specified in item 3
subpart. or 4 of Table 3 to
this subpart, and
you use an
alternative fuel in
the affected kiln,
by letter within 10
working days after
terminating the use
of the alternative
fuel.
------------------------------------------------------------------------
Table 11 to Subpart SSSSS of Part 63--Applicability of General
Provisions to Subpart SSSSS
As stated in Sec. 63.9820, you must comply with the applicable
General Provisions requirements according to the following table:
----------------------------------------------------------------------------------------------------------------
Applies to subpart
Citation Subject Brief description SSSSS
----------------------------------------------------------------------------------------------------------------
Sec. 63.1....................... Applicability............. .......................... Yes.
Sec. 63.2....................... Definitions............... .......................... Yes.
Sec. 63.3....................... Units and Abbreviations... .......................... Yes.
Sec. 63.4....................... Prohibited Activities..... Compliance date; Yes.
circumvention,
severability.
Sec. 63.5....................... Construction/ Applicability; Yes.
Reconstruction. applications; approvals.
Sec. 63.6(a).................... Applicability............. General Provisions (GP) Yes.
apply unless compliance
extension; GP apply to
area sources that become
major.
Sec. 63.6(b)(1)-(4)............. Compliance Dates for New Standards apply at Yes.
and Reconstructed Sources. effective date; 3 years
after effective date;
upon startup; 10 years
after construction or
reconstruction commences
for section 112(f).
Sec. 63.6(b)(5)................. Notification.............. .......................... Yes.
Sec. 63.6(b)(6)................. [Reserved] ....................
Sec. 63.6(b)(7)................. Compliance Dates for New Area sources that become Yes.
and Reconstructed Area major must comply with
Sources That Become Major. major source standards
immediately upon becoming
major, regardless of
whether required to
comply when they were
area sources.
Sec. 63.6(c)(1)-(2)............. Compliance Dates for Comply according to date Yes.
Existing Sources. in subpart, which must be
no later than 3 years
after effective date; for
section 112(f) standards,
comply within 90 days of
effective date unless
compliance extension.
Sec. 63.6(c)(3)-(4)............. [Reserved] ....................
Sec. 63.6(c)(5)................. Compliance Dates for Area sources that become Yes.
Existing Area Sources major must comply with
That Become Major. major source standards by
date indicated in subpart
or by equivalent time
period (for example, 3
years).
Sec. 63.6(d).................... [Reserved] ....................
Sec. 63.6(e)(1)-(2)............. Operation & Maintenance... Operate to minimize Yes.
emissions at all times;
correct malfunctions as
soon as practicable;
requirements
independently
enforceable; information
Administrator will use to
determine if operation
and maintenance
requirements were met.
[[Page 133]]
Sec. 63.6(e)(3)................. Startup, Shutdown, and .......................... Yes.
Malfunction Plan (SSMP).
Sec. 63.6(f)(1)................. Compliance Except During You must comply with Yes.
SSM. emission standards at all
times except during SSM.
Sec. 63.6(f)(2)-(3)............. Methods for Determining Compliance based on Yes.
Compliance. performance test,
operation and maintenance
plans, records,
inspection.
Sec. 63.6(g)(1)-(3)............. Alternative Standard...... Procedures for getting an Yes.
alternative standard.
Sec. 63.6(h)(1)-(9)............. Opacity/Visible Emission .......................... Not applicable.
(VE) Standards.
Sec. 63.6(i)(1)-(14)............ Compliance Extension...... Procedures and criteria Yes.
for Administrator to
grant compliance
extension.
Sec. 63.6(j).................... Presidential Compliance President may exempt Yes.
Exemption. source category.
Sec. 63.7(a)(1)-(2)............. Performance Test Dates.... Dates for conducting Yes.
initial performance
testing and other
compliance
demonstrations; must
conduct 180 days after
first subject to rule.
Sec. 63.7(a)(3)................. Section 114 Authority..... Administrator may require Yes.
a performance test under
CAA section 114 at any
time.
Sec. 63.7(b)(1)................. Notification of Must notify Administrator Yes.
Performance Test. 60 days before the test.
Sec. 63.7(b)(2)................. Notification of Must notify Administrator Yes.
Rescheduling. 5 days before scheduled
date and provide
rescheduled date.
Sec. 63.7(c).................... Quality Assurance/Test Requirements; test plan Yes.
Plan. approval procedures;
performance audit
requirements; internal
and external QA
procedures for testing.
Sec. 63.7(d).................... Testing Facilities........ .......................... Yes.
Sec. 63.7(e)(1)................. Conditions for Conducting Performance tests must be No, Sec. 63.9800
Performance Tests. conducted under specifies
representative requirements; Yes;
conditions; cannot Yes.
conduct performance tests
during SSM; not a
violation to exceed
standard during SSM.
Sec. 63.7(e)(2)................. Conditions for Conducting Must conduct according to Yes.
Performance Tests. subpart and EPA test
methods unless
Administrator approves
alternative.
Sec. 63.7(e)(3)................. Test Run Duration......... Must have three test runs Yes; Yes, except
of at least 1 hour each; where specified in
compliance is based on Sec. 63.9800 for
arithmetic mean of three batch process
runs; conditions when sources; Yes.
data from an additional
test run can be used.
Sec. 63.7(f).................... Alternative Test Method... .......................... Yes.
Sec. 63.7(g).................... Performance Test Data .......................... Yes.
Analysis.
Sec. 63.7(h).................... Waiver of Test............ .......................... Yes.
Sec. 63.8(a)(1)................. Applicability of .......................... Yes.
Monitoring Requirements.
Sec. 63.8(a)(2)................. Performance Specifications Performance Specifications Yes.
in appendix B of 40 CFR
part 60 apply.
Sec. 63.8(a)(3)................. [Reserved]
Sec. 63.8(a)(4)................. Monitoring with Flares.... .......................... Not applicable.
Sec. 63.8(b)(1)................. Monitoring................ Must conduct monitoring Yes.
according to standard
unless Administrator
approves alternative.
Sec. 63.8(b)(2)-(3)............. Multiple Effluents and Specific requirements for Yes.
Multiple Monitoring installing and reporting
Systems. on monitoring systems.
Sec. 63.8(c)(1)................. Monitoring System Maintenance consistent Yes.
Operation and Maintenance. with good air pollution
control practices.
Sec. 63.8(c)(1)(i).............. Routine and Predictable Reporting requirements for Yes.
SSM. SSM when action is
described in SSMP.
Sec. 63.8(c)(1)(ii)............. SSM not in SSMP........... Reporting requirements for Yes.
SSM when action is not
described in SSMP.
Sec. 63.8(c)(1)(iii)............ Compliance with Operation How Administrator Yes.
and Maintenance determines if source is
Requirements. complying with operation
and maintenance
requirements.
Sec. 63.8(c)(2)-(3)............. Monitoring System Must install to get Yes.
Installation. representative emission
and parameter
measurements.
Sec. 63.8(c)(4)................. CMS Requirements.......... .......................... No, Sec. 63.9808
specifies
requirements.
Sec. 63.8(c)(5)................. COMS Minimum Procedures... .......................... Not applicable.
Sec. 63.8(c)(6)................. CMS Requirements.......... .......................... Applies only to
sources required to
install and operate
a THC CEMS.
[[Page 134]]
Sec. 63.8(c)(7)(i)(A)........... CMS Requirements.......... .......................... Applies only to
sources required to
install and operate
a THC CEMS.
Sec. 63.8(c)(7)(i)(B)........... CMS Requirements.......... .......................... Applies only to
sources required to
install and operate
a THC CEMS.
Sec. 63.8(c)(7)(i)(C)........... CMS Requirements.......... .......................... Not applicable.
Sec. 63.8(c)(7)(ii)............. CMS Requirements.......... Corrective action required Yes.
when CMS is out of
control.
Sec. 63.8(c)(8)................. CMS Requirements.......... .......................... Yes.
Sec. 63.8(d).................... CMS Quality Control....... .......................... Applies only to
sources required to
install and operate
a THC CEMS.
Sec. 63.8(e).................... CMS Performance Evaluation .......................... Applies only to
sources required to
install and operate
a THC CEMS.
Sec. 63.8(f)(1)-(5)............. Alternative Monitoring .......................... Yes.
Method.
Sec. 63.8(f)(6)................. Alternative to Relative .......................... Yes.
Accuracy Test.
Sec. 63.8(g).................... Data Reduction............ .......................... Applies only to
sources required to
install and operate
a THC CEMS.
Sec. 63.9(a).................... Notification Requirements. .......................... Yes.
Sec. 63.9(b)(1)-(5)............. Initial Notifications..... .......................... Yes.
Sec. 63.9(c).................... Request for Compliance .......................... Yes.
Extension.
Sec. 63.9(d).................... Notification of Special .......................... Yes.
Compliance Requirements
for New Source.
Sec. 63.9(e).................... Notification of Notify Administrator 60 Yes.
Performance Test. days prior.
Sec. 63.9(f).................... Notification of VE/Opacity .......................... Not applicable.
Test.
Sec. 63.9(g).................... Additional Notifications .......................... Applies only to
When Using CMS. sources required to
install and operate
a THC CEMS.
Sec. 63.9(h).................... Notification of Compliance .......................... Yes.
Status.
Sec. 63.9(i).................... Adjustment of Submittal .......................... Yes.
Deadlines.
Sec. 63.9(j).................... Change in Previous .......................... Yes.
Information.
Sec. 63.10(a)................... Recordkeeping/Reporting... .......................... Yes.
Sec. 63.10(b)(1)................ Recordkeeping/Reporting... .......................... Yes.
Sec. 63.10(b)(2)(i)-(v)......... Records Related to .......................... Yes.
Startup, Shutdown, and
Malfunction.
Sec. 63.10(b)(2)(vi) and (x-xi). CMS Records............... .......................... Yes.
Sec. 63.10(b)(2)(vii)-(ix)...... Records................... Measurements to Yes.
demonstrate compliance
with emission
limitations; performance
test, performance
evaluation, and visible
emission observation
results; measurements to
determine conditions of
performance tests and
performance evaluations.
Sec. 63.10(b)(2)(xii)........... Records................... Records when under waiver. Yes.
Sec. 63.10(b)(2)(xiii).......... Records................... Records when using Not applicable.
alternative to relative
accuracy test.
Sec. 63.10(b)(2)(xiv)........... Records................... All documentation Yes.
supporting Initial
Notification and
Notification of
Compliance Status.
Sec. 63.10(b)(3)................ Records................... Applicability Yes.
Determinations.
Sec. 63.10(c)(1)-(6), (9)-(15).. Records................... Additional Records for CMS Not applicable.
Sec. 63.10(c)(7)-(8)............ Records................... Records of excess No, Sec. 63.9816
emissions and parameter specifies
monitoring exceedances requirements.
for CMS.
Sec. 63.10(d)(1)................ General Reporting Requirements for reporting Yes.
Requirements.
Sec. 63.10(d)(2)................ Report of Performance Test When to submit to Federal Yes.
Results. or State authority.
Sec. 63.10(d)(3)................ Reporting Opacity or VE .......................... Not applicable.
Observations.
Sec. 63.10(d)(4)................ Progress Reports.......... Must submit progress Yes.
reports on schedule if
under compliance
extension.
Sec. 63.10(d)(5)................ Startup, Shutdown, and Contents and submission... Yes.
Malfunction Reports.
[[Page 135]]
Sec. 63.10(e)(1)-(2)............ Additional CMS Reports.... .......................... Applies only to
sources required to
install and operate
a THC CEMS.
Sec. 63.10(e)(3)................ Reports................... .......................... No, Sec. 63.9814
specifies
requirements.
Sec. 63.10(e)(4)................ Reporting COMS data....... .......................... Not applicable.
Sec. 63.10(f)................... Waiver for Recordkeeping/ .......................... Yes.
Reporting.
Sec. 63.11...................... Flares.................... .......................... Not applicable.
Sec. 63.12...................... Delegation................ .......................... Yes.
Sec. 63.13...................... Addresses................. .......................... Yes.
Sec. 63.14...................... Incorporation by Reference .......................... Yes.
Sec. 63.15...................... Availability of .......................... Yes.
Information.
----------------------------------------------------------------------------------------------------------------
Subpart TTTTT_National Emissions Standards for Hazardous Air Pollutants
for Primary Magnesium Refining
Source: 68 FR 58620, Oct. 10, 2003, unless otherwise noted.
What This Subpart Covers
Sec. 63.9880 What is the purpose of this subpart?
This subpart establishes national emission standards for hazardous
air pollutants (NESHAP) for primary magnesium refineries. This subpart
also establishes requirements to demonstrate initial and continuous
compliance with all applicable emission limitations, work practice
standards, and operation and maintenance requirements.
Sec. 63.9881 Am I subject to this subpart?
You are subject to this subpart if you own or operate a primary
magnesium refinery that is (or is part of) a major source of hazardous
air pollutant (HAP) emissions. Your primary magnesium refinery is a
major source of HAP if it emits or has the potential to emit any single
HAP at a rate of 10 tons or more per year or any combination of HAP at a
rate of 25 tons or more per year.
Sec. 63.9882 What parts of my plant does this subpart cover?
(a) The affected sources are each new and existing primary magnesium
refining facility.
(b) This subpart covers emissions from each spray dryer stack,
magnesium chloride storage bins scrubber stack, melt/reactor system
stack, and launder off-gas system stack at your primary magnesium
refining facility. This subpart also covers fugitive dust emissions.
(c) Each primary magnesium refining facility is existing if you
commenced construction or reconstruction of the affected source before
January 22, 2003.
(d) Each primary magnesium refining facility is new if you commence
construction or reconstruction of the affected source on or after
January 22, 2003. An affected source is reconstructed if it meets the
definition of reconstruction in Sec. 63.2.
Sec. 63.9883 When do I have to comply with this subpart?
(a) If you have an existing source, you must comply with each
emission limitation, work practice standard, and operation and
maintenance requirement in this subpart that applies to you no later
than October 11, 2004.
(b) If you have a new affected source and its initial startup date
is on or before October 11, 2003, you must comply with each emission
limitation, work practice standard, and operation and maintenance
requirement in this subpart that applies to you by October 10, 2003.
(c) If you have a new affected source and its initial startup date
is after October 10, 2003, you must comply with each emission
limitation, work practice standard, and operation and maintenance
requirement in this subpart that applies to you upon initial startup.
(d) If your primary magnesium refinery is an area source that
becomes a major source of HAP, the compliance
[[Page 136]]
dates in paragraphs (d)(1) and (2) of this section apply to you:
(1) Any portion of the existing primary magnesium refinery that is a
new affected source or a new reconstructed source must be in compliance
with this subpart upon startup.
(2) All other parts of the primary magnesium refinery must be in
compliance with this subpart no later than 2 years after it becomes a
major source.
(e) You must meet the notification and schedule requirements in
Sec. 63.9930. Several of these notifications must be submitted before
the compliance date for your affected source.
Emission Limitations and Work Practice Standards
Sec. 63.9890 What emission limitations must I meet?
(a) You must meet each emission limit in Table 1 to this subpart
that applies to you.
(b) For each wet scrubber applied to meet any particulate matter,
particulate matter less than 10 microns (PM10), chlorine,
hydrochloric acid, or dioxins/furans emission limit in Table 1 to this
subpart, you must maintain the hourly average pressure drop and scrubber
liquid flow rate at or above the minimum level established during the
initial or subsequent performance test.
Sec. 63.9891 What work practice standards must I meet for my fugitive
dust sources?
(a) You must prepare and at all times operate according to a
fugitive dust emissions control plan that describes in detail the
measures that will be put in place to control fugitive dust emissions
from all unpaved roads and other unpaved operational areas.
(b) You must submit a copy of your fugitive dust emissions control
plan for approval to the Administrator on or before the applicable
compliance date for the affected source as specified in Sec. 63.9883.
The requirement to operate according to the fugitive dust emissions
control plan must be incorporated by reference in the source's operating
permit issued by the permitting authority under 40 CFR part 70 or 40 CFR
part 71.
(c) You can use an existing fugitive dust emissions control plan
provided it meets the requirements in paragraphs (c)(1) through (3) of
this section.
(1) The plan satisfies the requirements of paragraph (a) of this
section.
(2) The plan describes the current measures to control fugitive dust
emission sources.
(3) The plan has been approved as part of a State implementation
plan or title V permit.
(d) You must maintain a current copy of the fugitive dust emissions
control plan on-site and available for inspection upon request. You must
keep the plan for the life of the affected source or until the affected
source is no longer subject to the requirements of this subpart.
Operation and Maintenance Requirements
Sec. 63.9900 What are my operation and maintenance requirements?
(a) As required by Sec. 63.6(e)(1)(i), you must always operate and
maintain your affected source, including air pollution control and
monitoring equipment, in a manner consistent with good air pollution
control practices for minimizing emissions at least to the levels
required by this subpart.
(b) You must prepare and operate at all times according to a written
operation and maintenance plan for each control device subject to an
operating limit in Sec. 63.9890(b). Each plan must address preventative
maintenance for each control device, including a preventative
maintenance schedule that is consistent with the manufacturer's
instructions for routine and long-term maintenance.
(c) You must maintain a current copy of the operation and
maintenance plan required in paragraph (b) of this section on-site and
available for inspection upon request. You must keep the plan for the
life of the affected source or until the affected source is no longer
subject to the requirements of this subpart.
[[Page 137]]
General Compliance Requirements
Sec. 63.9910 What are my general requirements for complying with this
subpart?
(a) You must be in compliance with the emission limitations, work
practice standards, and operation and maintenance requirements in this
subpart at all times, except during periods of startup, shutdown, and
malfunction as defined in Sec. 63.2.
(b) You must develop a written startup, shutdown, and malfunction
plan according to the provisions in Sec. 63.6(e)(3).
[68 FR 58620, Oct. 10, 2003, as amended at 71 FR 20471, Apr. 20, 2006]
Initial Compliance Requirements
Sec. 63.9911 By what date must I conduct performance tests or other
initial compliance demonstrations?
(a) As required in Sec. 63.7(a)(2), you must conduct a performance
test to demonstrate initial compliance with each emission limit in Table
1 to this subpart that applies to you as indicated in paragraphs (a)(1)
through (3) of this section:
(1) Within 180 calendar days after the compliance date that is
specified in Sec. 63.9883 for your existing affected source;
(2) By April 7, 2004 for a new source that has an initial startup
date before October 10, 2003; or
(3) Within 180 days after initial startup for a new source that has
an initial startup date after October 10, 2003.
(b) For each operation and maintenance requirement that applies to
you where initial compliance is not demonstrated using a performance
test, you must demonstrate initial compliance within 30 calendar days
after the compliance date that is specified for your affected source in
Sec. 63.9883.
(c) If you commenced construction or reconstruction between January
22, 2003 and October 10, 2003, you must demonstrate initial compliance
with either the proposed emission limitation or the promulgated emission
limitation no later than April 7, 2004 or no later than 180 calendar
days after startup of the source, whichever is later, according to Sec.
63.7(a)(2)(ix).
(d) If you commenced construction or reconstruction between January
22, 2003 and October 10, 2003, and you chose to comply with the proposed
emission limit when demonstrating initial compliance, you must conduct a
second performance test to demonstrate compliance with the promulgated
emission limit by April 11, 2005, or after startup of the source,
whichever is later, according to Sec. 63.7(a)(2)(ix).
Sec. 63.9912 When must I conduct subsequent performance tests?
You must conduct subsequent performance tests to demonstrate
continuous compliance with all applicable emission limits in Table 1 to
this subpart no less frequently than twice (at mid-term and renewal)
during each term of your title V operating permit.
Sec. 63.9913 What test methods and other procedures must I use to
demonstrate initial compliance with the emission limits for particulate
matter and PM[bdi1][bdi0]?
(a) You must conduct each performance test that applies to your
affected source according to the requirements in Sec. 63.7(e)(1).
(b) To determine compliance with the applicable emission limits for
particulate matter in Table 1 to this subpart, you must follow the test
methods and procedures in paragraphs (b)(1) and (2) of this section.
(1) Determine the concentration of particulate matter according to
the following test methods in appendix A to 40 CFR part 60:
(i) Method 1 to select sampling port locations and the number of
traverse points. Sampling ports must be located at the outlet of the
control device and prior to any releases to the atmosphere.
(ii) Method 2, 2F, or 2G to determine the volumetric flow rate of
the stack gas.
(iii) Method 3, 3A, or 3B to determine the dry molecular weight of
the stack gas.
(iv) Method 4 to determine the moisture content of the stack gas.
(v) Method 5 or 5D, as applicable, to determine the concentration of
particulate matter.
[[Page 138]]
(vi) Method 201 or 201A, as applicable, to determine the
concentration of PM10.
(2) Collect a minimum sample volume of 60 dry standard cubic feet
(dscf) during each particulate matter or PM10 test run. Three
valid test runs are needed to comprise a performance test.
(c) Compute the mass emissions rate in pounds per hour (lbs/hr) for
each test run using Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR10OC03.000
Where:
Elbs/hr = Mass emissions rate of particulate matter or
PM10 (lbs/hr);
Cs = Concentration of particulate matter or PM10
in the gas stream, grains per dry standard cubic feet (gr/dscf);
Qstd = Volumetric flow rate of stack gas, dry standard cubic
feet per minute (dscfm);
60 = Conversion factor, minutes per hour (min/hr); and
7,000 = Conversion factor, grains per pound (gr/lb).
Sec. 63.9914 What test methods and other procedures must I use to
demonstrate initial compliance with chlorine and hydrochloric acid
emission limits?
(a) You must conduct each performance test that applies to your
affected source according to the requirements in Sec. 63.7(e)(1).
(b) To determine compliance with the applicable emission limits for
chlorine and hydrochloric acid in Table 1 to this subpart, you must
follow the test methods and procedures specified in paragraphs (b)(1)
and (2) of this section.
(1) Determine the concentration of chlorine and hydrochloric acid
according to the following test methods in appendix A to 40 CFR part 60:
(i) Method 1 to select sampling port locations and the number of
traverse points. Sampling ports must be located at the outlet of the
control device and prior to any releases to the atmosphere.
(ii) Method 2, 2F, or 2G to determine the volumetric flow of the
stack gas.
(iii) Method 3, 3A, or 3B to determine the dry molecular weight of
the stack gas.
(iv) Method 4 to determine the moisture content of the stack gas.
(v) Method 26 or 26A, as applicable, to determine the concentration
of hydrochloric acid and chlorine.
(2) Collect a minimum sample of 60 dscf during each test run for
chlorine and hydrochloric acid. Three valid test runs are needed to
comprise a performance test.
(c) Compute the mass emissions rate (lbs/hr) for each test run using
Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR10OC03.001
Where:
Elbs/hr = Mass emissions rate of chlorine or hydrochloric
acid (lbs/hr);
Cs = Concentration of chlorine or hydrochloric acid in the
gas stream, milligrams per dry standard cubic meter (mg/dscm);
Qstd = Volumetric flow rate of stack gas (dscfm);
60 = Conversion factor (min/hr);
35.31 = Conversion factor (dscf/dscm); and
454,000 = Conversion factor (mg/lb).
Sec. 63.9915 What test methods and other procedures must I use to
demonstrate initial compliance with dioxin/furan emission limits?
(a) You must conduct each performance test that applies to your
affected source according to the requirements in Sec. 63.7(e)(1).
(b) To determine compliance with the applicable emission limit for
dioxins/furans in Table 1 to this subpart, you must follow the test
methods and procedures specified in paragraphs (b)(1) and (2) of this
section.
(1) Determine the concentration of dioxin and furan according to the
following test methods in appendix A to 40 CFR part 60:
(i) Method 1 to select sampling port locations and the number of
traverse points. Sampling ports must be located at the outlet of the
control device and prior to any releases to the atmosphere.
(ii) Method 2, 2F, or 2G to determine the volumetric flow of the
stack gas.
(iii) Method 3, 3A, or 3B to determine the dry molecular weight of
the stack gas.
(iv) Method 4 to determine the moisture content of the stack gas.
(v) Method 23 to determine the concentration of dioxins/furans. For
each
[[Page 139]]
dioxin/furan congener measured in accordance with this paragraph (b)(v),
multiply the congener concentration by its corresponding toxic
equivalency factor specified in Table 2 of this subpart.
(2) Collect a minimum sample of 100 dscf during each test run. Three
valid test runs are needed to comprise a performance test.
Sec. 63.9916 What test methods and other procedures must I use to
establish and demonstrate initial compliance with the operating limits?
For a wet scrubber subject to operating limits for pressure drop and
scrubber water flow rate in Sec. 63.9890(b), you must establish site-
specific operating limits according to the procedures in paragraphs (a)
and (b) of this section.
(a) Using the continuous parameter monitoring system (CPMS) required
in Sec. 63.9920, measure and record the pressure drop and scrubber
water flow rate at least every 15 minutes during each run of the
particulate matter performance test.
(b) Compute and record the average pressure drop and scrubber water
flow rate for each individual test run. Your operating limits are the
lowest average individual pressure drop and scrubber water flow rate
values in any of the three runs that meet the applicable emission limit.
Sec. 63.9917 How do I demonstrate initial compliance with the emission
limitations and work practice standards that apply to me?
(a) For each affected source subject to an emission limit in Table 1
to this subpart, you have demonstrated initial compliance if:
(1) You have met the conditions in Table 3 to this subpart; and
(2) For each wet scrubber subject to the operating limits for
pressure drop and scrubber water flow rate in Sec. 63.9890(b), you have
established appropriate site-specific operating limits and have a record
of the pressure drop and scrubber water flow rate measured during the
performance test in accordance with Sec. 63.9916.
(b) You have demonstrated initial compliance with the work practice
standards in Sec. 63.9891 if you have certified in your notification of
compliance status that:
(1) You have prepared a fugitive dust emissions control plan
according to the requirements in Sec. 63.9891 and submitted the plan
for approval; and
(2) You will operate according to the requirements in the plan.
Sec. 63.9918 How do I demonstrate initial compliance with the operation
and maintenance requirements that apply to me?
You must demonstrate initial compliance by certifying in your
notification of compliance status that you have met the requirements in
paragraphs (a) and (b) of this section.
(a) You have prepared the operation and maintenance plan according
to the requirements in Sec. 63.9910; and
(b) You will operate each control device according to the procedures
in the plan.
Continuous Compliance Requirements
Sec. 63.9920 What are my continuous monitoring requirements?
For each wet scrubber subject to the operating limits for pressure
drop and scrubber water flow rates in Sec. 63.9890(b), you must at all
times monitor the hourly average pressure drop and liquid flow rate
using a CPMS according to the requirements in Sec. 63.9921(a).
Sec. 63.9921 What are the installation, operation and maintenance
requirements for my monitors?
(a) For each wet scrubber subject to the operating limits in Sec.
63.9890(b) for pressure drop and scrubber water flow rate, you must
install, operate, and maintain each CPMS according to the requirements
in paragraphs (a)(1) and (2) of this section.
(1) For the pressure drop CPMS, you must:
(i) Locate the pressure sensor(s) in or as close to a position that
provides a representative measurement of the pressure and that minimizes
or eliminates pulsating pressure, vibration, and internal and external
corrosion.
(ii) Use a gauge with a minimum measurement sensitivity of 0.5 inch
of water or a transducer with a minimum measurement sensitivity of 1
percent of the pressure range.
[[Page 140]]
(iii) Check the pressure tap for pluggage daily.
(iv) Using a manometer, check gauge calibration quarterly and
transducer calibration monthly.
(v) Conduct calibration checks any time the sensor exceeds the
manufacturer's specified maximum operating pressure range, or install a
new pressure sensor.
(vi) At least monthly, inspect all components for integrity, all
electrical connections for continuity, and all mechanical connections
for leakage.
(2) For the scrubber water flow rate CPMS, you must:
(i) Locate the flow sensor and other necessary equipment in a
position that provides a representative flow and that reduces swirling
flow or abnormal velocity distributions due to upstream and downstream
disturbances.
(ii) Use a flow sensor with a minimum measurement sensitivity of 2
percent of the flow rate.
(iii) Conduct a flow sensor calibration check at least semiannually
according to the manufacturer's instructions.
(iv) At least monthly, inspect all components for integrity, all
electrical connections for continuity, and all mechanical connections
for leakage.
(b) You must install, operate, and maintain each CPMS for a wet
scrubber according to the requirements in paragraphs (b)(1) through (3)
of this section.
(1) Each CPMS must complete a minimum of one cycle of operation for
each successive 15-minute period.
(2) Each CPMS must have valid data for at least 95 percent of every
averaging period.
(3) Each CPMS must determine and record the hourly average of all
recorded readings.
Sec. 63.9922 How do I monitor and collect data to demonstrate
continuous compliance?
(a) Except for monitoring malfunctions, associated repairs, and
required quality assurance or control activities (including, as
applicable, calibration checks and required zero and span adjustments),
you must monitor continuously (or collect data at all required
intervals) at all times an affected source is operating.
(b) You may not use data recorded during monitoring malfunctions,
associated repairs, and required quality assurance or control activities
in data averages and calculations used to report emission or operating
levels or to fulfill a minimum data availability requirement, if
applicable. You must use all the data collected during all other periods
in assessing compliance.
(c) A monitoring malfunction is any sudden, infrequent, not
reasonably preventable failure of the monitoring to provide valid data.
Monitoring failures that are caused in part by poor maintenance or
careless operation are not malfunctions.
Sec. 63.9923 How do I demonstrate continuous compliance with the emission
limitations and work practice standards that apply to me?
(a) For each affected source subject to an emission limit in Table 1
to this subpart, you must demonstrate continuous compliance according to
the requirements in Table 4 to this subpart.
(b) For each wet scrubber subject to the operating limits for
pressure drop and scrubber water flow rate in Sec. 63.9890(b), you must
demonstrate continuous compliance according to the requirements in
paragraphs (b)(1) and (2) of this section.
(1) Collecting and reducing the monitoring data according to Sec.
63.9921(b); and
(2) Maintaining the hourly average pressure drop and scrubber water
flow rate at or above the minimum level established during the initial
or subsequent performance.
(c) You must demonstrate continuous compliance with the work
practice standards in Sec. 63.9891 by operating according to the
requirements in your fugitive dust emissions control plan and recording
information needed to document conformance with the requirements.
[[Page 141]]
Sec. 63.9924 How do I demonstrate continuous compliance with the
operation and maintenance requirements that apply to me?
For each emission point subject to an emission limit in Table 1 to
this subpart, you must demonstrate continuous compliance with the
operation and maintenance requirements in Sec. 63.9900 by performing
preventive maintenance for each control device according to Sec.
63.9900(b) and recording all information needed to document conformance
with these requirements.
Sec. 63.9925 What other requirements must I meet to demonstrate
continuous compliance?
(a) Deviations. You must report each instance in which you did not
meet each emission limitation in Sec. 63.9890 or work practice standard
in Sec. 63.9891 that applies to you. This includes periods of startup,
shutdown, and malfunction. You must also report each instance in which
you did not meet each operation and maintenance requirement required in
Sec. 63.9900 that applies to you. These instances are deviations from
the emission limitations, work practice standards, and operation and
maintenance requirements in this subpart. These deviations must be
reported according to the requirements in Sec. 63.9931.
(b) Startups, shutdowns, and malfunctions. (1) Consistent with
Sec. Sec. 63.6(e) and 63.7(e)(1), deviations that occur during a period
of startup, shutdown, or malfunction are not violations if you
demonstrate to the Administrator's satisfaction that you were operating
in accordance with Sec. 63.6(e)(1).
(2) The Administrator will determine whether deviations that occur
during a period of startup, shutdown, or malfunction are violations,
according to the provisions in Sec. 63.6(e).
[68 FR 58620, Oct. 10, 2003, as amended at 71 FR 20471, Apr. 20, 2006]
Notifications, Reports, and Records
Sec. 63.9930 What notifications must I submit and when?
(a) You must submit all of the notifications in Sec. Sec. 63.7(b)
and (c), 63.8(f)(4), 63.9(b), and 63.9(h) that apply to you by the
specified dates.
(b) As specified in Sec. 63.9(b)(2), if you startup your affected
source before October 10, 2003, you must submit your initial
notification no later than February 9, 2004.
(c) As specified in Sec. 63.9(b)(3), if you start your new affected
source on or after October 10, 2003, you must submit your initial
notification no later that 120 calendar days after you become subject to
this subpart.
(d) If you are required to conduct a performance test, you must
submit a notification of intent to conduct a performance test at least
60 calendar days before the performance test is scheduled to begin as
required in Sec. 63.7(b)(1).
(e) If you are required to conduct a performance test or other
initial compliance demonstration, you must submit a notification of
compliance status according to Sec. 63.9(h)(2)(ii), and the
requirements in paragraphs (e)(1) and (2) of this section:
(1) For each initial compliance demonstration that does not include
a performance test, you must submit the notification of compliance
status before the close of business on the 30th calendar day following
completion of the initial compliance demonstration.
(2) For each initial compliance demonstration that does include a
performance test, you must submit the notification of compliance status,
including the performance test results, before the close of business on
the 60th calendar day following the completion of the performance test
according to Sec. 63.10(d)(2).
Sec. 63.9931 What reports must I submit and when?
(a) Compliance report due dates. Unless the Administrator has
approved a different schedule, you must submit a semiannual compliance
report to your permitting authority according to the requirements in
paragraphs (a) (1) through (5) of this section.
(1) The first compliance report must cover the period beginning on
the compliance date that is specified for your affected source in Sec.
63.9883 and ending on June 30 or December 31, whichever date comes after
the compliance date that is specified for your source in Sec. 63.9883.
[[Page 142]]
(2) The first compliance report must be postmarked or delivered no
later than July 31 or January 31, whichever date comes first after your
compliance report is due.
(3) Each subsequent compliance report must cover the semiannual
reporting period from January 1 through June 30 or the semiannual
reporting period from July 1 through December 31.
(4) Each subsequent compliance report must be postmarked or
delivered no later than July 31 or January 31, whichever date comes
first after the end of the semiannual reporting period.
(5) For each affected source that is subject to permitting
regulations pursuant to 40 CFR part 70 or 40 CFR part 71, and if the
permitting authority has established dates for submitting semiannual
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance
reports according to the dates the permitting authority has established
instead of according to the dates in paragraphs (a)(1) through (4) of
this section.
(b) Compliance report contents. Each compliance report must include
the information in paragraphs (b)(1) through (3) of this section and, as
applicable, paragraphs (b)(4) through (8) of this section.
(1) Company name and address.
(2) Statement by a responsible official, with that official's name,
title, and signature, certifying the truth, accuracy, and completeness
of the content of the report.
(3) Date of report and beginning and ending dates of the reporting
period.
(4) If you had a startup, shutdown, or malfunction during the
reporting period and you took actions consistent with your startup,
shutdown, and malfunction plan, the compliance report must include the
information in Sec. 63.10(d)(5)(i).
(5) If there were no deviations from the continuous compliance
requirements in Sec. Sec. 63.9923 and 63.9924 that apply to you, a
statement that there were no deviations from the emission limitations,
work practice standards, or operation and maintenance requirements
during the reporting period.
(6) If there were no periods during which a CPMS was out-of-control
as specified in Sec. 63.8(c)(7), a statement that there were no periods
during which the CPMS was out-of-control during the reporting period.
(7) For each deviation from an emission limitation in Sec. 63.9890
that occurs at an affected source where you are not using a CPMS to
comply with an emission limitation in this subpart, the compliance
report must contain the information in paragraphs (b)(1) through (4) of
this section and the information in paragraphs (b)(7)(i) and (ii) of
this section. This includes periods of startup, shutdown, and
malfunction.
(i) The total operating time of each affected source during the
reporting period.
(ii) Information on the number, duration, and cause of deviations
(including unknown cause, if applicable) as applicable and the
corrective action taken.
(8) For each deviation from an emission limitation occurring at an
affected source where you are using a CPMS to comply with the emission
limitation in this subpart, you must include the information in
paragraphs (b)(1) through (4) of this section and the information in
paragraphs (b)(8)(i) through (xi) of this section. This includes periods
of startup, shutdown, and malfunction.
(i) The date and time that each malfunction started and stopped.
(ii) The date and time that each continuous monitoring was
inoperative, except for zero (low-level) and high-level checks.
(iii) The date, time, and duration that each continuous monitoring
system was out-of-control, including the information in Sec.
63.8(c)(8).
(iv) The date and time that each deviation started and stopped, and
whether each deviation occurred during a period of startup, shutdown, or
malfunction or during another period.
(v) A summary of the total duration of the deviation during the
reporting period and the total duration as a percent of the total source
operating time during that reporting period.
(vi) A breakdown of the total duration of the deviations during the
reporting period including those that are due to startup, shutdown,
control
[[Page 143]]
equipment problems, process problems, other known causes, and other
unknown causes.
(vii) A summary of the total duration of continuous monitoring
system downtime during the reporting period and the total duration of
continuous monitoring system downtime as a percent of the total source
operating time during the reporting period.
(viii) A brief description of the process units.
(ix) A brief description of the continuous monitoring system.
(x) The date of the latest continuous monitoring system
certification or audit.
(xi) A description of any changes in continuous monitoring systems,
processes, or controls since the last reporting period.
(c) Immediate startup, shutdown, and malfunction report. If you had
a startup, shutdown, or malfunction during the semiannual reporting
period that was not consistent with your startup, shutdown, and
malfunction plan, you must submit an immediate startup, shutdown, and
malfunction report according to the requirements in Sec.
63.10(d)(5)(ii).
(d) Part 70 monitoring report. If you have obtained a title V
operating permit for an affected source pursuant to 40 CFR part 70 or 40
CFR part 71, you must report all deviations as defined in this subpart
in the semiannual monitoring report required by 40 CFR
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A). If you submit a
compliance report for an affected source along with, or as part of, the
semiannual monitoring report required by 40 CFR 70.6(a)(3)(iii)(A) or 40
CFR 71.6(a)(3)(iii)(A), and the compliance report includes all the
required information concerning deviations from any emissions
limitation, work practice standards, or operation and maintenance
requirement in this subpart, submission of the compliance report
satisfies any obligation to report the same deviations in the semiannual
monitoring report. However, submission of the compliance report does not
otherwise affect any obligation you may have to report deviations from
permit requirements for an affected source to your permitting authority.
Sec. 63.9932 What records must I keep?
(a) You must keep the records as indicated in paragraphs (a)(1)
through (3) of this section:
(1) A copy of each notification and report that you submitted to
comply with this subpart, including all documentation supporting any
initial notification or notification of compliance status that you
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
(2) The records in Sec. 63.6(e)(3)(iii) through (v) related to
startup, shutdown, and malfunction.
(3) Records of performance tests and performance evaluations as
required in Sec. 63.10(b)(2)(viii).
(b) You must keep the records required in Sec. Sec. 63.9932 and
63.9933 to show continuous compliance with each emission limitation,
work practice standard, and operating and maintenance requirement that
applies to you.
Sec. 63.9933 In what form and how long must I keep my records?
(a) Your records must be in a form suitable and readily available
for expeditious review, according to Sec. 63.10(b)(1).
(b) As specified in Sec. 63.10(b)(1), you must keep each record for
5 years following the date of each occurrence, measurement, maintenance,
corrective action, report, or record.
(c) You must keep each record on site for at least 2 years after the
date of each occurrence, measurement, maintenance, corrective action,
report, or record according to Sec. 63.10(b)(1). You can keep the
records off site for the remaining 3 years.
(d) You must keep your fugitive dust emissions control plan and your
operation and maintenance plan on-site according to the requirements in
Sec. Sec. 63.9891(d) and 63.9900(c).
Other Requirements and Information
Sec. 63.9940 What parts of the General Provisions apply to me?
Table 4 to this subpart shows which parts of the General Provisions
in Sec. Sec. 63.1 through 63.15 apply to you.
[[Page 144]]
Sec. 63.9941 Who implements and enforces this subpart?
(a) This subpart can be implemented and enforced by us, the United
States Environmental Protection Agency (U.S. EPA) or a delegated
authority such as your State, local, or tribal agency. If the EPA
Administrator has delegated authority to your State, local, or tribal
agency, then that agency has the authority to implement and enforce this
subpart. You should contact your EPA Regional Office to find out if this
subpart is delegated to your State, local, or tribal agency.
(b) In delegating implementation and enforcement authority of this
subpart to a State, local, or tribal agency under subpart E of this
part, the authorities contained in paragraph (c) of this section are
retained by the Administrator of the EPA and are not transferred to the
State, local, or tribal agency.
(c) The authorities that will not be delegated to State, local, or
tribal agencies are specified in paragraphs (c)(1) through (4) of this
section.
(1) Approval of alternatives to the non-opacity emission limitations
in Sec. 63.9890 and work practice standards in Sec. 63.9891 under
Sec. 63.6(g).
(2) Approval of major alternatives to test methods under Sec.
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
(3) Approval of major alternatives to monitoring under Sec. 63.8(f)
and as defined in Sec. 63.90.
(4) Approval of major alternatives to recordkeeping and reporting
under Sec. 63.10(f) and as defined in Sec. 63.90.
Sec. 63.9942 What definitions apply to this subpart?
Terms used in this subpart are defined in the Clean Air Act, in
Sec. 63.2, and in this section as follows:
Chlorine plant bypass scrubber means the wet scrubber that captures
chlorine gas during a chlorine plant shut down or failure.
Deviation means any instance in which an affected source subject to
this subpart, or an owner or operator of such a source:
(1) Fails to meet any requirement or obligation established by this
subpart, including but not limited to any emission limitation (including
operating limits) or operation and maintenance requirement;
(2) Fails to meet any term or condition that is adopted to implement
an applicable requirement in this subpart and that is included in the
operating permit for any affected source required to obtain such a
permit; or
(3) Fails to meet any emission limitation in this subpart during
startup, shutdown, or malfunction, regardless of whether or not such
failure is permitted by this subpart.
Emission limitation means any emission limit, opacity limit, or
operating limit.
Launder off-gas system means a system that collects chlorine and
hydrochloric acid fumes from collection points within the melt/reactor
system building. The system then removes particulate matter and
hydrochloric acid from the collected gases prior to discharge to the
atmosphere.
Magnesium chloride storage bins means vessels that store dried
magnesium chloride powder produced from the spray drying operation.
Melt/reactor system means a system that melts and chlorinates
dehydrated brine to produce high purity molten magnesium chloride feed
for electrolysis.
Primary magnesium refining means the production of magnesium metal
and magnesium metal alloys from natural sources of magnesium chloride
such as sea water or water from the Great Salt Lake and magnesium
bearing ores.
Responsible official means responsible official as defined in Sec.
63.2.
Spray dryer means dryers that evaporate brine to form magnesium
powder by contact with high temperature gases exhausted from gas
turbines.
Wet scrubber means a device that contacts an exhaust gas with a
liquid to remove particulate matter and acid gases from the exhaust.
Examples are packed-bed wet scrubbers and venturi scrubbers.
Work practice standard means any design, equipment, work practice,
or operational standard, or combination thereof, that is promulgated
pursuant to section 112(h) of the Clean Air Act.
[[Page 145]]
Table 1 to Subpart TTTTT of Part 63--Emission Limits
As required in Sec. 63.9890(a), you must comply with each
applicable emission limit in the following table:
------------------------------------------------------------------------
You must comply with each of the
For . . . following . . .
------------------------------------------------------------------------
1. Each spray dryer stack.... a. You must not cause to be discharged to
the atmosphere any gases that contain
particulate matter in excess of 100 lbs/
hr; and
b. You must not cause to be discharged to
the atmosphere any gases that contain
hydrochloric acid in excess of 200 lbs/
hr.
2. Each magnesium chloride a. You must not cause to be discharged to
storage bins scrubber stack. the atmosphere any gases that contain
hydrochloric acid in excess of 47.5 lbs/
hr and 0.35 gr/dscf; and
b. You must not cause to be discharged to
the atmosphere any gases that contain
PM10 in excess of 2.7 lbs/hr and 0.016
gr/dscf.
3. Each melt/reactor system a. You must not cause to be discharged to
stack. the atmosphere any gases that contain
PM10 in excess of 13.1 lbs/hr; and
b. You must not cause to be discharged to
the atmosphere any gases that contain
hydrochloric acid in excess of 7.2 lbs/
hr; and
c. You must not cause to be discharged to
the atmosphere any gases that contain
chlorine in excess of 100 lbs/hr; and
d. You must not cause to be discharged to
the atmosphere any gases that contain 36
ng TEQ/dscm corrected to 7% oxygen.
4. Each launder off-gas a. You must not cause to be discharged to
system stack. the atmosphere any gases that contain
particulate matter in excess of 37.5 lbs/
hr; and
b. You must not cause to be discharged to
the atmosphere any gases that contain
hydrochloric acid in excess of 46.0 lbs/
hr; and
c. You must not cause to be discharged to
the atmosphere any gases that contain
chlorine in excess of 26.0 lbs/hr.
------------------------------------------------------------------------
Table 2 to Subpart TTTTT of Part 63--Toxic Equivalency Factors
------------------------------------------------------------------------
Toxic
Dioxin/furan congener equivalency
factor
------------------------------------------------------------------------
2,3,7,8-tetrachlorinated dibenzo-p-dioxin.............. 1
1,2,3,7,8-pentachlorinated dibenzo-p-dioxin............ 1
1,2,3,4,7,8-hexachlorinated dibenzo-p-dioxin........... 0.1
1,2,3,7,8,9-hexachlorinated dibenzo-p-dioxin........... 0.1
1,2,3,6,7,8-hexachlorinated dibenzo-p-dioxin........... 0.1
1,2,3,4,6,7,8-heptachlorinated dibenzo-p-dioxin........ 0.01
octachlorinated dibenzo-p-dioxin....................... 0.0001
2,3,7,8-tetrachlorinated dibenzofuran.................. 0.1
2,3,4,7,8-pentachlorinated dibenzofuran................ 0.5
1,2,3,7,8-pentachlorinated dibenzofuran................ 0.05
1,2,3,4,7,8-hexachlorinated dibenzofuran............... 0.1
1,2,3,6,7,8-hexachlorinated dibenzofuran............... 0.1
1,2,3,7,8,9-hexachlorinated dibenzofuran............... 0.1
2,3,4,6,7,8-hexachlorinated dibenzofuran............... 0.1
1,2,3,4,6,7,8-heptachlorinated dibenzofuran............ 0.01
1,2,3,4,7,8,9-heptachlorinated dibenzofuran............ 0.01
octachlorinated dibenzofuran........................... 0.0001
------------------------------------------------------------------------
Table 3 to Subpart TTTTT of Part 63--Initial Compliance with Emission
Limits
As required in 63.9916, you must demonstrate initial compliance with
the emission limits according to the following table:
------------------------------------------------------------------------
You have demonstrated initial compliance
For . . . if . . .
------------------------------------------------------------------------
1. Each spray dryer stack.... a. The average mass flow of particulate
matter from the control system applied
to emissions from each spray dryer,
measured according to the performance
test procedures in Sec. 63.9913(c),
did not exceed 100 lbs/hr; and
b. The average mass flow of hydrochloric
acid from the control system applied to
emissions from each spray dryer,
determined according to the performance
test procedures in Sec. 63.9914(c),
did not exceed 200 lbs/hr.
2. Each magnesium chloride a. The average mass flow of hydrochloric
storage bin scrubber stack. acid from the control system applied to
the magnesium chloride storage bins
scrubber exhaust, measured according to
the performance test procedure in Sec.
63.9914, did not exceed 47.5 lbs/hr and
0.35 gr/dscf; and
[[Page 146]]
b. The average mass flow of PM10 from the
control system applied to the magnesium
chloride storage bins scrubber exhaust,
determined according to the performance
test procedures in Sec. 63.9913, did
not exceed 2.7 lbs/hr and 0.016 gr/dscf.
3. Each melt/reactor system a. The average mass flow of PM10 from the
stack. control system applied to the melt/
reactor system exhaust, measured
according to the performance test
procedures in Sec. 63.9913, did not
exceed 13.1 lbs/hr; and
b. The average mass flow of hydrochloric
acid from the control system applied to
the melt/reactor system exhaust,
measured according to the performance
test procedures in Sec. 63.9914, did
not exceed 7.2 lbs/hr; and
c. The average mass flow of chlorine from
the control system applied to the melt/
reactor system exhaust, measured
according to the performance test
procedures in Sec. 63.9914, did not
exceed 100 lbs/hr.
d. The average concentration of dioxins/
furans from the control system applied
to the melt/reactor system exhaust,
measured according to the performance
test procedures in Sec. 63.9915, did
not exceed 36 ng TEQ/dscm corrected to
7% oxygen.
4. Each launder off-gas a. The average mass flow of particulate
system stack. matter from the control system applied
to the launder off-gas system collection
system exhaust, measured according to
the performance test procedures in Sec.
63.9913, did not exceed 37.5 lbs/hr;
and
b. The average mass flow of hydrochloric
acid from the control system applied to
the launder off-gas system collection
system exhaust, measured according to
the performance test procedures in Sec.
63.9914, did not exceed 46.0 lbs/hr;
and
c. The average mass flow of chlorine from
the control system applied to the
launder off-gas system collection system
exhaust, measured according to the
performance test procedures in Sec.
63.9914, did not exceed 26.0 lbs/hr.
------------------------------------------------------------------------
Table 4 to Subpart TTTTT of Part 63--Continuous Compliance with Emission
Limits
As required in Sec. 63.9923, you must demonstrate continuous
compliance with the emission limits according to the following table:
------------------------------------------------------------------------
You must demonstrate continuous
For . . . compliance by . . .
------------------------------------------------------------------------
1. Each spray dryer stack.... a. Maintaining emissions of PM10 at or
below 100 lbs/hr; and
b. Maintaining emissions of hydrochloric
acid at or below 200 lbs/hr; and
c. Conducting subsequent performance
tests at least twice during each term of
your title V operating permit (at mid-
term and renewal).
2. Magnesium chloride storage a. Maintaining emissions of hydrochloric
bins scrubber stack. acid at or below 47.5 lbs/hr and 0.35 gr/
dscf; and
b. Maintaining emissions of PM10 at or
below 2.7 lbs/hr and 0.016 gr/dscf; and
c. Conducting subsequent performance
tests at least twice during each term of
your title V operating permit (at mid-
term and renewal).
3. Each melt/reactor system a. Maintaining emissions of PM10 at or
stack. below 13.1 lbs/hr; and
b. Maintaining emissions of hydrochloric
acid at or below 7.2 lbs/hr; and
c. Maintaining emissions of chlorine at
or below 100 lbs/hr; and
d. Maintaining emissions of dioxins/
furans at or below 36 ng TEQ/dscm
corrected to 7% oxygen.
e. Conducting subsequent performance test
at least twice during each term of your
title V operating permit (at mid-term
and renewal).
4. Each launder off-gas a. Maintaining emissions of particulate
system stack. matter at or below 37.5 lbs/hr; and
b. Maintaining emissions of hydrochloric
acid at or below 46.0 lbs/hr; and
c. Maintaining emissions of chlorine at
or below 26.0 lbs/hr; and
d. Conducting subsequent performance
tests at least twice during each term of
your title V operating permit (at mid-
term and renewal).
------------------------------------------------------------------------
Table 5 to Subpart TTTTT of Part 63--Applicability of General Provisions
to Subpart TTTTT of Part 63
As required in Sec. 63.9950, you must comply with the requirements
of the NESHAP General Provisions (40 CFR part 63, subpart A) shown in
the following table:
----------------------------------------------------------------------------------------------------------------
Citation Subject Applies to Subpart TTTTT Explanation
----------------------------------------------------------------------------------------------------------------
63.1............................... Applicability......... Yes.
63.2............................... Definitions........... Yes.
63.3............................... Units and Yes.
Abbreviations.
63.4............................... Prohibited Activities. Yes.
63.5............................... Construction and Yes.
Reconstruction.
[[Page 147]]
63.6(a)-(g)........................ Compliance with Yes.
Standards and
Maintenance
Requirements.
63.6(h)............................ Determining Compliance No.
with Opacity and
Visible Emission
Standards.
63.6(i)-(j)........................ Extension of Yes.
Compliance and
Presidential
Compliance Exemption.
63.7(a)(1)-(2)..................... Applicability and No Subpart TTTTT
Performance Test specifies performance
Dates. test applicability
and dates.
63.7(a)(3), (b)-(h)................ Performance Testing Yes.
Requirements.
63.8 except for (a)(4),(c)(4), and Monitoring Yes.
(f)(6). Requirements.
63.8(a)(4)......................... Additional Monitoring No......................... Subpart TTTTT does not
Requirements for require flares.
Control Devices in
Sec. 63.11.
63.8(c)(4)......................... Continuous Monitoring No......................... Subpart TTTTT
System Requirements. specifies
requirements for
operation of CMS.
63.8(f)(6)......................... Relative Accuracy Test No......................... Subpart TTTTT does not
Alternative (RATA). require continuous
emission monitoring
systems.
63.9............................... Notification Yes.
Requirements.
63.9(g)(5)......................... Data Reduction........ No......................... Subpart TTTTT
specifies data
reduction
requirements.
63.10 except for (b)(2)(xiii) and Recordkeeping and Yes.
(c)(7)-(8). Reporting
Requirements.
63.10(b)(2)(xiii).................. Continuous Monitoring No......................... Subpart TTTTT does not
System (CMS) Records require continuous
for RATA Alternative. emission monitoring
systems.
63.10(c)(7)-(8).................... Records of Excess No......................... Subpart TTTTT
Emissions and specifies
Parameter Monitoring recordkeeping
Accedences for CMS. requirements.
63.11.............................. Control Device No......................... Subpart TTTTT does not
Requirements. require flares.
63.12.............................. State Authority and Yes.
Delegations.
63.13-63.15........................ Addresses, Yes.
Incorporation by
Reference,
Availability of
Information.
----------------------------------------------------------------------------------------------------------------
Appendix A to Part 63--Test Methods
Method 301--Field Validation of Pollutant Measurement Methods from
Various Waste Media
1. Applicability and principle
1.1 Applicability. This method, as specified in the applicable
subpart, is to be used whenever a source owner or operator (hereafter
referred to as an ``analyst'') proposes a test method to meet a U.S.
Environmental Protection Agency (EPA) requirement in the absence of a
validated method. This Method includes procedures for determining and
documenting the quality, i.e., systematic error (bias) and random error
(precision), of the measured concentrations from an effected source.
This method is applicable to various waste media (i.e., exhaust gas,
wastewater, sludge, etc.).
1.1.1 If EPA currently recognizes an appropriate test method or
considers the analyst's test method to be satisfactory for a particular
source, the Administrator may waive the use of this protocol or may
specify a less rigorous validation procedure. A list of validated
methods may be obtained by contacting the Emission Measurement Technical
Information Center (EMTIC), Mail Drop 19, U.S. Environmental Protection
Agency, Research Triangle Park, NC 27711, (919) 541-0200. Procedures for
obtaining a waiver are in Section 12.0.
1.1.2 This method includes optional procedures that may be used to
expand the applicability of the proposed method. Section 7.0 involves
ruggedness testing (Laboratory Evaluation), which demonstrates the
sensitivity of the method to various parameters. Section 8.0 involves a
procedure for including sample stability in bias and precision for
assessing sample recovery and analysis times; Section 9.0 involves a
procedure for the determination of the practical limit of quantitation
for determining the lower limit of the method. These optional procedures
are required for the waiver consideration outlined in Section 12.0.
[[Page 148]]
1.2 Principle. The purpose of these procedures is to determine bias
and precision of a test method at the level of the applicable standard.
The procedures involve (a) introducing known concentrations of an
analyte or comparing the test method against a validated test method to
determine the method's bias and (b) collecting multiple or collocated
simultaneous samples to determine the method's precision.
1.2.1 Bias. Bias is established by comparing the method's results
against a reference value and may be eliminated by employing a
correction factor established from the data obtained during the
validation test. An offset bias may be handled accordingly. Methods that
have bias correction factors outside 0.7 to 1.3 are unacceptable.
Validated method to proposed method comparisons, section 6.2, requires a
more restrictive test of central tendency and a lower correction factor
allowance of 0.90 to 1.10.
1.2.2 Precision. At the minimum, paired sampling systems shall be
used to establish precision. The precision of the method at the level of
the standard shall not be greater than 50 percent relative standard
deviation. For a validated method to proposed method equivalency
comparisons, section 6.2, the analyst must demonstrate that the
precision of the proposed test method is as precise as the validated
method for acceptance.
2. Definitions
2.1 Negative bias. Bias resulting when the measured result is less
than the ``true'' value.
2.2 Paired sampling system. A sampling system capable of obtaining
two replicate samples that were collected as closely as possible in
sampling time and sampling location.
2.3 Positive bias. Bias resulting when the measured result is
greater than the ``true'' value.
2.4 Proposed method. The sampling and analytical methodology
selected for field validation using the method described herein.
2.5 Quadruplet sampling system. A sampling system capable of
obtaining four replicate samples that were collected as closely as
possible in sampling time and sampling location.
2.6 Surrogate compound. A compound that serves as a model for the
types of compounds being analyzed (i.e., similar chemical structure,
properties, behavior). The model can be distinguished by the method from
the compounds being analyzed.
3. Reference Material
The reference materials shall be obtained or prepared at the level
of the standard. Additional runs with higher and lower reference
material concentrations may be made to expand the applicable range of
the method, in accordance with the ruggedness test procedures.
3.1 Exhaust Gas Tests. The analyst shall obtain a known
concentration of the reference material (i.e., analyte of concern) from
an independent source such as a specialty gas manufacturer, specialty
chemical company, or commercial laboratory. A list of vendors may be
obtained from EMTIC (see Section 1.1.1). The analyst should obtain the
manufacturer's stability data of the analyte concentration and
recommendations for recertification.
3.2 Other Waste Media Tests. The analyst shall obtain pure liquid
components of the reference materials (i.e., analytes of concern) from
an independent manufacturer and dilute them in the same type matrix as
the source waste. The pure reference materials shall be certified by the
manufacturer as to purity and shelf life. The accuracy of all diluted
reference material concentrations shall be verified by comparing their
response to independently-prepared materials (independently prepared in
this case means prepared from pure components by a different analyst).
3.3 Surrogate Reference Materials. The analyst may use surrogate
compounds, e.g., for highly toxic or reactive organic compounds,
provided the analyst can demonstrate to the Administrator's satisfaction
that the surrogate compound behaves as the analyte. A surrogate may be
an isotope or one that contains a unique element (e.g., chlorine) that
is not present in the source or a derivation of the toxic or reactive
compound, if the derivative formation is part of the method's procedure.
Laboratory experiments or literature data may be used to show behavioral
acceptability.
3.4 Isotopically Labeled Materials. Isotope mixtures may contain the
isotope and the natural analyte. For best results, the isotope labeled
analyte concentration should be more than five times the natural
concentration of the analyte.
4. EPA Performance Audit Material
4.1 To assess the method bias independently, the analyst shall use
(in addition to the reference material) an EPA performance audit
material, if it is available. The analyst may contact EMTIC (see section
1.1.1) to receive a list of currently available EPA audit materials. If
the analyte is listed, the analyst should request the audit material at
least 30 days before the validation test. If an EPA audit material is
not available, request documentation from the validation report
reviewing authority that the audit material is currently not available
from EPA. Include this documentation with the field validation report.
4.2 The analyst shall sample and analyze the performance audit
sample three times according to the instructions provided with
[[Page 149]]
the audit sample. The analyst shall submit the three results with the
field validation report. Although no acceptance criteria are set for
these performance audit results, the analyst and reviewing authority may
use them to assess the relative error of sample recovery, sample
preparation, and analytical procedures and then consider the relative
error in evaluating the measured emissions.
5. Procedure for Determination of Bias and Precision in the Field
The analyst shall select one of the sampling approaches below to
determine the bias and precision of the data. After analyzing the
samples, the analyst shall calculate the bias and precision according to
the procedure described in section 6.0. When sampling a stationary
source, follow the probe placement procedures in section 5.4.
5.1 Isotopic Spiking. This approach shall be used only for methods
that require mass spectrometry (MS) analysis. Bias and precision are
calculated by procedures described in section 6.1.
5.1.1 Number of Samples and Sampling Runs. Collect a total of 12
replicate samples by either obtaining six sets of paired samples or
three sets of quadruplet samples.
5.1.2 Spiking Procedure. Spike all 12 samples with the reference
material at the level of the standard. Follow the appropriate spiking
procedures listed below for the applicable waste medium.
5.1.2.1 Exhaust Gas Testing. The spike shall be introduced as close
to the tip of the sampling probe as possible.
5.1.2.1.1 Gaseous Reference Material with Sorbent or Impinger
Sampling Trains. Sample the reference material (in the laboratory or in
the field) at a concentration which is close to the allowable
concentration standard for the time required by the method, and then
sample the gas stream for an equal amount of time. The time for sampling
both the reference material and gas stream should be equal; however, the
time should be adjusted to avoid sorbent breakthrough.
5.1.2.1.2 Gaseous Reference Material with Sample Container (Bag or
Canister). Spike the sample containers after completion of each test run
with an amount equal to the allowable concentration standard of the
emission point. The final concentration of the reference material shall
approximate the level of the emission concentration in the stack. The
volume amount of reference material shall be less than 10 percent of the
sample volume.
5.1.2.1.3 Liquid and Solid Reference Material with Sorbent or
Impinger Trains. Spike the trains with an amount equal to the allowable
concentration standard before sampling the stack gas. The spiking should
be done in the field; however, it may be done in the laboratory.
5.1.2.1.4 Liquid and Solid Reference Material with Sample Container
(Bag or Canister). Spike the containers at the completion of each test
run with an amount equal to the level of the emission standard.
5.1.2.2 Other Waste Media. Spike the 12 replicate samples with the
reference material either before or directly after sampling in the
field.
5.2 Comparison Against a Validated Test Method. Bias and precision
are calculated using the procedures described in section 6.2. This
approach shall be used when a validated method is available and an
alternative method is being proposed.
5.2.1 Number of Samples and Sampling Runs. Collect nine sets of
replicate samples using a paired sampling system (a total of 18 samples)
or four sets of replicate samples using a quadruplet sampling system (a
total of 16 samples). In each sample set, the validated test method
shall be used to collect and analyze half of the samples.
5.2.2 Performance Audit Exception. Conduct the performance audit as
required in section 4.0 for the validated test method. Conducting a
performance audit on the test method being evaluated is recommended.
5.3 Analyte Spiking. This approach shall be used when sections 5.1
and 5.2 are not applicable. Bias and precision are calculated using the
procedures described in Section 6.3.
5.3.1 Number of Samples and Sampling Runs. Collect a total of 24
samples using the quadruplet sampling system (a total of 6 sets of
replicate samples).
5.3.2 In each quadruplet set, spike half of the samples (two out of
the four) with the reference material according to the applicable
procedure in section 5.1.2.1 or 5.1.2.2.
5.4 Probe Placement and Arrangement for Stationary Source Stack or
Duct Sampling. The probes shall be placed in the same horizontal plane.
For paired sample probes the arrangement should be that the probe tip is
2.5 cm from the outside edge of the other with a pitot tube on the
outside of each probe. Other paired arrangements for the pitot tube may
be acceptable. For quadruplet sampling probes, the tips should be in a
6.0 cm x 6.0 cm square area measured from the center line of the opening
of the probe tip with a single pitot tube in the center or two pitot
tubes with their location on either side of the probe tip configuration.
An alternative arrangement should be proposed whenever the cross-
sectional area of the probe tip configuration is approximately 5 percent
of the stack or duct cross-sectional area.
6. Calculations
Data resulting from the procedures specified in section 5.0 shall be
treated as follows to determine bias, correction factors, relative
standard deviations, precision, and data acceptance.
[[Page 150]]
6.1 Isotopic Spiking. Analyze the data for isotopic spiking tests as
outlined in sections 6.1.1 through 6.1.6.
6.1.1 Calculate the numerical value of the bias using the results
from the analysis of the isotopically spiked field samples and the
calculated value of the isotopically labeled spike:
B=CS-Sm Eq. 301=1
where:
B=Bias at the spike level.
Sm=Mean of the measured values of the isotopically spiked
samples.
CS=Calculated value of the isotopically labeled spike.
6.1.2 Calculate the standard deviation of the Si values
as follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.048
Eq. 301-2
where:
S i=Measured value of the isotopically labeled analyte in the
ith field sample,
n=Number of isotopically spiked samples, 12.
6.1.3. Calculate the standard deviation of the mean (SDM) as
follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.049
Eq. 301-3
6.1.4 Test the bias for statistical significance by calculating the
t-statistic,
[GRAPHIC] [TIFF OMITTED] TC01MY92.050
Eq. 301-4
and compare it with the critical value of the two-sided t-distribution
at the 95-percent confidence level and n-1 degrees of freedom. This
critical value is 2.201 for the eleven degrees of freedom when the
procedure specified in section 5.1.2 is followed. If the calculated t-
value is greater than the critical value the bias is statistically
significant and the analyst should proceed to evaluate the correction
factor.
6.1.5 Calculation of a Correction Factor. If the t-test does not
show that the bias is statistically significant, use all analytical
results without correction and proceed to the precision evaluation. If
the method's bias is statistically significant, calculate the correction
factor, CF, using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.051
Eq. 301-5
If the CF is outside the range of 0.70 to 1.30, the data and method are
considered unacceptable. For correction factors within the range,
multiply all analytical results by the CF to obtain the final values.
6.1.6 Calculation of the Relative Standard Deviation (Precision).
Calculate the relative standard deviation as follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.052
Eq. 301-6
where Sm is the measured mean of the isotopically labeled
spiked samples.
6.2 Comparison with Validated Method. Analyze the data for
comparison with a validated method as outlined in sections 6.2.1 or
6.2.2, as appropriate. Conduct these procedures in order to determine if
a proposed method produces results equivalent to a validated method.
Make all necessary bias corrections for the validated method, as
appropriate. If the proposed method fails either test, the method
results are unacceptable, and conclude that the proposed method is not
as precise or accurate as the validated method. For highly variable
sources, additional precision checks may be necessary. The analyst
should consult with the Administrator if a highly variable source is
suspected.
6.2.1 Paired Sampling Systems.
6.2.1.1. Precision. Determine the acceptance of the proposed
method's variance with respect to the variability of the validated
method results. If a significant difference is determined, the proposed
method and the results are rejected. Proposed methods demonstrating F-
values equal to or less than the critical value have acceptable
precision.
6.2.1.2 Calculate the variance of the proposed method,
Sp2, and the variance of the validated method,
Sv2, using the following equation:
S(porv)2=SD\2\ Eq. 301-7
where:
SDv=Standard deviation provided with the validated method,
SDp=Standard deviation of the proposed method calculated
using Equation 301-9a.
6.2.1.3 The F-test. Determine if the variance of the proposed method
is significantly different from that of the validated method by
calculating the F-value using the following equation:
[[Page 151]]
[GRAPHIC] [TIFF OMITTED] TC01MY92.053
Eq. 301-8
Compare the experimental F value with the critical value of F. The
critical value is 1.0 when the procedure specified in section 5.2.1 for
paired trains is followed. If the calculated F is greater than the
critical value, the difference in precision is significant and the data
and proposed method are unacceptable.
6.2.1.4 Bias Analysis. Test the bias for statistical significance by
calculating the t-statistic and determine if the mean of the differences
between the proposed method and the validated method is significant at
the 80-percent confidence level. This procedure requires the standard
deviation of the validated method, SDv, to be known. Employ
the value furnished with the method. If the standard deviation of the
validated method is not available, the paired replicate sampling
procedure may not be used. Determine the mean of the paired sample
differences, dm, and the standard deviation, SDd,
of the differences, d1's, using Equation 301-2 where:
di replaces Si, dm replaces
Sm. Calculate the standard deviation of the proposed method,
SDp, as follows:
SDp=SDd-SDv Eq. 301-9a
(If SDvSDd, let SD=SDd/
1.414).
Calculate the value of the t-statistic using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.054
Eq. 301-9
where n is the total number of paired samples. For the procedure in
section 5.2.1, n equals nine. Compare the calculated t-statistic with
the corresponding value from the table of the t-statistic. When nine
runs are conducted, as specified in section 5.2.1, the critical value of
the t-statistic is 1.397 for eight degrees of freedom. If the calculated
t-value is greater than the critical value the bias is statistically
significant and the analyst should proceed to evaluate the correction
factor.
6.2.1.5 Calculation of a Correction Factor. If the statistical test
cited above does not show a significant bias with respect to the
reference method, assume that the proposed method is unbiased and use
all analytical results without correction. If the method's bias is
statistically significant, calculate the correction factor, CF, as
follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.055
Eq. 301-10
where Vm is the mean of the validated method's values.
Multiply all analytical results by CF to obtain the final values.
The method results, and the method, are unacceptable if the correction
factor is outside the range of 0.9 to 1.10.
6.2.2 Quadruplet Replicate Sampling Systems.
6.2.2.1 Precision. Determine the acceptance of the proposed method's
variance with respect to the variability of the validated method
results. If a significant difference is determined the proposed method
and the results are rejected.
6.2.2.2 Calculate the variance of the proposed method,
Sp\2\, using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.056
Eq. 301-11
where the di's are the differences between the validated
method values and the proposed method values.
6.2.2.3 The F-test. Determine if the variance of the proposed method
is more variable than that of the validated method by calculating the F-
value using Equation 301-8. Compare the experimental F value with the
critical value of F. The critical value is 1.0 when the procedure
specified in section 5.2.2 for quadruplet trains is followed. The
calculated F should be less than or equal to the critical value. If the
difference in precision is significant the results and the proposed
method are unacceptable.
6.2.2.4 Bias Analysis. Test the bias for statistical significance at
the 80 percent confidence level by calculating the t-statistic.
Determine the bias (mean of the differences between the proposed method
and the validated method, dm) and the standard deviation,
SDd, of the differences. Calculate the standard deviation of
the differences, SDd, using Equation 301-2 and substituting
di for Si. The following equation is used to
calculate di:
[GRAPHIC] [TIFF OMITTED] TC01MY92.057
Eq. 301-12
and: V1i=First measured value of the validated method in the
ith test sample.
[[Page 152]]
P1i=First measured value of the proposed method in the ith
test sample.
Calculate the t-statistic using Equation 301-9 where n is the total
number of test sample differences (di). For the procedure in
section 5.2.2, n equals four. Compare the calculated t-statistic with
the corresponding value from the table of the t-statistic and determine
if the mean is significant at the 80-percent confidence level. When four
runs are conducted, as specified in section 5.2.2, the critical value of
the t-statistic is 1.638 for three degrees of freedom. If the calculated
t-value is greater than the critical value the bias is statistically
significant and the analyst should proceed to evaluate the correction
factor.
6.2.2.5 Correction Factor Calculation. If the method's bias is
statistically significant, calculate the correction factor, CF, using
Equation 301-10. Multiply all analytical results by CF to obtain the
final values. The method results, and the method, are unacceptable if
the correction factor is outside the range of 0.9 to 1.10.
6.3 Analyte Spiking. Analyze the data for analyte spike testing as
outlined in Sections 6.3.1 through 6.3.3.
6.3.1 Precision.
6.3.1.1 Spiked Samples. Calculate the difference, di,
between the pairs of the spiked proposed method measurements for each
replicate sample set. Determine the standard deviation (SDs)
of the spiked values using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.058
Eq. 301-13
where: n = Number of runs.
Calculate the relative standard deviation of the proposed spiked
method using Equation 301-6 where Sm is the measured mean of
the analyte spiked samples. The proposed method is unacceptable if the
RSD is greater than 50 percent.
6.3.1.2 Unspiked Samples. Calculate the standard deviation of the
unspiked values using Equation 301-13 and the relative standard
deviation of the proposed unspiked method using Equation 301-6 where
Sm is the measured mean of the analyte spiked samples. The
RSD must be less than 50 percent.
6.3.2 Bias. Calculate the numerical value of the bias using the
results from the analysis of the spiked field samples, the unspiked
field samples, and the calculated value of the spike:
B=Sm-Mm-CS
Eq. 301-14
where: B = Bias at the spike level.
Sm = Mean of the spiked samples.
Mm = Mean of the unspiked samples.
CS = Calculated value of the spiked level.
6.3.2.1 Calculate the standard deviation of the mean using the
following equation where SDs and SDu are the
standard deviations of the spiked and unspiked sample values
respectively as calculated using Equation 301-13.
[GRAPHIC] [TIFF OMITTED] TC01MY92.059
Eq. 301-15
6.3.2.2 Test the bias for statistical significance by calculating
the t-statistic using Equation 301-4 and comparing it with the critical
value of the two-sided t-distribution at the 95-percent confidence level
and n-1 degrees of freedom. This critical value is 2.201 for the eleven
degrees of freedom.
6.3.3 Calculation of a Correction Factor. If the t-test shows that
the bias is not statistically significant, use all analytical results
without correction. If the method's bias is statistically significant,
calculate the correction factor using Equation 301-5. Multiply all
analytical results by CF to obtain the final values.
7. Ruggedness Testing (Optional)
7.1 Laboratory Evaluation.
7.1.1 Ruggedness testing is a useful and cost-effective laboratory
study to determine the sensitivity of a method to certain parameters
such as sample collection rate, interferant concentration, collecting
medium temperature, or sample recovery temperature. This Section
generally discusses the principle of the ruggedness test. A more
detailed description is presented in citation 10 of Section 13.0.
7.1.2 In a ruggedness test, several variables are changed
simultaneously rather than one variable at a time. This reduces the
number of experiments required to evaluate the effect of a variable. For
example, the effect of seven variables can be determined in eight
experiments rather than 128 (W.J. Youden, Statistical Manual of the
Association of Official Analytical Chemists, Association of Official
Analytical Chemists, Washington, DC, 1975, pp. 33-36).
7.1.3 Data from ruggedness tests are helpful in extending the
applicability of a test method to different source concentrations or
source categories.
8. Procedure for Including Sample Stability in Bias and Precision
Evaluations
8.1 Sample Stability.
8.1.1 The test method being evaluated must include procedures for
sample storage and the time within which the collected samples shall be
analyzed.
8.1.2 This section identifies the procedures for including the
effect of storage time
[[Page 153]]
in bias and precision evaluations. The evaluation may be deleted if the
test method specifies a time for sample storage.
8.2 Stability Test Design. The following procedures shall be
conducted to identify the effect of storage times on analyte samples.
Store the samples according to the procedure specified in the test
method. When using the analyte spiking procedures (section 5.3), the
study should include equal numbers of spiked and unspiked samples.
8.2.1 Stack Emission Testing.
8.2.1.1 For sample container (bag or canister) and impinger sampling
systems, sections 5.1 and 5.3, analyze six of the samples at the minimum
storage time. Then analyze the same six samples at the maximum storage
time.
8.2.1.2 For sorbent and impinger sampling systems, sections 5.1 and
5.3, that require extraction or digestion, extract or digest six of the
samples at the minimum storage time and extract or digest six other
samples at the maximum storage time. Analyze an aliquot of the first six
extracts (digestates) at both the minimum and maximum storage times.
This will provide some freedom to analyze extract storage impacts.
8.2.1.3 For sorbent sampling systems, sections 5.1 and 5.3, that
require thermal desorption, analyze six samples at the minimum storage
time. Analyze another set of six samples at the maximum storage time.
8.2.1.4 For systems set up in accordance with section 5.2, the
number of samples analyzed at the minimum and maximum storage times
shall be half those collected (8 or 9). The procedures for samples
requiring extraction or digestion should parallel those in section
8.2.1.
8.2.2 Other Waste Media Testing. Analyze half of the replicate
samples at the minimum storage time and the other half at the maximum
storage time in order to identify the effect of storage times on analyte
samples.
9. Procedure for Determination of Practical Limit of Quantitation
(Optional)
9.1 Practical Limit of Quantitation.
9.1.1 The practical limit of quantitation (PLQ) is the lowest level
above which quantitative results may be obtained with an acceptable
degree of confidence. For this protocol, the PLQ is defined as 10 times
the standard deviation, so, at the blank level. This PLQ
corresponds to an uncertainty of 30 percent at the
99-percent confidence level.
9.1.2 The PLQ will be used to establish the lower limit of the test
method.
9.2 Procedure I for Estimating so. This procedure is
acceptable if the estimated PLQ is no more than twice the calculated
PLQ. If the PLQ is greater than twice the calculated PLQ use Procedure
II.
9.2.1 Estimate the PLQ and prepare a test standard at this level.
The test standard could consist of a dilution of the reference material
described in section 3.0.
9.2.2 Using the normal sampling and analytical procedures for the
method, sample and analyze this standard at least seven times in the
laboratory.
9.2.3 Calculate the standard deviation, so, of the
measured values.
9.2.4 Calculate the PLQ as 10 times so.
9.3 Procedure II for Estimating so. This procedure is to
be used if the estimated PLQ is more than twice the calculated PLQ.
9.3.1 Prepare two additional standards at concentration levels lower
than the standard used in Procedure I.
9.3.2 Sample and analyze each of these standards at least seven
times.
9.3.3 Calculate the standard deviation for each concentration level.
9.3.4 Plot the standard deviations of the three test standards as a
function of the standard concentrations.
9.3.5 Draw a best-fit straight line through the data points and
extrapolate to zero concentration. The standard deviation at zero
concentration is S0.
9.3.6 Calculate the PLQ as 10 times S0.
10.0 Field Validation Report Requirements
The field validation report shall include a discussion of the
regulatory objectives for the testing which describe the reasons for the
test, applicable emission limits, and a description of the source. In
addition, validation results shall include:
10.1 Summary of the results and calculations shown in section 6.0.
10.2 Reference material certification and value(s).
10.3 Performance audit results or letter from the reviewing
authority stating the audit material is currently not available.
10.4 Laboratory demonstration of the quality of the spiking system.
10.5 Discussion of laboratory evaluations.
10.6 Discussion of field sampling.
10.7 Discussion of sample preparations and analysis.
10.8 Storage times of samples (and extracts, if applicable).
10.9 Reasons for eliminating any results.
11. Followup Testing
The correction factor calculated in section 6.0 shall be used to
adjust the sample concentrations in all followup tests conducted at the
same source. These tests shall consist of at least three replicate
samples, and the average shall be used to determine the pollutant
concentration. The number of samples to be collected and analyzed shall
be as follows, depending on the validated method precision level:
[[Page 154]]
11.1 Validated relative standard deviation (RSD) <= 15 Percent. Three replicate samples.
11.2 Validated RSD <= 30 Percent. Six
replicate samples.
11.3 Validated RSD <= 50 Percent. Nine
replicate samples.
11.4 Equivalent method. Three replicate samples.
12. Procedure for Obtaining a Waiver
12.1 Waivers. These procedures may be waived or a less rigorous
protocol may be granted for site-specific applications. The following
are three example situations for which a waiver may be considered.
12.1.1 ``Similar'' Sources. If the test method has been validated
previously at a ``similar'' source, the procedures may be waived
provided the requester can demonstrate to the satisfaction of the
Administrator that the sources are ``similar.'' The methods's
applicability to the ``similar'' source may be demonstrated by
conducting a ruggedness test as described in section 6.0.
12.1.2 ``Documented'' Methods. In some cases, bias and precision may
have been documented through laboratory tests or protocols different
from this method. If the analyst can demonstrate to the satisfaction of
the Administrator that the bias and precision apply to a particular
application, the Administrator may waive these procedures or parts of
the procedures.
12.1.3 ``Conditional'' Test Methods. When the method has been
demonstrated to be valid at several sources, the analyst may seek a
``conditional'' method designation from the Administrator.
``Conditional'' method status provides an automatic waiver from the
procedures provided the test method is used within the stated
applicability.
12.2 Application for Waiver. In general, the requester shall provide
a thorough description of the test method, the intended application, and
results of any validation or other supporting documents. Because of the
many potential situations in which the Administrator may grant a waiver,
it is neither possible nor desirable to prescribe the exact criteria for
a waiver. At a minimum, the requester is responsible for providing the
following.
12.2.1 A clearly written test method, preferably in the format of 40
CFR part 60, appendix A Test Methods. The method must include an
applicability statement, concentration range, precision, bias
(accuracy), and time in which samples must be analyzed.
12.2.2.2 Summaries (see section 10.0) of previous validation tests
or other supporting documents. If a different procedure from that
described in this method was used, the requester shall provide
appropriate documents substantiating (to the satisfaction of the
Administrator) the bias and precision values.
12.2.2.3 Results of testing conducted with respect to sections 7.0,
8.0, and 9.0.
12.2.3 Discussion of the applicability statement and arguments for
approval of the waiver. This discussion should address as applicable the
following: Applicable regulation, emission standards, effluent
characteristics, and process operations.
12.3 Requests for Waiver. Each request shall be in writing and
signed by the analyst. Submit requests to the Director, OAQPS, Technical
Support Division, U.S. Environmental Protection Agency, Research
Triangle Park, NC 27711.
13. Bibliography
1. Albritton, J.R., G.B. Howe, S.B. Tompkins, R.K.M. Jayanty, and
C.E. Decker, 1989. Stability of Parts-Per-Million Organic Cylinder Gases
and Results of Source Test Analysis Audits, Status Report No. 11.
Environmental Protection Agency Contract 68-02-4125. Research Triangle
Institute, Research Triangle Park, NC. September.
2. DeWees, W.G., P.M. Grohse, K.K. Luk, and F.E. Butler. 1989.
Laboratory and Field Evaluation of a Methodology for Speciating Nickel
Emissions from Stationary Sources. EPA Contract 68-02-4442. Prepared for
Atmospheric Research and Environmental Assessment Laboratory, Office of
Research and Development, U.S. Environmental Protection Agency, Research
Triangle Park, NC 27711. January.
3. Keith, L.H., W. Crummer, J. Deegan Jr., R.A. Libby, J.K. Taylor,
and G. Wentler. 1983. Principles of Environmental Analysis. American
Chemical Society, Washington, DC.
4. Maxwell, E.A. 1974. Estimating variances from one or two
measurements on each sample. Amer. Statistician 28:96-97.
5. Midgett, M.R. 1977. How EPA Validates NSPS Methodology. Environ.
Sci. & Technol. 11(7):655-659.
6. Mitchell, W.J., and M.R. Midgett. 1976. Means to evaluate
performance of stationary source test methods. Environ. Sci. & Technol.
10:85-88.
7. Plackett, R.L., and J.P. Burman. 1946. The design of optimum
multifactorial experiments. Biometrika, 33:305.
8. Taylor, J.K. 1987. Quality Assurance of Chemical Measurements.
Lewis Publishers, Inc., pp. 79-81.
9. U.S. Environmental Protection Agency. 1978. Quality Assurance
Handbook for Air Pollution Measurement Systems: Volume III. Stationary
Source Specific Methods. Publication No. EPA-600/4-77-027b. Office of
Research and Development Publications, 26 West St. Clair St.,
Cincinnati, OH 45268.
10. U.S. Environmental Protection Agency. 1981. A Procedure for
Establishing Traceability of Gas Mixtures to Certain National Bureau of
Standards Standard Reference Materials. Publication No. EPA-600/7-
[[Page 155]]
81-010. Available from the U.S. EPA, Quality Assurance Division (MD-77),
Research Triangle Park, NC 27711.
11. U.S. Environmental Protection Agency. 1991. Protocol for The
Field Validation of Emission Concentrations From Stationary Sources.
Publication No. 450/4-90-015. Available from the U.S. EPA, Emission
Measurement Technical Information Center, Technical Support Division
(MD-14), Research Triangle Park, NC 27711.
12. Youdon, W.J. Statistical techniques for collaborative tests. In:
Statistical Manual of the Association of Official Analytical Chemists,
Association of Official Analytical Chemists, Washington, DC, 1975, pp.
33-36.
Method 303--Determination of Visible Emissions From By-Product Coke Oven
Batteries
Note: This method is not inclusive with respect to observer
certification. Some material is incorporated by reference from other
methods in appendix A to 40 CFR part 60. Therefore, to obtain reliable
results, persons using this method should have a thorough knowledge of
Method 9.
1.0 Scope and Application
1.1 Applicability. This method is applicable for the determination
of visible emissions (VE) from the following by-product coke oven
battery sources: charging systems during charging; doors, topside port
lids, and offtake systems on operating coke ovens; and collecting mains.
This method is also applicable for qualifying observers for visually
determining the presence of VE.
2.0 Summary of Method
2.1 A certified observer visually determines the VE from coke oven
battery sources. Certification procedures are presented. This method
does not require that opacity of emissions be determined or that
magnitude be differentiated.
3.0 Definitions
3.1 Bench means the platform structure in front of the oven doors.
3.2 By-product Coke Oven Battery means a source consisting of a
group of ovens connected by common walls, where coal undergoes
destructive distillation under positive pressure to produce coke and
coke oven gas, from which by-products are recovered.
3.3 Charge or charging period means the period of time that
commences when coal begins to flow into an oven through a topside port
and ends when the last charging port is recapped.
3.4 Charging system means an apparatus used to charge coal to a coke
oven (e.g., a larry car for wet coal charging systems).
3.5 Coke oven door means each end enclosure on the push side and the
coking side of an oven. The chuck, or leveler-bar, door is considered
part of the push side door. The coke oven door area includes the entire
area on the vertical face of a coke oven between the bench and the top
of the battery between two adjacent buck stays.
3.6 Coke side means the side of a battery from which the coke is
discharged from ovens at the end of the coking cycle.
3.7 Collecting main means any apparatus that is connected to one or
more offtake systems and that provides a passage for conveying gases
under positive pressure from the by-product coke oven battery to the by-
product recovery system.
3.8 Consecutive charges means charges observed successively,
excluding any charge during which the observer's view of the charging
system or topside ports is obscured.
3.9 Damper-off means to close off the gas passage between the coke
oven and the collecting main, with no flow of raw coke oven gas from the
collecting main into the oven or into the oven's offtake system(s).
3.10 Decarbonization period means the period of time for combusting
oven carbon that commences when the oven lids are removed from an empty
oven or when standpipe caps of an oven are opened. The period ends with
the initiation of the next charging period for that oven.
3.11 Larry car means an apparatus used to charge coal to a coke oven
with a wet coal charging system.
3.12 Log average means logarithmic average as calculated in Section
12.4.
3.13 Offtake system means any individual oven apparatus that is
stationary and provides a passage for gases from an oven to a coke oven
battery collecting main or to another oven. Offtake system components
include the standpipe and standpipe caps, goosenecks, stationary jumper
pipes, mini-standpipes, and standpipe and gooseneck connections.
3.14 Operating oven means any oven not out of operation for rebuild
or maintenance work extensive enough to require the oven to be skipped
in the charging sequence.
3.15 Oven means a chamber in the coke oven battery in which coal
undergoes destructive distillation to produce coke.
3.16 Push side means the side of the battery from which the coke is
pushed from ovens at the end of the coking cycle.
3.17 Run means the observation of visible emissions from topside
port lids, offtake systems, coke oven doors, or the charging of a single
oven in accordance with this method.
3.18 Shed means an enclosure that covers the side of the coke oven
battery, captures emissions from pushing operations and from leaking
coke oven doors on the coke side or push side of the coke oven battery,
and routes the emissions to a control device or system.
[[Page 156]]
3.19 Standpipe cap means An apparatus used to cover the opening in
the gooseneck of an offtake system.
3.20 Topside port lid means a cover, removed during charging or
decarbonizing, that is placed over the opening through which coal can be
charged into the oven of a by-product coke oven battery.
3.21 Traverse time means accumulated time for a traverse as measured
by a stopwatch. Traverse time includes time to stop and write down oven
numbers but excludes time waiting for obstructions of view to clear or
for time to walk around obstacles.
3.22 Visible Emissions or VE means any emission seen by the unaided
(except for corrective lenses) eye, excluding steam or condensing water.
4.0 Interferences [Reserved]
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of the
user of this test method to establish appropriate safety and health
practices and determine the applicability of regulatory limitations
prior to performing this test method.
5.2 Safety Training. Because coke oven batteries have hazardous
environments, the training materials and the field training (Section
10.0) shall cover the precautions required by the company to address
health and safety hazards. Special emphasis shall be given to the
Occupational Safety and Health Administration (OSHA) regulations
pertaining to exposure of coke oven workers (see Reference 3 in Section
16.0). In general, the regulation requires that special fire-retardant
clothing and respirators be worn in certain restricted areas of the coke
oven battery. The OSHA regulation also prohibits certain activities,
such as chewing gum, smoking, and eating in these areas.
6.0 Equipment and Supplies [Reserved]
7.0 Reagents and Standards [Reserved]
8.0 Sample Collection, Preservation, Transport, and Storage [Reserved]
9.0 Quality Control [Reserved]
10.0 Calibration and Standardization
Observer certification and training requirements are as follows:
10.1 Certification Procedures. This method requires only the
determination of whether VE occur and does not require the determination
of opacity levels; therefore, observer certification according to Method
9 in appendix A to part 60 of this chapter is not required to obtain
certification under this method. However, in order to receive Method 303
observer certification, the first-time observer (trainee) shall have
attended the lecture portion of the Method 9 certification course. In
addition, the trainee shall successfully complete the Method 303
training course, satisfy the field observation requirement, and
demonstrate adequate performance and sufficient knowledge of Method 303.
The Method 303 training course shall be conducted by or under the
sanction of the EPA and shall consist of classroom instruction and field
observations, and a proficiency test.
10.1.1 The classroom instruction shall familiarize the trainees with
Method 303 through lecture, written training materials, and a Method 303
demonstration video. A successful completion of the classroom portion of
the Method 303 training course shall be demonstrated by a perfect score
on a written test. If the trainee fails to answer all of the questions
correctly, the trainee may review the appropriate portion of the
training materials and retake the test.
10.1.2 The field observations shall be a minimum of 12 hours and
shall be completed before attending the Method 303 certification course.
Trainees shall observe the operation of a coke oven battery as it
pertains to Method 303, including topside operations, and shall also
practice conducting Method 303 or similar methods. During the field
observations, trainees unfamiliar with coke battery operations shall
receive instruction from an experienced coke oven observer familiar with
Method 303 or similar methods and with the operation of coke batteries.
The trainee must verify completion of at least 12 hours of field
observation prior to attending the Method 303 certification course.
10.1.3 All trainees must demonstrate proficiency in the application
of Method 303 to a panel of three certified Method 303 observers,
including an ability to differentiate coke oven emissions from
condensing water vapor and smoldering coal. Each panel member shall have
at least 120 days experience in reading visible emissions from coke
ovens. The visible emissions inspections that will satisfy the
experience requirement must be inspections of coke oven battery fugitive
emissions from the emission points subject to emission standards under
subpart L of this part (i.e., coke oven doors, topside port lids,
offtake system(s), and charging operations), using either Method 303 or
predecessor State or local test methods. A ``day's experience'' for a
particular inspection is a day on which one complete inspection was
performed for that emission point under Method 303 or a predecessor
State or local method. A ``day's experience'' does not mean 8 or 10
hours performing inspections, or any particular time expressed in
minutes or hours that may have been spent performing
[[Page 157]]
them. Thus, it would be possible for an individual to qualify as a
Method 303 panel member for some emission points, but not others (e.g.,
an individual might satisfy the experience requirement for coke oven
doors, but not topside port lids). Until November 15, 1994, the EPA may
waive the certification requirement (but not the experience requirement)
for panel members. The composition of the panel shall be approved by the
EPA. The panel shall observe the trainee in a series of training runs
and a series of certification runs. There shall be a minimum of 1
training run for doors, topside port lids, and offtake systems, and a
minimum of 5 training runs (i.e., 5 charges) for charging. During
training runs, the panel can advise the trainee on proper procedures.
There shall be a minimum of 3 certification runs for doors, topside port
lids, and offtake systems, and a minimum of 15 certification runs for
charging (i.e., 15 charges). The certifications runs shall be
unassisted. Following the certification test runs, the panel shall
approve or disapprove certification based on the trainee's performance
during the certification runs. To obtain certification, the trainee
shall demonstrate to the satisfaction of the panel a high degree of
proficiency in performing Method 303. To aid in evaluating the trainee's
performance, a checklist, provided by the EPA, will be used by the panel
members.
10.2 Observer Certification/Recertification. The coke oven observer
certification is valid for 1 year from date of issue. The observer shall
recertify annually by viewing the training video and answering all of
the questions on the certification test correctly. Every 3 years, an
observer shall be required to pass the proficiency test in Section
10.1.3 in order to be certified.
10.3 The EPA (or applicable enforcement agency) shall maintain
records reflecting a certified observer's successful completion of the
proficiency test, which shall include the completed proficiency test
checklists for the certification runs.
10.4 An owner or operator of a coke oven battery subject to subpart
L of this part may observe a training and certification program under
this section.
11.0 Procedure
11.1 Procedure for Determining VE from Charging Systems During
Charging.
11.1.1 Number of Oven Charges. Refer to Sec. 63.309(c)(1) of this
part for the number of oven charges to observe. The observer shall
observe consecutive charges. Charges that are nonconsecutive can only be
observed when necessary to replace observations terminated prior to the
completion of a charge because of visual interferences. (See Section
11.1.5).
11.1.2 Data Records. Record all the information requested at the top
of the charging system inspection sheet (Figure 303-1). For each charge,
record the identification number of the oven being charged, the
approximate beginning time of the charge, and the identification of the
larry car used for the charge.
11.1.3 Observer Position. Stand in an area or move to positions on
the topside of the coke oven battery with an unobstructed view of the
entire charging system. For wet coal charging systems or non-pipeline
coal charging systems, the observer should have an unobstructed view of
the emission points of the charging system, including larry car hoppers,
drop sleeves, and the topside ports of the oven being charged. Some
charging systems are configured so that all emission points can only be
seen from a distance of five ovens. For other batteries, distances of 8
to 12 ovens are adequate.
11.1.4 Observation. The charging period begins when coal begins to
flow into the oven and ends when the last charging port is recapped.
During the charging period, observe all of the potential sources of VE
from the entire charging system. For wet coal charging systems or non-
pipeline coal charging systems, sources of VE typically include the
larry car hoppers, drop sleeves, slide gates, and topside ports on the
oven being charged. Any VE from an open standpipe cap on the oven being
charged is included as charging VE.
11.1.4.1 Using an accumulative-type stopwatch with unit divisions of
at least 0.5 seconds, determine the total time VE are observed as
follows. Upon observing any VE emerging from any part of the charging
system, start the stopwatch. Stop the watch when VE are no longer
observed emerging, and restart the watch when VE reemerges.
11.1.4.2 When VE occur simultaneously from several points during a
charge, consider the sources as one. Time overlapping VE as continuous
VE. Time single puffs of VE only for the time it takes for the puff to
emerge from the charging system. Continue to time VE in this manner for
the entire charging period. Record the accumulated time to the nearest
0.5 second under ``Visible emissions, seconds'' on Figure 303-1.
11.1.5 Visual Interference. If fugitive VE from other sources at the
coke oven battery site (e.g., door leaks or condensing water vapor from
the coke oven wharf) prevent a clear view of the charging system during
a charge, stop the stopwatch and make an appropriate notation under
``Comments'' on Figure 303-1. Label the observation an observation of an
incomplete charge, and observe another charge to fulfill the
requirements of Section 11.1.1.
11.1.6 VE Exemptions. Do not time the following VE:
11.1.6.1 The VE from burning or smoldering coal spilled on top of
the oven, topside port lid, or larry car surfaces;
[[Page 158]]
Note: The VE from smoldering coal are generally white or gray. These
VE generally have a plume of less than 1 meter long. If the observer
cannot safely and with reasonable confidence determine that VE are from
charging, do not count them as charging emissions.
11.1.6.2 The VE from the coke oven doors or from the leveler bar; or
11.1.6.3 The VE that drift from the top of a larry car hopper if the
emissions had already been timed as VE from the drop sleeve.
Note: When the slide gate on a larry car hopper closes after the
coal has been added to the oven, the seal may not be airtight. On
occasions, a puff of smoke observed at the drop sleeves is forced past
the slide gate up into the larry car hopper and may drift from the top;
time these VE either at the drop sleeves or the hopper. If the larry car
hopper does not have a slide gate or the slide gate is left open or
partially closed, VE may quickly pass through the larry car hopper
without being observed at the drop sleeves and will appear as a strong
surge of smoke; time these as charging VE.
11.1.7 Total Time Record. Record the total time that VE were
observed for each charging operation in the appropriate column on the
charging system inspection sheet.
11.1.8 Determination of Validity of a Set of Observations. Five
charging observations (runs) obtained in accordance with this method
shall be considered a valid set of observations for that day. No
observation of an incomplete charge shall be included in a daily set of
observations that is lower than the lowest reading for a complete
charge. If both complete and incomplete charges have been observed, the
daily set of observations shall include the five highest values
observed. Four or three charging observations (runs) obtained in
accordance with this method shall be considered a valid set of charging
observations only where it is not possible to obtain five charging
observations, because visual interferences (see Section 11.1.5) or
inclement weather prevent a clear view of the charging system during
charging. However, observations from three or four charges that satisfy
these requirements shall not be considered a valid set of charging
observations if use of such set of observations in a calculation under
Section 12.4 would cause the value of A to be less than 145.
11.1.9 Log Average. For each day on which a valid daily set of
observations is obtained, calculate the daily 30-day rolling log average
of seconds of visible emissions from the charging operation for each
battery using these data and the 29 previous valid daily sets of
observations, in accordance with Section 12.4.
11.2. Procedure for Determining VE from Coke Oven Door Areas. The
intent of this procedure is to determine VE from coke oven door areas by
carefully observing the door area from a standard distance while walking
at a normal pace.
11.2.1 Number of Runs. Refer to Sec. 63.309(c)(1) of this part for
the appropriate number of runs.
11.2.2 Battery Traverse. To conduct a battery traverse, walk the
length of the battery on the outside of the pusher machine and quench
car tracks at a steady, normal walking pace, pausing to make appropriate
entries on the door area inspection sheet (Figure 303-2). A single test
run consists of two timed traverses, one for the coke side and one for
the push side. The walking pace shall be such that the duration of the
traverse does not exceed an average of 4 seconds per oven door,
excluding time spent moving around stationary obstructions or waiting
for other obstructions to move from positions blocking the view of a
series of doors. Extra time is allowed for each leak (a maximum of 10
additional seconds for each leaking door) for the observer to make the
proper notation. A walking pace of 3 seconds per oven door has been
found to be typical. Record the actual traverse time with a stopwatch.
11.2.2.1 Include in the traverse time only the time spent observing
the doors and recording door leaks. To measure actual traverse time, use
an accumulative-type stopwatch with unit divisions of 0.5 seconds or
less. Exclude interruptions to the traverse and time required for the
observer to move to positions where the view of the battery is
unobstructed, or for obstructions, such as the door machine, to move
from positions blocking the view of a series of doors.
11.2.2.2 Various situations may arise that will prevent the observer
from viewing a door or a series of doors. Prior to the door inspection,
the owner or operator may elect to temporarily suspend charging
operations for the duration of the inspection, so that all of the doors
can be viewed by the observer. The observer has two options for dealing
with obstructions to view: (a) Stop the stopwatch and wait for the
equipment to move or the fugitive emissions to dissipate before
completing the traverse; or (b) stop the stopwatch, skip the affected
ovens, and move to an unobstructed position to continue the traverse.
Restart the stopwatch and continue the traverse. After the completion of
the traverse, if the equipment has moved or the fugitive emissions have
dissipated, inspect the affected doors. If the equipment is still
preventing the observer from viewing the doors, then the affected doors
may be counted as not observed. If option (b) is used because of doors
blocked by machines during charging operations, then, of the affected
doors, exclude the door from the most recently charged oven from the
inspection.
[[Page 159]]
Record the oven numbers and make an appropriate notation under
``Comments'' on the door area inspection sheet (Figure 303-2).
11.2.2.3 When batteries have sheds to control emissions, conduct the
inspection from outside the shed unless the doors cannot be adequately
viewed. In this case, conduct the inspection from the bench. Be aware of
special safety considerations pertinent to walking on the bench and
follow the instructions of company personnel on the required equipment
and procedures. If possible, conduct the bench traverse whenever the
bench is clear of the door machine and hot coke guide.
11.2.3 Observations. Record all the information requested at the top
of the door area inspection sheet (Figure 303-2), including the number
of non-operating ovens. Record the clock time at the start of the
traverse on each side of the battery. Record which side is being
inspected (i.e., coke side or push side). Other information may be
recorded at the discretion of the observer, such as the location of the
leak (e.g., top of the door, chuck door, etc.), the reason for any
interruption of the traverse, or the position of the sun relative to the
battery and sky conditions (e.g., overcast, partly sunny, etc.).
11.2.3.1 Begin the test run by starting the stopwatch and traversing
either the coke side or the push side of the battery. After completing
one side, stop the watch. Complete this procedure on the other side. If
inspecting more than one battery, the observer may view the push sides
and the coke sides sequentially.
11.2.3.2 During the traverse, look around the entire perimeter of
each oven door. The door is considered leaking if VE are detected in the
coke oven door area. The coke oven door area includes the entire area on
the vertical face of a coke oven between the bench and the top of the
battery between two adjacent buck stays (e.g., the oven door, chuck
door, between the masonry brick, buck stay or jamb, or other sources).
Record the oven number and make the appropriate notation on the door
area inspection sheet (Figure 303-2).
Note: Multiple VE from the same door area (e.g., VE from both the
chuck door and the push side door) are counted as only one emitting
door, not as multiple emitting doors.
11.2.3.3 Do not record the following sources as door area VE:
11.2.3.3.1 VE from ovens with doors removed. Record the oven number
and make an appropriate notation under ``Comments;''
11.2.3.3.2 VE from ovens taken out of service. The owner or operator
shall notify the observer as to which ovens are out of service. Record
the oven number and make an appropriate notation under ``Comments;'' or
11.2.3.3.3 VE from hot coke that has been spilled on the bench as a
result of pushing.
11.2.4 Criteria for Acceptance. After completing the run, calculate
the maximum time allowed to observe the ovens using the equation in
Section 12.2. If the total traverse time exceeds T, void the run, and
conduct another run to satisfy the requirements of Sec. 63.309(c)(1) of
this part.
11.2.5 Percent Leaking Doors. For each day on which a valid
observation is obtained, calculate the daily 30-day rolling average for
each battery using these data and the 29 previous valid daily
observations, in accordance with Section 12.5.
11.3 Procedure for Determining VE from Topside Port Lids and Offtake
Systems.
11.3.1 Number of Runs. Refer to Sec. 63.309(c)(1) of this part for
the number of runs to be conducted. Simultaneous runs or separate runs
for the topside port lids and offtake systems may be conducted.
11.3.2 Battery Traverse. To conduct a topside traverse of the
battery, walk the length of the battery at a steady, normal walking
pace, pausing only to make appropriate entries on the topside inspection
sheet (Figure 303-3). The walking pace shall not exceed an average rate
of 4 seconds per oven, excluding time spent moving around stationary
obstructions or waiting for other obstructions to move from positions
blocking the view. Extra time is allowed for each leak for the observer
to make the proper notation. A walking pace of 3 seconds per oven is
typical. Record the actual traverse time with a stopwatch.
11.3.3 Topside Port Lid Observations. To observe lids of the ovens
involved in the charging operation, the observer shall wait to view the
lids until approximately 5 minutes after the completion of the charge.
Record all the information requested on the topside inspection sheet
(Figure 303-3). Record the clock time when traverses begin and end. If
the observer's view is obstructed during the traverse (e.g., steam from
the coke wharf, larry car, etc.), follow the guidelines given in Section
11.2.2.2.
11.3.3.1 To perform a test run, conduct a single traverse on the
topside of the battery. The observer shall walk near the center of the
battery but may deviate from this path to avoid safety hazards (such as
open or closed charging ports, luting buckets, lid removal bars, and
topside port lids that have been removed) and any other obstacles. Upon
noting VE from the topside port lid(s) of an oven, record the oven
number and port number, then resume the traverse. If any oven is
dampered-off from the collecting main for decarbonization, note this
under ``Comments'' for that particular oven.
Note: Count the number of topside ports, not the number of points,
exhibiting VE, i.e., if a topside port has several points of VE, count
this as one port exhibiting VE.
[[Page 160]]
11.3.3.2 Do not count the following as topside port lid VE:
11.3.3.2.1 VE from between the brickwork and oven lid casing or VE
from cracks in the oven brickwork. Note these VE under ``Comments;''
11.3.3.2.2 VE from topside ports involved in a charging operation.
Record the oven number, and make an appropriate notation (e.g., not
observed because ports open for charging) under ``Comments;''
11.3.3.2.3 Topside ports having maintenance work done. Record the
oven number and make an appropriate notation under ``Comments;'' or
11.3.3.2.4 Condensing water from wet-sealing material. Ports with
only visible condensing water from wet-sealing material are counted as
observed but not as having VE.
11.3.3.2.5 Visible emissions from the flue inspection ports and
caps.
11.3.4 Offtake Systems Observations. To perform a test run, traverse
the battery as in Section 11.3.3.1. Look ahead and back two to four
ovens to get a clear view of the entire offtake system for each oven.
Consider visible emissions from the following points as offtake system
VE: (a) the flange between the gooseneck and collecting main
(``saddle''), (b) the junction point of the standpipe and oven
(``standpipe base''), (c) the other parts of the offtake system (e.g.,
the standpipe cap), and (d) the junction points with ovens and flanges
of jumper pipes.
11.3.4.1 Do not stray from the traverse line in order to get a
``closer look'' at any part of the offtake system unless it is to
distinguish leaks from interferences from other sources or to avoid
obstacles.
11.3.4.2 If the centerline does not provide a clear view of the
entire offtake system for each oven (e.g., when standpipes are longer
than 15 feet), the observer may conduct the traverse farther from
(rather than closer to) the offtake systems.
11.3.4.3 Upon noting a leak from an offtake system during a
traverse, record the oven number. Resume the traverse. If the oven is
dampered-off from the collecting main for decarbonization and VE are
observed, note this under ``Comments'' for that particular oven.
11.3.4.4 If any part or parts of an offtake system have VE, count it
as one emitting offtake system. Each stationary jumper pipe is
considered a single offtake system.
11.3.4.5 Do not count standpipe caps open for a decarbonization
period or standpipes of an oven being charged as source of offtake
system VE. Record the oven number and write ``Not observed'' and the
reason (i.e., decarb or charging) under ``Comments.''
Note: VE from open standpipes of an oven being charged count as
charging emissions. All VE from closed standpipe caps count as offtake
leaks.
11.3.5 Criteria for Acceptance. After completing the run (allow 2
traverses for batteries with double mains), calculate the maximum time
allowed to observe the topside port lids and/or offtake systems using
the equation in Section 12.3. If the total traverse time exceeds T, void
the run and conduct another run to satisfy the requirements of Sec.
63.309(c)(1) of this part.
11.3.6 In determining the percent leaking topside port lids and
percent leaking offtake systems, do not include topside port lids or
offtake systems with VE from the following ovens:
11.3.6.1 Empty ovens, including ovens undergoing maintenance, which
are properly dampered off from the main.
11.3.6.2 Ovens being charged or being pushed.
11.3.6.3 Up to 3 full ovens that have been dampered off from the
main prior to pushing.
11.3.6.4 Up to 3 additional full ovens in the pushing sequence that
have been dampered off from the main for offtake system cleaning, for
decarbonization, for safety reasons, or when a charging/pushing schedule
involves widely separated ovens (e.g., a Marquard system); or that have
been dampered off from the main for maintenance near the end of the
coking cycle. Examples of reasons that ovens are dampered off for safety
reasons are to avoid exposing workers in areas with insufficient
clearance between standpipes and the larry car, or in areas where
workers could be exposed to flames or hot gases from open standpipes,
and to avoid the potential for removing a door on an oven that is not
dampered off from the main.
11.3.7 Percent Leaking Topside Port Lids and Offtake Systems. For
each day on which a valid observation is obtained, calculate the daily
30-day rolling average for each battery using these data and the 29
previous valid daily observations, in accordance with Sections 12.6 and
12.7.
11.4 Procedure for Determining VE from Collecting Mains.
11.4.1 Traverse. To perform a test run, traverse both the collecting
main catwalk and the battery topside along the side closest to the
collecting main. If the battery has a double main, conduct two sets of
traverses for each run, i.e., one set for each main.
11.4.2 Data Recording. Upon noting VE from any portion of a
collection main, identify the source and approximate location of the
source of VE and record the time under ``Collecting main'' on Figure
303-3; then resume the traverse.
11.4.3 Collecting Main Pressure Check. After the completion of the
door traverse, the topside port lids, and offtake systems, compare the
collecting main pressure during the inspection to the collecting main
pressure during the previous 8 to 24 hours. Record the following: (a)
the pressure during inspection, (b) presence of pressure deviation
[[Page 161]]
from normal operations, and (c) the explanation for any pressure
deviation from normal operations, if any, offered by the operators. The
owner or operator of the coke battery shall maintain the pressure
recording equipment and conduct the quality assurance/quality control
(QA/QC) necessary to ensure reliable pressure readings and shall keep
the QA/QC records for at least 6 months. The observer may periodically
check the QA/QC records to determine their completeness. The owner or
operator shall provide access to the records within 1 hour of an
observer's request.
12.0 Data Analysis and Calculations
12.1 Nomenclature.
A = 150 or the number of valid observations (runs). The value of A shall
not be less than 145, except for purposes of determinations under Sec.
63.306(c) (work practice plan implementation) or Sec. 63.306(d) (work
practice plan revisions) of this part. No set of observations shall be
considered valid for such a recalculation that otherwise would not be
considered a valid set of observations for a calculation under this
paragraph.
Di = Number of doors on non-operating ovens.
Dno = Number of doors not observed.
Dob = Total number of doors observed on operating ovens.
Dt = Total number of oven doors on the battery.
e = 2.72
J = Number of stationary jumper pipes.
L = Number of doors with VE.
Lb = Yard-equivalent reading.
Ls = Number of doors with VE observed from the bench under
sheds.
Ly = Number of doors with VE observed from the yard.
Ly = Number of doors with VE observed from the yard on the
push side.
ln = Natural logarithm.
N = Total number of ovens in the battery.
Ni = Total number of inoperable ovens.
PNO = Number of ports not observed.
Povn = Number of ports per oven.
PVE = Number of topside port lids with VE.
PLD = Percent leaking coke oven doors for the test run.
PLL = Percent leaking topside port lids for the run.
PLO = Percent leaking offtake systems.
T = Total time allowed for traverse, seconds.
Tovn = Number of offtake systems (excluding jumper pipes) per
oven.
TNO = Number of offtake systems not observed.
TVE = Number of offtake systems with VE.
Xi = Seconds of VE during the ith charge.
Z = Number of topside port lids or offtake systems with VE.
12.2 Criteria for Acceptance for VE Determinations from Coke Oven
Door Areas. After completing the run, calculate the maximum time allowed
to observe the ovens using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.535
12.3 Criteria for Acceptance for VE Determinations from Topside Port
Lids and Offtake Systems. After completing the run (allow 2 traverses
for batteries with double mains), calculate the maximum time allowed to
observe the topside port lids and/or offtake systems by the following
equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.536
12.4 Average Duration of VE from Charging Operations. Use Equation
303-3 to calculate the daily 30-day rolling log average of seconds of
visible emissions from the charging operation for each battery using
these current day's observations and the 29 previous valid daily sets of
observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.537
12.5 Percent Leaking Doors (PLD). Determine the total number of
doors for which observations were made on the coke oven battery as
follows:
[[Page 162]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.538
12.5.1 For each test run (one run includes both the coke side and
the push side traverses), sum the number of doors with door area VE. For
batteries subject to an approved alternative standard under Sec. 63.305
of this part, calculate the push side and the coke side PLD separately.
12.5.2 Calculate percent leaking doors by using Equation 303-5:
[GRAPHIC] [TIFF OMITTED] TR17OC00.539
12.5.3 When traverses are conducted from the bench under sheds,
calculate the coke side and the push side separately. Use Equation 303-6
to calculate a yard-equivalent reading:
[GRAPHIC] [TIFF OMITTED] TR17OC00.540
If Lb is less than zero, use zero for Lb in
Equation 303-7 in the calculation of PLD.
12.5.3.1 Use Equation 303-7 to calculate PLD:
[GRAPHIC] [TIFF OMITTED] TR17OC00.541
Round off PLD to the nearest hundredth of 1 percent and record as the
percent leaking coke oven doors for the run.
12.5.3.2 Average Percent Leaking Doors. Use Equation 303-8 to
calculate the daily 30-day rolling average percent leaking doors for
each battery using these current day's observations and the 29 previous
valid daily sets of observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.542
12.6 Topside Port Lids. Determine the percent leaking topside port
lids for each run as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.543
12.6.1 Round off this percentage to the nearest hundredth of 1
percent and record this percentage as the percent leaking topside port
lids for the run.
[[Page 163]]
12.6.2 Average Percent Leaking Topside Port Lids. Use Equation 303-
10 to calculate the daily 30-day rolling average percent leaking topside
port lids for each battery using these current day's observations and
the 29 previous valid daily sets of observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.544
12.7 Offtake Systems. Determine the percent leaking offtake systems
for the run as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.545
12.7.1 Round off this percentage to the nearest hundredth of 1
percent and record this percentage as the percent leaking offtake
systems for the run.
12.7.2 Average Percent Leaking Offtake Systems. Use Equation 303-12
to calculate the daily 30-day rolling average percent leaking offtake
systems for each battery using these current day's observations and the
29 previous valid daily sets of observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.546
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 References.
1. Missan, R., and A. Stein. Guidelines for Evaluation of Visible
Emissions Certification, Field Procedures, Legal Aspects, and Background
Material. U.S. Environmental Protection Agency. EPA Publication No. EPA-
340/1-75-007. April 1975.
2. Wohlschlegel, P., and D. E. Wagoner. Guideline for Development of
a Quality Assurance Program: Volume IX--Visual Determination of Opacity
Emission from Stationary Sources. U.S. Environmental Protection Agency.
EPA Publication No. EPA-650/4-74-005i. November 1975.
3. U.S. Occupational Safety and Health Administration. Code of
Federal Regulations. Title 29, Chapter XVII, Section 1910.1029(g).
Washington, D.C. Government Printing Office. July 1, 1990.
4. U.S. Environmental Protection Agency. National Emission Standards
for Hazardous Air Pollutants; Coke Oven Emissions from Wet-Coal Charged
By-Product Coke Oven Batteries; Proposed Rule and Notice of Public
Hearing. Washington, D.C. Federal Register. Vol. 52, No. 78 (13586).
April 23, 1987.
17.0 Tables, Diagrams, Flowcharts, and Validation Data
Company name:___________________________________________________________
Battery no.: ------ Date: ------ Run no.: ------
City, State:____________________________________________________________
Observer name:__________________________________________________________
Company representative(s):______________________________________________
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Visible
Charge No. Oven No. Clock time emissions, Comments
seconds
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[[Page 164]]
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Figure 303-1. Charging System Inspection
Company name:___________________________________________________________
Battery no.:____________________________________________________________
Date:___________________________________________________________________
City, State:____________________________________________________________
Total no. of ovens in battery:__________________________________________
Observer name:__________________________________________________________
Certification expiration date:__________________________________________
Inoperable ovens:_______________________________________________________
Company representative(s):______________________________________________
Traverse time CS:_______________________________________________________
Traverse time PS:_______________________________________________________
Valid run (Y or N):_____________________________________________________
----------------------------------------------------------------------------------------------------------------
Comments (No. of blocked doors,
Time traverse started/completed PS/CS Door No. interruptions to traverse, etc.)
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[[Page 165]]
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Figure 303-2. Door Area Inspection.
Company name:___________________________________________________________
Battery no.:____________________________________________________________
Date:___________________________________________________________________
City, State:____________________________________________________________
Total no. of ovens in battery:__________________________________________
Observer name:__________________________________________________________
Certification expiration date:__________________________________________
Inoperable ovens:_______________________________________________________
Company representative(s):______________________________________________
Total no. of lids:______________________________________________________
Total no. of offtakes:__________________________________________________
Total no. of jumper pipes:______________________________________________
Ovens not observed:_____________________________________________________
Total traverse time:____________________________________________________
Valid run (Y or N):_____________________________________________________
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Type of Inspection
Time traverse started/completed (lids, offtakes, Location of VE (Oven / Comments
collecting main) Port )
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[[Page 166]]
Figure 303-3. Topside Inspection
Method 303A--Determination of Visible Emissions From Nonrecovery Coke
Oven Batteries
Note: This method does not include all of the specifications
pertaining to observer certification. Some material is incorporated by
reference from other methods in this part and in appendix A to 40 CFR
Part 60. Therefore, to obtain reliable results, persons using this
method should have a thorough knowledge of Method 9 and Method 303.
1.0 Scope and Application
1.1 Applicability. This method is applicable for the determination
of visible emissions (VE) from leaking doors at nonrecovery coke oven
batteries.
2.0 Summary of Method
2.1 A certified observer visually determines the VE from coke oven
battery sources while walking at a normal pace. This method does not
require that opacity of emissions be determined or that magnitude be
differentiated.
3.0 Definitions
3.1 Bench means the platform structure in front of the oven doors.
3.2 Coke oven door means each end enclosure on the push side and the
coking side of an oven.
3.3 Coke side means the side of a battery from which the coke is
discharged from ovens at the end of the coking cycle.
3.4 Nonrecovery coke oven battery means a source consisting of a
group of ovens connected by common walls and operated as a unit, where
coal undergoes destructive distillation under negative pressure to
produce coke, and which is designed for the combustion of coke oven gas
from which by-products are not recovered.
3.5 Operating oven means any oven not out of operation for rebuild
or maintenance work extensive enough to require the oven to be skipped
in the charging sequence.
3.6 Oven means a chamber in the coke oven battery in which coal
undergoes destructive distillation to produce coke.
3.7 Push side means the side of the battery from which the coke is
pushed from ovens at the end of the coking cycle.
3.8 Run means the observation of visible emissions from coke oven
doors in accordance with this method.
3.9 Shed means an enclosure that covers the side of the coke oven
battery, captures emissions from pushing operations and from leaking
coke oven doors on the coke side or push side of the coke oven battery,
and routes the emissions to a control device or system.
3.10 Traverse time means accumulated time for a traverse as measured
by a stopwatch. Traverse time includes time to stop and write down oven
numbers but excludes time waiting for obstructions of view to clear or
for time to walk around obstacles.
3.11 Visible Emissions or VE means any emission seen by the unaided
(except for corrective lenses) eye, excluding steam or condensing water.
4.0 Interferences [Reserved]
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of the
user of this test method to establish appropriate safety and health
practices and determine the applicability of regulatory limitations
prior to performing this test method.
5.2 Safety Training. Because coke oven batteries have hazardous
environments, the training materials and the field training (Section
10.0) shall cover the precautions required by the company to address
health and safety hazards. Special emphasis shall be given to the
Occupational Safety and Health Administration (OSHA) regulations
pertaining to exposure of coke oven workers (see Reference 3 in Section
16.0). In general, the regulation requires that special fire-retardant
clothing and respirators be worn in certain restricted areas of the coke
oven battery. The OSHA regulation also prohibits certain activities,
such as chewing gum, smoking, and eating in these areas.
6.0 Equipment and Supplies [Reserved]
7.0 Reagents and Standards [Reserved]
8.0 Sample Collection, Preservation, Transport, and Storage [Reserved]
9.0 Quality Control [Reserved]
10.0 Calibration and Standardization.
10.1 Training. This method requires only the determination of
whether VE occur and does not require the determination of opacity
levels; therefore, observer certification according to Method 9 in
Appendix A to Part 60 is not required. However, the first-time observer
(trainee) shall have attended the lecture portion of the Method 9
certification course. Furthermore, before conducting any VE
observations, an observer shall become familiar with nonrecovery coke
oven battery operations and with this test method by observing for a
minimum of 4 hours the operation of a nonrecovery coke oven battery in
the presence of personnel experienced in performing Method 303
assessments.
[[Page 167]]
11.0 Procedure
The intent of this procedure is to determine VE from coke oven door
areas by carefully observing the door area while walking at a normal
pace.
11.1 Number of Runs. Refer to Sec. 63.309(c)(1) of this part for
the appropriate number of runs.
11.2 Battery Traverse. To conduct a battery traverse, walk the
length of the battery on the outside of the pusher machine and quench
car tracks at a steady, normal walking pace, pausing to make appropriate
entries on the door area inspection sheet (Figure 303A-1). The walking
pace shall be such that the duration of the traverse does not exceed an
average of 4 seconds per oven door, excluding time spent moving around
stationary obstructions or waiting for other obstructions to move from
positions blocking the view of a series of doors. Extra time is allowed
for each leak (a maximum of 10 additional seconds for each leaking door)
for the observer to make the proper notation. A walking pace of 3
seconds per oven door has been found to be typical. Record the actual
traverse time with a stopwatch. A single test run consists of two timed
traverses, one for the coke side and one for the push side.
11.2.1 Various situations may arise that will prevent the observer
from viewing a door or a series of doors. The observer has two options
for dealing with obstructions to view: (a) Wait for the equipment to
move or the fugitive emissions to dissipate before completing the
traverse; or (b) skip the affected ovens and move to an unobstructed
position to continue the traverse. Continue the traverse. After the
completion of the traverse, if the equipment has moved or the fugitive
emissions have dissipated, complete the traverse by inspecting the
affected doors. Record the oven numbers and make an appropriate notation
under ``Comments'' on the door area inspection sheet (Figure 303A-1).
Note: Extra time incurred for handling obstructions is not counted
in the traverse time.
11.2.2 When batteries have sheds to control pushing emissions,
conduct the inspection from outside the shed, if the shed allows such
observations, or from the bench. Be aware of special safety
considerations pertinent to walking on the bench and follow the
instructions of company personnel on the required equipment and
operations procedures. If possible, conduct the bench traverse whenever
the bench is clear of the door machine and hot coke guide.
11.3 Observations. Record all the information requested at the top
of the door area inspection sheet (Figure 303A-1), including the number
of non-operating ovens. Record which side is being inspected, i.e., coke
side or push side. Other information may be recorded at the discretion
of the observer, such as the location of the leak (e.g., top of the
door), the reason for any interruption of the traverse, or the position
of the sun relative to the battery and sky conditions (e.g., overcast,
partly sunny, etc.).
11.3.1 Begin the test run by traversing either the coke side or the
push side of the battery. After completing one side, traverse the other
side.
11.3.2 During the traverse, look around the entire perimeter of each
oven door. The door is considered leaking if VE are detected in the coke
oven door area. The coke oven door area includes the entire area on the
vertical face of a coke oven between the bench and the top of the
battery and the adjacent doors on both sides. Record the oven number and
make the appropriate notation on the door area inspection sheet (Figure
303A-1).
11.3.3 Do not record the following sources as door area VE:
11.3.3.1 VE from ovens with doors removed. Record the oven number
and make an appropriate notation under ``Comments'';
11.3.3.2 VE from ovens where maintenance work is being conducted.
Record the oven number and make an appropriate notation under
``Comments''; or
11.3.3.3 VE from hot coke that has been spilled on the bench as a
result of pushing.
12.0 Data Analysis and Calculations
Same as Method 303, Section 12.1, 12.2, 12.3, 12.4, and 12.5.
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 References
Same as Method 303, Section 16.0.
17.0 Tables, Diagrams, Flowcharts, and Validation Data
Company name:___________________________________________________________
Battery no.:____________________________________________________________
Date:___________________________________________________________________
City, State:____________________________________________________________
Total no. of ovens in battery:__________________________________________
Observer name:__________________________________________________________
Certification expiration date:__________________________________________
[[Page 168]]
Inoperable ovens:_______________________________________________________
Company representative(s):______________________________________________
Traverse time CS:_______________________________________________________
Traverse time PS:_______________________________________________________
Valid run (Y or N):_____________________________________________________
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Comments (No. of blocked doors,
Time traverse started/completed PS/CS Door No. interruptions to traverse, etc.)
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Figure 303A-1. Door Area Inspection
Method 304A: Determination of Biodegradation Rates of Organic Compounds
(Vent Option)
1.0 Scope and Application
1.1 Applicability. This method is applicable for the determination
of biodegradation rates of organic compounds in an activated sludge
process. The test method is designed to evaluate the ability of an
aerobic biological reaction system to degrade or destroy specific
components in waste streams. The method may also be used to determine
the effects of changes in wastewater composition on operation. The
biodegradation rates determined by utilizing this method are not
representative of a full-scale system. The rates measured by this method
shall be used in conjunction with the procedures listed in appendix C of
this part to calculate the fraction emitted to the air versus the
fraction biodegraded.
2.0 Summary of Method
2.1 A self-contained benchtop bioreactor system is assembled in the
laboratory. A sample of mixed liquor is added and the waste stream is
then fed continuously. The benchtop bioreactor is operated under
conditions nearly identical to the target full-scale activated sludge
process. Bioreactor temperature, dissolved oxygen concentration, average
residence time in the reactor, waste composition, biomass concentration,
and biomass composition of the full-scale process are the parameters
which are duplicated in the benchtop bioreactor. Biomass shall be
removed from the target full-scale activated sludge unit and held for no
more than 4 hours prior to use in the benchtop bioreactor. If
antifoaming agents are used in the full-scale system, they shall also be
used in the benchtop bioreactor. The feed flowing into and the effluent
exiting the benchtop bioreactor are analyzed to determine the
[[Page 169]]
biodegradation rates of the target compounds. The flow rate of the exit
vent is used to calculate the concentration of target compounds
(utilizing Henry's law) in the exit gas stream. If Henry's law constants
for the compounds of interest are not known, this method cannot be used
in the determination of the biodegradation rate and Method 304B is the
suggested method. The choice of analytical methodology for measuring the
compounds of interest at the inlet and outlet to the benchtop bioreactor
are left to the discretion of the source, except where validated methods
are available.
3.0 Definitions [Reserved]
4.0 Interferences [Reserved]
5.0 Safety
5.1 If explosive gases are produced as a byproduct of biodegradation
and could realistically pose a hazard, closely monitor headspace
concentration of these gases to ensure laboratory safety. Placement of
the benchtop bioreactor system inside a laboratory hood is recommended
regardless of byproducts produced.
6.0. Equipment and Supplies
Note: Figure 304A-1 illustrates a typical laboratory apparatus used
to measure biodegradation rates. While the following description refers
to Figure 304A-1, the EPA recognizes that alternative reactor
configurations, such as alternative reactor shapes and locations of
probes and the feed inlet, will also meet the intent of this method.
Ensure that the benchtop bioreactor system is self-contained and
isolated from the atmosphere (except for the exit vent stream) by leak-
checking fittings, tubing, etc.
6.1 Benchtop Bioreactor. The biological reaction is conducted in a
biological oxidation reactor of at least 6 liters capacity. The benchtop
bioreactor is sealed and equipped with internal probes for controlling
and monitoring dissolved oxygen and internal temperature. The top of the
reactor is equipped for aerators, gas flow ports, and instrumentation
(while ensuring that no leaks to the atmosphere exist around the
fittings).
6.2 Aeration gas. Aeration gas is added to the benchtop bioreactor
through three diffusers, which are glass tubes that extend to the bottom
fifth of the reactor depth. A pure oxygen pressurized cylinder is
recommended in order to maintain the specified oxygen concentration.
Install a blower (e.g., Diaphragm Type, 15 SCFH capacity) to blow the
aeration gas into the reactor diffusers. Measure the aeration gas flow
rate with a rotameter (e.g., 0-15 SCFH recommended). The aeration gas
will rise through the benchtop bioreactor, dissolving oxygen into the
mixture in the process. The aeration gas must provide sufficient
agitation to keep the solids in suspension. Provide an exit for the
aeration gas from the top flange of the benchtop bioreactor through a
water-cooled (e.g., Allihn-type) vertical condenser. Install the
condenser through a gas-tight fitting in the benchtop bioreactor
closure. Install a splitter which directs a portion of the gas to an
exit vent and the rest of the gas through an air recycle pump back to
the benchtop bioreactor. Monitor and record the flow rate through the
exit vent at least 3 times per day throughout the day.
6.3 Wastewater Feed. Supply the wastewater feed to the benchtop
bioreactor in a collapsible low-density polyethylene container or
collapsible liner in a container (e.g., 20 L) equipped with a spigot cap
(collapsible containers or liners of other material may be required due
to the permeability of some volatile compounds through polyethylene).
Obtain the wastewater feed by sampling the wastewater feed in the target
process. A representative sample of wastewater shall be obtained from
the piping leading to the aeration tank. This sample may be obtained
from existing sampling valves at the discharge of the wastewater feed
pump, or collected from a pipe discharging to the aeration tank, or by
pumping from a well-mixed equalization tank upstream from the aeration
tank. Alternatively, wastewater can be pumped continuously to the
laboratory apparatus from a bleed stream taken from the equalization
tank of the full-scale treatment system.
6.3.1 Refrigeration System. Keep the wastewater feed cool by ice or
by refrigeration to 4 [deg]C. If using a bleed stream from the
equalization tank, refrigeration is not required if the residence time
in the bleed stream is less than five minutes.
6.3.2 Wastewater Feed Pump. The wastewater is pumped from the
refrigerated container using a variable-speed peristaltic pump drive
equipped with a peristaltic pump head. Add the feed solution to the
benchtop bioreactor through a fitting on the top flange. Determine the
rate of feed addition to provide a retention time in the benchtop
bioreactor that is numerically equivalent to the retention time in the
full-scale system. The wastewater shall be fed at a rate sufficient to
achieve 90 to 100 percent of the full-scale system residence time.
6.3.3 Treated wastewater feed. The benchtop bioreactor effluent
exits at the bottom of the reactor through a tube and proceeds to the
clarifier.
6.4 Clarifier. The effluent flows to a separate closed clarifier
that allows separation of biomass and effluent (e.g., 2-liter pear-
shaped glass separatory funnel, modified by removing the stopcock and
adding a 25-mm OD glass tube at the bottom). Benchtop bioreactor
effluent enters the clarifier through a tube inserted to a depth of 0.08
m (3 in.) through a stopper at the top of the clarifier.
[[Page 170]]
System effluent flows from a tube inserted through the stopper at the
top of the clarifier to a drain (or sample bottle when sampling). The
underflow from the clarifier leaves from the glass tube at the bottom of
the clarifier. Flexible tubing connects this fitting to the sludge
recycle pump. This pump is coupled to a variable speed pump drive. The
discharge from this pump is returned through a tube inserted in a port
on the side of the benchtop bioreactor. An additional port is provided
near the bottom of the benchtop bioreactor for sampling the reactor
contents. The mixed liquor from the benchtop bioreactor flows into the
center of the clarifier. The clarified system effluent separates from
the biomass and flows through an exit near the top of the clarifier.
There shall be no headspace in the clarifier.
6.5 Temperature Control Apparatus. Capable of maintaining the system
at a temperature equal to the temperature of the full-scale system. The
average temperature should be maintained within 2
[deg]C of the set point.
6.5.1 Temperature Monitoring Device. A resistance type temperature
probe or a thermocouple connected to a temperature readout with a
resolution of 0.1 [deg]C or better.
6.5.2 Benchtop Bioreactor Heater. The heater is connected to the
temperature control device.
6.6 Oxygen Control System. Maintain the dissolved oxygen
concentration at the levels present in the full-scale system. Target
full-scale activated sludge systems with dissolved oxygen concentration
below 2 mg/L are required to maintain the dissolved oxygen concentration
in the benchtop ioreactor within 0.5 mg/L of the target dissolved oxygen
level. Target full-scale activated sludge systems with dissolved oxygen
concentration above 2 mg/L are required to maintain the dissolved oxygen
concentration in the benchtop bioreactor within 1.5 mg/L of the target
dissolved oxygen concentration; however, for target full-scale activated
sludge systems with dissolved oxygen concentrations above 2 mg/L, the
dissolved oxygen concentration in the benchtop bioreactor may not drop
below 1.5 mg/L. If the benchtop bioreactor is outside the control range,
the dissolved oxygen is noted and the reactor operation is adjusted.
6.6.1 Dissolved Oxygen Monitor. Dissolved oxygen is monitored with a
polarographic probe (gas permeable membrane) connected to a dissolved
oxygen meter (e.g., 0 to 15 mg/L, 0 to 50 [deg]C).
6.6.2 Benchtop Bioreactor Pressure Monitor. The benchtop bioreactor
pressure is monitored through a port in the top flange of the reactor.
This is connected to a gauge control with a span of 13-cm water vacuum
to 13-cm water pressure or better. A relay is activated when the vacuum
exceeds an adjustable setpoint which opens a solenoid valve (normally
closed), admitting oxygen to the system. The vacuum setpoint controlling
oxygen addition to the system shall be set at approximately 2.5 0.5 cm water and maintained at this setting except
during brief periods when the dissolved oxygen concentration is
adjusted.
6.7 Connecting Tubing. All connecting tubing shall be Teflon or
equivalent in impermeability. The only exception to this specification
is the tubing directly inside the pump head of the wastewater feed pump,
which may be Viton, Silicone or another type of flexible tubing.
Note: Mention of trade names or products does not constitute
endorsement by the U.S. Environmental Protection Agency.
7.0 Reagents and Standards
7.1 Wastewater. Obtain a representative sample of wastewater at the
inlet to the full-scale treatment plant if there is an existing full-
scale treatment plant (see section 6.3). If there is no existing full-
scale treatment plant, obtain the wastewater sample as close to the
point of determination as possible. Collect the sample by pumping the
wastewater into the 20-L collapsible container. The loss of volatiles
shall be minimized from the wastewater by collapsing the container
before filling, by minimizing the time of filling, and by avoiding a
headspace in the container after filling. If the wastewater requires the
addition of nutrients to support the biomass growth and maintain biomass
characteristics, those nutrients are added and mixed with the container
contents after the container is filled.
7.2 Biomass. Obtain the biomass or activated sludge used for rate
constant determination in the bench-scale process from the existing
full-scale process or from a representative biomass culture (e.g.,
biomass that has been developed for a future full-scale process). This
biomass is preferentially obtained from a thickened acclimated mixed
liquor sample. Collect the sample either by bailing from the mixed
liquor in the aeration tank with a weighted container, or by collecting
aeration tank effluent at the effluent overflow weir. Transport the
sample to the laboratory within no more than 4 hours of collection.
Maintain the biomass concentration in the benchtop bioreactor at the
level of the full-scale system +10 percent throughout the sampling
period of the test method.
8.0 Sample Collection, Preservation, Storage, and Transport
8.1 Benchtop Bioreactor Operation. Charge the mixed liquor to the
benchtop bioreactor, minimizing headspace over the liquid surface to
minimize entrainment of mixed liquor in the circulating gas. Fasten the
benchtop bioreactor headplate to the reactor over the liquid surface.
Maintain the
[[Page 171]]
temperature of the contents of the benchtop bioreactor system at the
temperature of the target full-scale system, 2
[deg]C, throughout the testing period. Monitor and record the
temperature of the benchtop bioreactor contents at least to the nearest
0.1 [deg]C.
8.1.1 Wastewater Storage. Collect the wastewater sample in the 20-L
collapsible container. Store the container at 4 [deg]C throughout the
testing period. Connect the container to the benchtop bioreactor feed
pump.
8.1.2 Wastewater Flow Rate.
8.1.2.1 The hydraulic residence time of the aeration tank is
calculated as the ratio of the volume of the tank (L) to the flow rate
(L/min). At the beginning of a test, the container shall be connected to
the feed pump and solution shall be pumped to the benchtop bioreactor at
the required flow rate to achieve the calculated hydraulic residence
time of wastewater in the aeration tank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.547
Where:
Qtest = wastewater flow rate (L/min)
Qfs = average flow rate of full-scale process (L/min)
Vfs = volume of full-scale aeration tank (L)
8.1.2.2 The target flow rate in the test apparatus is the same as
the flow rate in the target full-scale process multiplied by the ratio
of benchtop bioreactor volume (e.g., 6 L) to the volume of the full-
scale aeration tank. The hydraulic residence time shall be maintained at
90 to 100 percent of the residence time maintained in the full-scale
unit. A nominal flow rate is set on the pump based on a pump
calibration. Changes in the elasticity of the tubing in the pump head
and the accumulation of material in the tubing affect this calibration.
The nominal pumping rate shall be changed as necessary based on
volumetric flow measurements. Discharge the benchtop bioreactor effluent
to a wastewater storage, treatment, or disposal facility, except during
sampling or flow measurement periods.
8.1.3 Sludge Recycle Rate. Set the sludge recycle rate at a rate
sufficient to prevent accumulation in the bottom of the clarifier. Set
the air circulation rate sufficient to maintain the biomass in
suspension.
8.1.4 Benchtop Bioreactor Operation and Maintenance. Temperature,
dissolved oxygen concentration, exit vent flow rate, benchtop bioreactor
effluent flow rate, and air circulation rate shall be measured and
recorded three times throughout each day of benchtop bioreactor
operation. If other parameters (such as pH) are measured and maintained
in the target full-scale unit, these parameters, where appropriate,
shall be monitored and maintained to target full-scale specifications in
the benchtop bioreactor. At the beginning of each sampling period
(Section 8.2), sample the benchtop bioreactor contents for suspended
solids analysis. Take this sample by loosening a clamp on a length of
tubing attached to the lower side port. Determine the suspended solids
gravimetrically by the Gooch crucible/glass fiber filter method for
total suspended solids, in accordance with Standard Methods\3\ or
equivalent. When necessary, sludge shall be wasted from the lower side
port of the benchtop bioreactor, and the volume that is wasted shall be
replaced with an equal volume of the reactor effluent. Add thickened
activated sludge mixed liquor as necessary to the benchtop bioreactor to
increase the suspended solids concentration to the desired level. Pump
this mixed liquor to the benchtop bioreactor through the upper side port
(Item 24 in Figure 304A-1). Change the membrane on the dissolved oxygen
probe before starting the test. Calibrate the oxygen probe immediately
before the start of the test and each time the membrane is changed.
8.1.5 Inspection and Correction Procedures. If the feed line tubing
becomes clogged, replace with new tubing. If the feed flow rate is not
within 5 percent of target flow any time the flow rate is measured,
reset pump or check the flow measuring device and measure flow rate
again until target flow rate is achieved.
8.2 Test Sampling. At least two and one half hydraulic residence
times after the system has reached the targeted specifications shall be
permitted to elapse before the first sample is taken. Effluent samples
of the clarifier discharge (Item 20 in Figure 304A-1) and the influent
wastewater feed are collected in 40-mL septum vials to which two drops
of 1:10 hydrochloric acid (HCl) in water have been added. Sample the
clarifier discharge directly from the drain line. These samples will be
composed of the entire flow from the system for a period of several
minutes. Feed samples shall be taken from the feed pump suction line
after temporarily stopping the benchtop bioreactor feed, removing a
connector, and squeezing the collapsible feed container. Store both
influent and effluent samples at 4 [deg]C immediately
[[Page 172]]
after collection and analyze within 8 hours of collection.
8.2.1 Frequency of Sampling. During the test, sample and analyze the
wastewater feed and the clarifier effluent at least six times. The
sampling intervals shall be separated by at least 8 hours. During any
individual sampling interval, sample the wastewater feed simultaneously
with or immediately after the effluent sample. Calculate the relative
standard deviation (RSD) of the amount removed (i.e., effluent
concentration--wastewater feed concentration). The RSD values shall be <
15 percent. If an RSD value is 15 percent, continue sampling
and analyzing influent and effluent sets of samples until the RSD values
are within specifications.
8.2.2 Sampling After Exposure of System to Atmosphere. If, after
starting sampling procedures, the benchtop bioreactor system is exposed
to the atmosphere (due to leaks, maintenance, etc.), allow at least one
hydraulic residence time to elapse before resuming sampling.
9.0 Quality Control
9.1 Dissolved Oxygen. Fluctuation in dissolved oxygen concentration
may occur for numerous reasons, including undetected gas leaks,
increases and decreases in mixed liquor suspended solids resulting from
cell growth and solids loss in the effluent stream, changes in diffuser
performance, cycling of effluent flow rate, and overcorrection due to
faulty or sluggish dissolved oxygen probe response. Control the
dissolved oxygen concentration in the benchtop bioreactor by changing
the proportion of oxygen in the circulating aeration gas. Should the
dissolved oxygen concentration drift below the designated experimental
condition, bleed a small amount of aeration gas from the system on the
pressure side (i.e., immediately upstream of one of the diffusers). This
will create a vacuum in the system, triggering the pressure sensitive
relay to open the solenoid valve and admit oxygen to the system. Should
the dissolved oxygen concentration drift above the designated
experimental condition, slow or stop the oxygen input to the system
until the dissolved oxygen concentration approaches the correct level.
9.2 Sludge Wasting.
9.2.1 Determine the suspended solids concentration (section 8.1.4)
at the beginning of a test, and once per day thereafter during the test.
If the test is completed within a two day period, determine the
suspended solids concentration after the final sample set is taken. If
the suspended solids concentration exceeds the specified concentration,
remove a fraction of the sludge from the benchtop bioreactor. The
required volume of mixed liquor to remove is determined as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.548
Where:
Vw is the wasted volume (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sm is the measured solids (g/L), and
Ss is the specified solids (g/L).
9.2.2 Remove the mixed liquor from the benchtop bioreactor by
loosening a clamp on the mixed liquor sampling tube and allowing the
required volume to drain to a graduated flask. Clamp the tube when the
correct volume has been wasted. Replace the volume of the liquid wasted
by pouring the same volume of effluent back into the benchtop
bioreactor. Dispose of the waste sludge properly.
9.3 Sludge Makeup. In the event that the suspended solids
concentration is lower than the specifications, add makeup sludge back
into the benchtop bioreactor. Determine the amount of sludge added by
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.549
Where:
Vw is the volume of sludge to add (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sw is the solids in the makeup sludge (g/L),
Sm is the measured solids (g/L), and Ss is the
specified solids (g/L).
[[Page 173]]
10.0 Calibration and Standardization
10.1 Wastewater Pump Calibration. Determine the wastewater flow rate
by collecting the system effluent for a time period of at least one
hour, and measuring the volume with a graduated cylinder. Record the
collection time period and volume collected. Determine flow rate. Adjust
the pump speed to deliver the specified flow rate.
10.2 Calibration Standards. Prepare calibration standards from pure
certified standards in an aqueous medium. Prepare and analyze three
concentrations of calibration standards for each target component (or
for a mixture of components) in triplicate daily throughout the analyses
of the test samples. At each concentration level, a single calibration
shall be within 5 percent of the average of the three calibration
results. The low and medium calibration standards shall bracket the
expected concentration of the effluent (treated) wastewater. The medium
and high standards shall bracket the expected influent concentration.
11.0 Analytical Procedures
11.1 Analysis. If the identity of the compounds of interest in the
wastewater is not known, a representative sample of the wastewater shall
be analyzed in order to identify all of the compounds of interest
present. A gas chromatography/mass spectrometry screening method is
recommended.
11.1.1 After identifying the compounds of interest in the
wastewater, develop and/or use one or more analytical techniques capable
of measuring each of those compounds (more than one analytical technique
may be required, depending on the characteristics of the wastewater).
Test Method 18, found in appendix A of 40 CFR 60, may be used as a
guideline in developing the analytical technique. Purge and trap
techniques may be used for analysis providing the target components are
sufficiently volatile to make this technique appropriate. The limit of
quantitation for each compound shall be determined (see reference 1). If
the effluent concentration of any target compound is below the limit of
quantitation determined for that compound, the operation of the Method
304 unit may be altered to attempt to increase the effluent
concentration above the limit of quantitation. Modifications to the
method shall be approved prior to the test. The request should be
addressed to Method 304 contact, Emissions Measurement Center, Mail Drop
19, U.S. Environmental Protection Agency, Research Triangle Park, NC
27711.
12.0 Data Analysis and Calculations
12.1 Nomenclature. The following symbols are used in the
calculations.
Ci = Average inlet feed concentration for a compound of
interest, as analyzed (mg/L)
Co = Average outlet (effluent) concentration for a compound
of interest, as analyzed (mg/L)
X = Biomass concentration, mixed liquor suspended solids (g/L)
t = Hydraulic residence time in the benchtop bioreactor (hours)
V = Volume of the benchtop bioreactor (L)
Q = Flow rate of wastewater into the benchtop bioreactor, average (L/
hour)
12.2 Residence Time. The hydraulic residence time of the benchtop
bioreactor is equal to the ratio of the volume of the benchtop
bioreactor (L) to the flow rate (L/h):
[GRAPHIC] [TIFF OMITTED] TR17OC00.550
12.3 Rate of Biodegradation. Calculate the rate of biodegradation
for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.551
12.4 First-Order Biorate Constant. Calculate the first-order biorate
constant (K1) for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.552
12.5 Relative Standard Deviation (RSD). Determine the standard
deviation of both the influent and effluent sample concentrations (S)
using the following equation:
[[Page 174]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.553
12.6 Determination of Percent Air Emissions and Percent Biodegraded.
Use the results from this test method and follow the applicable
procedures in appendix C of 40 CFR part 63, entitled, ``Determination of
the Fraction Biodegraded (Fbio) in a Biological Treatment
Unit'' to determine Fbio.
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 References
1. ``Guidelines for data acquisition and data quality evaluation in
Environmental Chemistry,'' Daniel MacDoughal, Analytical Chemistry,
Volume 52, p. 2242, 1980.
2. Test Method 18, 40 CFR 60, appendix A.
3. Standard Methods for the Examination of Water and Wastewater,
16th Edition, Method 209C, Total Suspended Solids Dried at 103-105
[deg]C, APHA, 1985.
4. Water7, Hazardous Waste Treatment, Storage, and Disposal
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection
Agency, EPA-450/3-87-026, Review Draft, November 1989.
5. Chemdat7, Hazardous Waste Treatment, Storage, and Disposal
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection
Agency, EPA-450/3-87-026, Review Draft, November 1989.
17.0 Tables, Diagrams, Flowcharts, and Validation Data
[[Page 175]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.554
Method 304B: Determination of Biodegradation Rates of Organic Compounds
(Scrubber Option)
1.0 Scope and Application
1.1 Applicability. This method is applicable for the determination
of biodegradation rates of organic compounds in an activated sludge
process. The test method is designed to evaluate the ability of an
aerobic biological reaction system to degrade or destroy specific
components in waste streams. The method may also be used to determine
the effects of changes in wastewater composition on operation. The
biodegradation rates determined by utilizing this method are not
representative of a full-scale system. Full-scale systems embody
biodegradation and air
[[Page 176]]
emissions in competing reactions. This method measures biodegradation in
absence of air emissions. The rates measured by this method shall be
used in conjunction with the procedures listed in appendix C of this
part to calculate the fraction emitted to the air versus the fraction
biodegraded.
2.0 Summary of Method
2.1 A self-contained benchtop bioreactor system is assembled in the
laboratory. A sample of mixed liquor is added and the waste stream is
then fed continuously. The benchtop bioreactor is operated under
conditions nearly identical to the target full-scale activated sludge
process, except that air emissions are not a factor. The benchtop
bioreactor temperature, dissolved oxygen concentration, average
residence time in the reactor, waste composition, biomass concentration,
and biomass composition of the target full-scale process are the
parameters which are duplicated in the laboratory system. Biomass shall
be removed from the target full-scale activated sludge unit and held for
no more than 4 hours prior to use in the benchtop bioreactor. If
antifoaming agents are used in the full-scale system, they shall also be
used in the benchtop bioreactor. The feed flowing into and the effluent
exiting the benchtop bioreactor are analyzed to determine the
biodegradation rates of the target compounds. The choice of analytical
methodology for measuring the compounds of interest at the inlet and
outlet to the benchtop bioreactor are left to the discretion of the
source, except where validated methods are available.
3.0 Definitions [Reserved]
4.0 Interferences [Reserved]
5.0 Safety
5.1 If explosive gases are produced as a byproduct of biodegradation
and could realistically pose a hazard, closely monitor headspace
concentration of these gases to ensure laboratory safety. Placement of
the benchtop bioreactor system inside a laboratory hood is recommended
regardless of byproducts produced.
6.0 Equipment and Supplies
Note: Figure 304B-1 illustrates a typical laboratory apparatus used
to measure biodegradation rates. While the following description refers
to Figure 304B-1, the EPA recognizes that alternative reactor
configurations, such as alternative reactor shapes and locations of
probes and the feed inlet, will also meet the intent of this method.
Ensure that the benchtop bioreactor system is self-contained and
isolated from the atmosphere by leak-checking fittings, tubing, etc.
6.1 Benchtop Bioreactor. The biological reaction is conducted in a
biological oxidation reactor of at least 6-liters capacity. The benchtop
bioreactor is sealed and equipped with internal probes for controlling
and monitoring dissolved oxygen and internal temperature. The top of the
benchtop bioreactor is equipped for aerators, gas flow ports, and
instrumentation (while ensuring that no leaks to the atmosphere exist
around the fittings).
6.2 Aeration gas. Aeration gas is added to the benchtop bioreactor
through three diffusers, which are glass tubes that extend to the bottom
fifth of the reactor depth. A pure oxygen pressurized cylinder is
recommended in order to maintain the specified oxygen concentration.
Install a blower (e.g., Diaphragm Type, 15 SCFH capacity) to blow the
aeration gas into the benchtop bioreactor diffusers. Measure the
aeration gas flow rate with a rotameter (e.g., 0-15 SCFH recommended).
The aeration gas will rise through the benchtop bioreactor, dissolving
oxygen into the mixture in the process. The aeration gas must provide
sufficient agitation to keep the solids in suspension. Provide an exit
for the aeration gas from the top flange of the benchtop bioreactor
through a water-cooled (e.g., Allihn-type) vertical condenser. Install
the condenser through a gas-tight fitting in the benchtop bioreactor
closure. Design the system so that at least 10 percent of the gas flows
through an alkaline scrubber containing 175 mL of 45 percent by weight
solution of potassium hydroxide (KOH) and 5 drops of 0.2 percent
alizarin yellow dye. Route the balance of the gas through an adjustable
scrubber bypass. Route all of the gas through a 1-L knock-out flask to
remove entrained moisture and then to the intake of the blower. The
blower recirculates the gas to the benchtop bioreactor.
6.3 Wastewater Feed. Supply the wastewater feed to the benchtop
bioreactor in a collapsible low-density polyethylene container or
collapsible liner in a container (e.g., 20 L) equipped with a spigot cap
(collapsible containers or liners of other material may be required due
to the permeability of some volatile compounds through polyethylene).
Obtain the wastewater feed by sampling the wastewater feed in the target
process. A representative sample of wastewater shall be obtained from
the piping leading to the aeration tank. This sample may be obtained
from existing sampling valves at the discharge of the wastewater feed
pump, or collected from a pipe discharging to the aeration tank, or by
pumping from a well-mixed equalization tank upstream from the aeration
tank. Alternatively, wastewater can be pumped continuously to the
laboratory apparatus from a bleed stream taken from the equalization
tank of the full-scale treatment system.
6.3.1 Refrigeration System. Keep the wastewater feed cool by ice or
by refrigeration to 4 [deg]C. If using a bleed stream from the
[[Page 177]]
equalization tank, refrigeration is not required if the residence time
in the bleed stream is less than five minutes.
6.3.2 Wastewater Feed Pump. The wastewater is pumped from the
refrigerated container using a variable-speed peristaltic pump drive
equipped with a peristaltic pump head. Add the feed solution to the
benchtop bioreactor through a fitting on the top flange. Determine the
rate of feed addition to provide a retention time in the benchtop
bioreactor that is numerically equivalent to the retention time in the
target full-scale system. The wastewater shall be fed at a rate
sufficient to achieve 90 to 100 percent of the target full-scale system
residence time.
6.3.3 Treated wastewater feed. The benchtop bioreactor effluent
exits at the bottom of the reactor through a tube and proceeds to the
clarifier.
6.4 Clarifier. The effluent flows to a separate closed clarifier
that allows separation of biomass and effluent (e.g., 2-liter pear-
shaped glass separatory funnel, modified by removing the stopcock and
adding a 25-mm OD glass tube at the bottom). Benchtop bioreactor
effluent enters the clarifier through a tube inserted to a depth of 0.08
m (3 in.) through a stopper at the top of the clarifier. System effluent
flows from a tube inserted through the stopper at the top of the
clarifier to a drain (or sample bottle when sampling). The underflow
from the clarifier leaves from the glass tube at the bottom of the
clarifier. Flexible tubing connects this fitting to the sludge recycle
pump. This pump is coupled to a variable speed pump drive. The discharge
from this pump is returned through a tube inserted in a port on the side
of the benchtop bioreactor. An additional port is provided near the
bottom of the benchtop bioreactor for sampling the reactor contents. The
mixed liquor from the benchtop bioreactor flows into the center of the
clarifier. The clarified system effluent separates from the biomass and
flows through an exit near the top of the clarifier. There shall be no
headspace in the clarifier.
6.5 Temperature Control Apparatus. Capable of maintaining the system
at a temperature equal to the temperature of the full-scale system. The
average temperature should be maintained within 2
[deg]C of the set point.
6.5.1 Temperature Monitoring Device. A resistance type temperature
probe or a thermocouple connected to a temperature readout with a
resolution of 0.1 [deg]C or better.
6.5.2 Benchtop Bioreactor Heater. The heater is connected to the
temperature control device.
6.6 Oxygen Control System. Maintain the dissolved oxygen
concentration at the levels present in the full-scale system. Target
full-scale activated sludge systems with dissolved oxygen concentration
below 2 mg/L are required to maintain the dissolved oxygen concentration
in the benchtop bioreactor within 0.5 mg/L of the target dissolved
oxygen level. Target full-scale activated sludge systems with dissolved
oxygen concentration above 2 mg/L are required to maintain the dissolved
oxygen concentration in the benchtop bioreactor within 1.5 mg/L of the
target dissolved oxygen concentration; however, for target full-scale
activated sludge systems with dissolved oxygen concentrations above 2
mg/L, the dissolved oxygen concentration in the benchtop bioreactor may
not drop below 1.5 mg/L. If the benchtop bioreactor is outside the
control range, the dissolved oxygen is noted and the reactor operation
is adjusted.
6.6.1 Dissolved Oxygen Monitor. Dissolved oxygen is monitored with a
polarographic probe (gas permeable membrane) connected to a dissolved
oxygen meter (e.g., 0 to 15 mg/L, 0 to 50 [deg]C).
6.6.2 Benchtop Bioreactor Pressure Monitor. The benchtop bioreactor
pressure is monitored through a port in the top flange of the reactor.
This is connected to a gauge control with a span of 13-cm water vacuum
to 13-cm water pressure or better. A relay is activated when the vacuum
exceeds an adjustable setpoint which opens a solenoid valve (normally
closed), admitting oxygen to the system. The vacuum setpoint controlling
oxygen addition to the system shall be set at approximately 2.5 0.5 cm water and maintained at this setting except
during brief periods when the dissolved oxygen concentration is
adjusted.
6.7 Connecting Tubing. All connecting tubing shall be Teflon or
equivalent in impermeability. The only exception to this specification
is the tubing directly inside the pump head of the wastewater feed pump,
which may be Viton, Silicone or another type of flexible tubing.
Note: Mention of trade names or products does not constitute
endorsement by the U.S. Environmental Protection Agency.
7.0. Reagents and Standards
7.1 Wastewater. Obtain a representative sample of wastewater at the
inlet to the full-scale treatment plant if there is an existing full-
scale treatment plant (See Section 6.3). If there is no existing full-
scale treatment plant, obtain the wastewater sample as close to the
point of determination as possible. Collect the sample by pumping the
wastewater into the 20-L collapsible container. The loss of volatiles
shall be minimized from the wastewater by collapsing the container
before filling, by minimizing the time of filling, and by avoiding a
headspace in the container after filling. If the wastewater requires the
addition of nutrients to support the biomass growth and maintain biomass
characteristics, those nutrients are added and mixed with the container
contents after the container is filled.
[[Page 178]]
7.2 Biomass. Obtain the biomass or activated sludge used for rate
constant determination in the bench-scale process from the existing
full-scale process or from a representative biomass culture (e.g.,
biomass that has been developed for a future full-scale process). This
biomass is preferentially obtained from a thickened acclimated mixed
liquor sample. Collect the sample either by bailing from the mixed
liquor in the aeration tank with a weighted container, or by collecting
aeration tank effluent at the effluent overflow weir. Transport the
sample to the laboratory within no more than 4 hours of collection.
Maintain the biomass concentration in the benchtop bioreactor at the
level of the target full-scale system +10 percent throughout the
sampling period of the test method.
8.0 Sample Collection, Preservation, Storage, and Transport
8.1 Benchtop Bioreactor Operation. Charge the mixed liquor to the
benchtop bioreactor, minimizing headspace over the liquid surface to
minimize entrainment of mixed liquor in the circulating gas. Fasten the
benchtop bioreactor headplate to the reactor over the liquid surface.
Maintain the temperature of the contents of the benchtop bioreactor
system at the temperature of the target full-scale system, 2 [deg]C, throughout the testing period. Monitor and
record the temperature of the reactor contents at least to the nearest
0.1 [deg]C.
8.1.1 Wastewater Storage. Collect the wastewater sample in the 20-L
collapsible container. Store the container at 4 [deg]C throughout the
testing period. Connect the container to the benchtop bioreactor feed
pump.
8.1.2 Wastewater Flow Rate.
8.1.2.1 The hydraulic residence time of the aeration tank is
calculated as the ratio of the volume of the tank (L) to the flow rate
(L/min). At the beginning of a test, the container shall be connected to
the feed pump and solution shall be pumped to the benchtop bioreactor at
the required flow rate to achieve the calculated hydraulic residence
time of wastewater in the aeration tank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.555
Where:
Qtest = wastewater flow rate (L/min)
Qfs = average flow rate of full-scale process (L/min)
Vfs = volume of full-scale aeration tank (L)
8.1.2.2 The target flow rate in the test apparatus is the same as
the flow rate in the target full-scale process multiplied by the ratio
of benchtop bioreactor volume (e.g., 6 L) to the volume of the full-
scale aeration tank. The hydraulic residence time shall be maintained at
90 to 100 percent of the residence time maintained in the target full-
scale unit. A nominal flow rate is set on the pump based on a pump
calibration. Changes in the elasticity of the tubing in the pump head
and the accumulation of material in the tubing affect this calibration.
The nominal pumping rate shall be changed as necessary based on
volumetric flow measurements. Discharge the benchtop bioreactor effluent
to a wastewater storage, treatment, or disposal facility, except during
sampling or flow measurement periods.
8.1.3 Sludge Recycle Rate. Set the sludge recycle rate at a rate
sufficient to prevent accumulation in the bottom of the clarifier. Set
the air circulation rate sufficient to maintain the biomass in
suspension.
8.1.4 Benchtop Bioreactor Operation and Maintenance. Temperature,
dissolved oxygen concentration, flow rate, and air circulation rate
shall be measured and recorded three times throughout each day of
testing. If other parameters (such as pH) are measured and maintained in
the target full-scale unit, these parameters shall, where appropriate,
be monitored and maintained to full-scale specifications in the benchtop
bioreactor. At the beginning of each sampling period (section 8.2),
sample the benchtop bioreactor contents for suspended solids analysis.
Take this sample by loosening a clamp on a length of tubing attached to
the lower side port. Determine the suspended solids gravimetrically by
the Gooch crucible/glass fiber filter method for total suspended solids,
in accordance with Standard Methods \3\ or equivalent. When necessary,
sludge shall be wasted from the lower side port of the benchtop
bioreactor, and the volume that is wasted shall be replaced with an
equal volume of the benchtop bioreactor effluent. Add thickened
activated sludge mixed liquor as necessary to the benchtop bioreactor to
increase the suspended solids concentration to the desired level. Pump
this mixed liquor to the benchtop bioreactor through the upper side port
(Item 24 in Figure 304B-1). Change the membrane on the dissolved oxygen
probe before starting the test. Calibrate the oxygen probe immediately
before the start of the test and each time the membrane is changed.
[[Page 179]]
The scrubber solution shall be replaced each weekday with 175 mL 45
percent W/W KOH solution to which five drops of 0.2 percent alizarin
yellow indicator in water have been added. The potassium hydroxide
solution in the alkaline scrubber shall be changed if the alizarin
yellow dye color changes.
8.1.5 Inspection and Correction Procedures. If the feed line tubing
becomes clogged, replace with new tubing. If the feed flow rate is not
within 5 percent of target flow any time the flow rate is measured,
reset pump or check the flow measuring device and measure flow rate
again until target flow rate is achieved.
8.2 Test Sampling. At least two and one half hydraulic residence
times after the system has reached the targeted specifications shall be
permitted to elapse before the first sample is taken. Effluent samples
of the clarifier discharge (Item 20 in Figure 304B-1) and the influent
wastewater feed are collected in 40-mL septum vials to which two drops
of 1:10 hydrochloric acid (HCl) in water have been added. Sample the
clarifier discharge directly from the drain line. These samples will be
composed of the entire flow from the system for a period of several
minutes. Feed samples shall be taken from the feed pump suction line
after temporarily stopping the benchtop bioreactor feed, removing a
connector, and squeezing the collapsible feed container. Store both
influent and effluent samples at 4 [deg]C immediately after collection
and analyze within 8 hours of collection.
8.2.1 Frequency of Sampling. During the test, sample and analyze the
wastewater feed and the clarifier effluent at least six times. The
sampling intervals shall be separated by at least 8 hours. During any
individual sampling interval, sample the wastewater feed simultaneously
with or immediately after the effluent sample. Calculate the RSD of the
amount removed (i.e., effluent concentration--wastewater feed
concentration). The RSD values shall be <15 percent. If an RSD value is
15 percent, continue sampling and analyzing influent and
effluent sets of samples until the RSD values are within specifications.
8.2.2 Sampling After Exposure of System to Atmosphere. If, after
starting sampling procedures, the benchtop bioreactor system is exposed
to the atmosphere (due to leaks, maintenance, etc.), allow at least one
hydraulic residence time to elapse before resuming sampling.
9.0 Quality Control
9.1 Dissolved Oxygen. Fluctuation in dissolved oxygen concentration
may occur for numerous reasons, including undetected gas leaks,
increases and decreases in mixed liquor suspended solids resulting from
cell growth and solids loss in the effluent stream, changes in diffuser
performance, cycling of effluent flow rate, and overcorrection due to
faulty or sluggish dissolved oxygen probe response. Control the
dissolved oxygen concentration in the benchtop bioreactor by changing
the proportion of oxygen in the circulating aeration gas. Should the
dissolved oxygen concentration drift below the designated experimental
condition, bleed a small amount of aeration gas from the system on the
pressure side (i.e., immediately upstream of one of the diffusers). This
will create a vacuum in the system, triggering the pressure sensitive
relay to open the solenoid valve and admit oxygen to the system. Should
the dissolved oxygen concentration drift above the designated
experimental condition, slow or stop the oxygen input to the system
until the dissolved oxygen concentration approaches the correct level.
9.2 Sludge Wasting.
9.2.1 Determine the suspended solids concentration (section 8.1.4)
at the beginning of a test, and once per day thereafter during the test.
If the test is completed within a two day period, determine the
suspended solids concentration after the final sample set is taken. If
the suspended solids concentration exceeds the specified concentration,
remove a fraction of the sludge from the benchtop bioreactor. The
required volume of mixed liquor to remove is determined as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.556
Where:
Vw is the wasted volume (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sm is the measured solids (g/L), and
Ss is the specified solids (g/L).
9.2.2 Remove the mixed liquor from the benchtop bioreactor by
loosening a clamp on the mixed liquor sampling tube and allowing the
required volume to drain to a graduated flask. Clamp the tube when the
correct volume has been wasted. Replace the volume of
[[Page 180]]
the liquid wasted by pouring the same volume of effluent back into the
benchtop bioreactor. Dispose of the waste sludge properly.
9.3 Sludge Makeup. In the event that the suspended solids
concentration is lower than the specifications, add makeup sludge back
into the benchtop bioreactor. Determine the amount of sludge added by
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.557
Where:
Vw is the volume of sludge to add (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sw is the solids in the makeup sludge (g/L),
Sm is the measured solids (g/L), and
Ss is the specified solids (g/L).
10.0 Calibration and Standardizations
10.1 Wastewater Pump Calibration. Determine the wastewater flow rate
by collecting the system effluent for a time period of at least one
hour, and measuring the volume with a graduated cylinder. Record the
collection time period and volume collected. Determine flow rate. Adjust
the pump speed to deliver the specified flow rate.
10.2 Calibration Standards. Prepare calibration standards from pure
certified standards in an aqueous medium. Prepare and analyze three
concentrations of calibration standards for each target component (or
for a mixture of components) in triplicate daily throughout the analyses
of the test samples. At each concentration level, a single calibration
shall be within 5 percent of the average of the three calibration
results. The low and medium calibration standards shall bracket the
expected concentration of the effluent (treated) wastewater. The medium
and high standards shall bracket the expected influent concentration.
11.0 Analytical Test Procedures
11.1 Analysis. If the identity of the compounds of interest in the
wastewater is not known, a representative sample of the wastewater shall
be analyzed in order to identify all of the compounds of interest
present. A gas chromatography/mass spectrometry screening method is
recommended.
11.1.1 After identifying the compounds of interest in the
wastewater, develop and/or use one or more analytical technique capable
of measuring each of those compounds (more than one analytical technique
may be required, depending on the characteristics of the wastewater).
Method 18, found in appendix A of 40 CFR 60, may be used as a guideline
in developing the analytical technique. Purge and trap techniques may be
used for analysis providing the target components are sufficiently
volatile to make this technique appropriate. The limit of quantitation
for each compound shall be determined.\1\ If the effluent concentration
of any target compound is below the limit of quantitation determined for
that compound, the operation of the Method 304 unit may be altered to
attempt to increase the effluent concentration above the limit of
quantitation. Modifications to the method shall be approved prior to the
test. The request should be addressed to Method 304 contact, Emissions
Measurement Center, Mail Drop 19, U.S. Environmental Protection Agency,
Research Triangle Park, NC 27711.
12.0 Data Analysis and Calculations
12.1 Nomenclature. The following symbols are used in the
calculations.
Ci = Average inlet feed concentration for a compound of
interest, as analyzed (mg/L)
Co = Average outlet (effluent) concentration for a compound
of interest, as analyzed (mg/L)
X = Biomass concentration, mixed liquor suspended solids (g/L)
t = Hydraulic residence time in the benchtop bioreactor (hours)
V = Volume of the benchtop bioreactor (L)
Q = Flow rate of wastewater into the benchtop bioreactor, average (L/
hour)
12.2 Residence Time. The hydraulic residence time of the benchtop
bioreactor is equal to the ratio of the volume of the benchtop
bioreactor (L) to the flow rate (L/h)
[GRAPHIC] [TIFF OMITTED] TR17OC00.558
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12.3 Rate of Biodegradation. Calculate the rate of biodegradation
for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.559
12.4 First-Order Biorate Constant. Calculate the first-order biorate
constant (K1) for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.560
12.5 Relative Standard Deviation (RSD). Determine the standard
deviation of both the influent and effluent sample concentrations (S)
using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.561
12.6 Determination of Percent Air Emissions and Percent Biodegraded.
Use the results from this test method and follow the applicable
procedures in appendix C of 40 CFR Part 63, entitled, ``Determination of
the Fraction Biodegraded (Fbio) in a Biological Treatment
Unit'' to determine Fbio.
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 References
1. ``Guidelines for data acquisition and data quality evaluation in
Environmental Chemistry'', Daniel MacDoughal, Analytical Chemistry,
Volume 52, p. 2242, 1980.
2. Test Method 18, 40 CFR 60, Appendix A.
3. Standard Methods for the Examination of Water and Wastewater,
16th Edition, Method 209C, Total Suspended Solids Dried at 103-105
[deg]C, APHA, 1985.
4. Water--7, Hazardous Waste Treatment, Storage, and Disposal
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection
Agency, EPA-450/3-87-026, Review Draft, November 1989.
5. Chemdat7, Hazardous Waste Treatment, Storage, and Disposal
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection
Agency, EPA-450/3-87-026, Review Draft, November 1989.
17.0 Tables, Diagrams, Flowcharts, and Validation Data
[[Page 182]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.562
Method 305: Measurement of Emission Potential of Individual Volatile
Organic Compounds in Waste
Note: This method does not include all of the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical)
essential to its performance. Some material is incorporated by reference
from other methods in 40 CFR Part 60, Appendix A. Therefore, to obtain
reliable results, persons using this method should have a thorough
knowledge of at least Method 25D.
1.0 Scope and Application
1.1 Analyte. Volatile Organics. No CAS No. assigned.
1.2 Applicability. This procedure is used to determine the emission
potential of individual volatile organics (VOs) in waste.
1.3 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.
[[Page 183]]
2.0 Summary of Method
2.1 The heated purge conditions established by Method 25D (40 CFR
Part 60, Appendix A) are used to remove VOs from a 10 gram sample of
waste suspended in a 50/50 solution of polyethylene glycol (PEG) and
water. The purged VOs are quantified by using the sample collection and
analytical techniques (e.g. gas chromatography) appropriate for the VOs
present in the waste. The recovery efficiency of the sample collection
and analytical technique is determined for each waste matrix. A
correction factor is determined for each compound (if acceptable
recovery criteria requirements are met of 70 to 130 percent recovery for
every target compound), and the measured waste concentration is
corrected with the correction factor for each compound. A minimum of
three replicate waste samples shall be analyzed.
3.0 Definitions [Reserved]
4.0 Interferences [Reserved]
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of the
user of this test method to establish appropriate safety and health
practices and to determine the applicability of regulatory limitations
prior to performing this test method.
6.0 Equipment and Supplies
6.1 Method 25D Purge Apparatus.
6.1.1 Purge Chamber. The purge chamber shall accommodate the 10 gram
sample of waste suspended in a matrix of 50 mL of PEG and 50 mL of
deionized, hydrocarbon-free water. Three fittings are used on the glass
chamber top. Two 7 Ace-threads are used for the purge gas inlet
and outlet connections. A 50 Ace-thread is used to connect the
top of the chamber to the base (see Figure 305-1). The base of the
chamber has a side-arm equipped with a 22 Sovirel fitting to
allow for easy sample introductions into the chamber. The dimensions of
the chamber are shown in Figure 305-1.
6.1.2 Flow Distribution Device (FDD). The FDD enhances the gas-to-
liquid contact for improved purging efficiency. The FDD is a 6 mm OD
(0.2 in) by 30 cm (12 in) long glass tube equipped with four arm
bubblers as shown in Figure 305-1. Each arm shall have an opening of 1
mm (0.04 in) in diameter.
6.1.3 Coalescing Filter. The coalescing filter serves to discourage
aerosol formation of sample gas once it leaves the purge chamber. The
glass filter has a fritted disc mounted 10 cm (3.9 in) from the bottom.
Two 7 Ace-threads are used for the inlet and outlet
connections. The dimensions of the chamber are shown in Figure 305-2.
6.1.4 Oven. A forced convection airflow oven capable of maintaining
the purge chamber and coalescing filter at 75 2
[deg]C (167 3.6 [deg]F).
6.1.5 Toggle Valve. An on/off valve constructed from brass or
stainless steel rated to 100 psig. This valve is placed in line between
the purge nitrogen source and the flow controller.
6.1.6 Flow Controller. High-quality stainless steel flow controller
capable of restricting a flow of nitrogen to 6 0.06 L/min (0.2 0.002 ft\3\/min)
at 40 psig.
6.1.7 Polyethylene Glycol Cleaning System.
6.1.7.1 Round-Bottom Flask. One liter, three-neck glass round-bottom
flask for cleaning PEG. Standard taper 24/40 joints are mounted on each
neck.
6.1.7.2 Heating Mantle. Capable of heating contents of the 1-L flask
to 120 [deg]C (248 [deg]F).
6.1.7.3 Nitrogen Bubbler. Teflon[reg] or glass tube, 0.25
in OD (6.35 mm).
6.1.7.4 Temperature Sensor. Partial immersion glass thermometer.
6.1.7.5 Hose Adapter. Glass with 24/40 standard tapered joint.
6.2 Volatile Organic Recovery System.
6.2.1 Splitter Valve (Optional). Stainless steel cross-pattern valve
capable of splitting nominal flow rates from the purge flow of 6 L/min
(0.2 ft\3\/min). The valve shall be maintained at 75 + 2 [deg]C (167
3.6 [deg]F) in the heated zone and shall be placed
downstream of the coalescing filter. It is recommended that 0.125 in OD
(3.175 mm) tubing be used to direct the split vent flow from the heated
zone. The back pressure caused by the 0.125 in OD (3.175 mm) tubing is
critical for maintaining proper split valve operation.
Note: The splitter valve design is optional; it may be used in cases
where the concentration of a pollutant would saturate the adsorbents.
6.2.2 Injection Port. Stainless steel 1/4 in OD (6.35 mm)
compression fitting tee with a 6 mm (0.2 in) septum fixed on the top
port. The injection port is the point of entry for the recovery study
solution. If using a gaseous standard to determine recovery efficiency,
connect the gaseous standard to the injection port of the tee.
6.2.3 Knockout Trap (Optional but Recommended). A 25 mL capacity
glass reservoir body with a full-stem impinger (to avoid leaks, a
modified midget glass impinger with a screw cap and ball/socket clamps
on the inlet and outlet is recommended). The empty impinger is placed in
an ice water bath between the injection port and the sorbent cartridge.
Its purpose is to reduce the water content of the purge gas (saturated
at 75 [deg]C (167 [deg]F)) before the sorbent cartridge.
6.2.4 Insulated Ice Bath. A 350 mL dewar or other type of insulated
bath is used to
[[Page 184]]
maintain ice water around the knockout trap.
6.2.5 Sorbent Cartridges. Commercially available glass or stainless
steel cartridge packed with one or more appropriate sorbents. The amount
of adsorbent packed in the cartridge depends on the breakthrough volume
of the test compounds but is limited by back pressure caused by the
packing (not to exceed 7 psig). More than one sorbent cartridge placed
in series may be necessary depending upon the mixture of the measured
components.
6.2.6 Volumetric Glassware. Type A glass 10 mL volumetric flasks for
measuring a final volume from the water catch in the knockout trap.
6.2.7 Thermal Desorption Unit. A clam-shell type oven, used for the
desorption of direct thermal desorption sorbent tubes. The oven shall be
capable of increasing the temperature of the desorption tubes rapidly to
recommended desorption temperature.
6.2.8 Ultrasonic Bath. Small bath used to agitate sorbent material
and desorption solvent. Ice water shall be used in the bath because of
heat transfer caused by operation of the bath.
6.2.9 Desorption Vials. Four-dram (15 mL) capacity borosilicate
glass vials with Teflon-lined caps.
6.3 Analytical System. A gas chromatograph (GC) is commonly used to
separate and quantify compounds from the sample collection and recovery
procedure. Method 18 (40 CFR Part 60, Appendix A) may be used as a
guideline for determining the appropriate GC column and GC detector
based on the test compounds to be determined. Other types of analytical
instrumentation may be used (HPLC) in lieu of GC systems as long as the
recovery efficiency criteria of this method are met.
6.3.1 Gas Chromatograph (GC). The GC shall be equipped with a
constant-temperature liquid injection port or a heated sampling loop/
valve system, as appropriate. The GC oven shall be temperature-
programmable over the useful range of the GC column. The choice of
detectors is based on the test compounds to be determined.
6.3.2 GC Column. Select the appropriate GC column based on (1)
literature review or previous experience, (2) polarity of the analytes,
(3) capacity of the column, or (4) resolving power (e.g., length,
diameter, film thickness) required.
6.3.3 Data System. A programmable electronic integrator for
recording, analyzing, and storing the signal generated by the detector.
7.0 Reagents and Standards
7.1 Method 25D Purge Apparatus.
7.1.1 Polyethylene Glycol (PEG). Ninety-eight percent pure organic
polymer with an average molecular weight of 400 g/mol. Volatile organics
are removed from the PEG prior to use by heating to 120 5 [deg]C (248 9 [deg]F) and
purging with pure nitrogen at 1 L/min (0.04 ft\3\/min) for 2 hours.
After purging and heating, the PEG is maintained at room temperature
under a nitrogen purge maintained at 1 L/min (0.04 ft\3\/min) until
used. A typical apparatus used to clean the PEG is shown in Figure 305-
3.
7.1.2 Water. Organic-free deionized water is required.
7.1.3 Nitrogen. High-purity nitrogen (less than 0.5 ppm total
hydrocarbons) is used to remove test compounds from the purge matrix.
The source of nitrogen shall be regulated continuously to 40 psig before
the on/off toggle valve.
7.2 Volatile Organic Recovery System.
7.2.1 Water. Organic-free deionized water is required.
7.2.2 Desorption Solvent (when used). Appropriate high-purity (99.99
percent) solvent for desorption shall be used. Analysis shall be
performed (utilizing the same analytical technique as that used in the
analysis of the waste samples) on each lot to determine purity.
7.3 Analytical System. The gases required for GC operation shall be
of the highest obtainable purity (hydrocarbon free). Consult the
operating manual for recommended settings.
8.0 Sample Collection, Preservation, Storage, and Transport
8.1 Assemble the glassware and associated fittings (see Figures 305-
3 and 305-4, as appropriate) and leak-check the system (approximately 7
psig is the target pressure). After an initial leak check, mark the
pressure gauge and use the initial checkpoint to monitor for leaks
throughout subsequent analyses. If the pressure in the system drops
below the target pressure at any time during analysis, that analysis
shall be considered invalid.
8.2 Recovery Efficiency Determination. Determine the individual
recovery efficiency (RE) for each of the target compounds in duplicate
before the waste samples are analyzed. To determine the RE, generate a
water blank (Section 11.1) and use the injection port to introduce a
known volume of spike solution (or certified gaseous standard)
containing all of the target compounds at the levels expected in the
waste sample. Introduce the spike solution immediately after the
nitrogen purge has been started (Section 8.3.2). Follow the procedures
outlined in Section 8.3.3. Analyze the recovery efficiency samples using
the techniques described in Section 11.2. Determine the recovery
efficiency (Equation 305-1, Section 12.2) by comparing the amount of
compound recovered to the theoretical amount spiked. Determine the RE
twice for each compound; the relative
[[Page 185]]
standard deviation, (RSD) shall be <=10 percent for each compound. If
the RSD for any compound is not <= 10 percent, modify the sampling/
analytical procedure and complete an RE study in duplicate, or continue
determining RE until the RSD meets the acceptable criteria. The average
RE shall be 0.70 <= RE <= 1.30 for each compound. If the average RE does
not meet these criteria, an alternative sample collection and/or
analysis technique shall be developed and the recovery efficiency
determination shall be repeated for that compound until the criteria are
met for every target compound. Example modifications of the sampling/
analytical system include changing the adsorbent material, changing the
desorption solvent, utilizing direct thermal desorption of test
compounds from the sorbent tubes, utilizing another analytical
technique.
8.3 Sample Collection and Recovery.
8.3.1 The sample collection procedure in Method 25D shall be used to
collect (into a preweighed vial) 10 g of waste into PEG, cool, and ship
to the laboratory. Remove the sample container from the cooler and wipe
the exterior to remove any ice or water. Weigh the container and sample
to the nearest 0.01 g and record the weight. Pour the sample from the
container into the purge flask. Rinse the sample container three times
with approximately 6 mL of PEG (or the volume needed to total 50 mL of
PEG in the purge flask), transferring the rinses to the purge flask. Add
50 mL of organic-free deionized water to the purge flask. Cap the purge
flask tightly in between each rinse and after adding all the components
into the flask.
8.3.2 Allow the oven to equilibrate to 75 2
[deg]C (167 3.6 [deg]F). Begin the sample recovery
process by turning the toggle valve on, thus allowing a 6 L/min flow of
pure nitrogen through the purge chamber.
8.3.3 Stop the purge after 30 min. Immediately remove the sorbent
tube(s) from the apparatus and cap both ends. Remove the knockout trap
and transfer the water catch to a 10 mL volumetric flask. Rinse the trap
with organic-free deionized water and transfer the rinse to the
volumetric flask. Dilute to the 10 mL mark with water. Transfer the
water sample to a sample vial and store at 4 [deg]C (39.2 [deg]F) with
zero headspace. The analysis of the contents of the water knockout trap
is optional for this method. If the target compounds are water soluble,
analysis of the water is recommended; meeting the recovery efficiency
criteria in these cases would be difficult without adding the amount
captured in the knockout trap.
9.0 Quality Control
9.1 Miscellaneous Quality Control Measures.
------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
8.1........................... Sampling Ensures accurate
equipment leak- measurement of
check. sample volume.
8.2........................... Recovery Ensures accurate
efficiency (RE) sample collection
determination and analysis.
for each
measured
compound..
8.3........................... Calibration of Ensures linear
analytical measurement of
instrument with compounds over the
at least 3 instrument span.
calibration
standards..
------------------------------------------------------------------------
10.0 Calibration and Standardization
10.1 The analytical instrument shall be calibrated with a minimum of
three levels of standards for each compound whose concentrations bracket
the concentration of test compounds from the sorbent tubes. Liquid
calibration standards shall be used for calibration in the analysis of
the solvent extracts. The liquid calibration standards shall be prepared
in the desorption solvent matrix. The calibration standards may be
prepared and injected individually or as a mixture. If thermal
desorption and focusing (onto another sorbent or cryogen focusing) are
used, a certified gaseous mixture or a series of gaseous standards shall
be used for calibration of the instrument. The gaseous standards shall
be focused and analyzed in the same manner as the samples.
10.2 The analytical system shall be certified free from contaminants
before a calibration is performed (see Section 11.1). The calibration
standards are used to determine the linearity of the analytical system.
Perform an initial calibration and linearity check by analyzing the
three calibration standards for each target compound in triplicate
starting with the lowest level and continuing to the highest level. If
the triplicate analyses do not agree within 5 percent of their average,
additional analyses will be needed until the 5 percent criteria is met.
Calculate the response factor (Equation 305-3, Section 12.4) from the
average area counts of the injections for each concentration level.
Average the response factors of the standards for each compound. The
linearity of the detector is acceptable if the response factor of each
compound at a particular concentration is within 10 percent of the
overall mean response factor for that compound. Analyze daily a mid-
level calibration standard in duplicate and calculate a new response
factor. Compare the daily response factor average to the average
response factor calculated for the mid-level calibration during the
initial linearity check; repeat the three-
[[Page 186]]
level calibration procedure if the daily average response factor differs
from the initial linearity check mid-level response factor by more than
10 percent. Otherwise, proceed with the sample analysis.
11.0 Analytical Procedure
11.1 Water Blank Analysis. A water blank shall be analyzed daily to
determine the cleanliness of the purge and recovery system. A water
blank is generated by adding 60 mL of organic-free deionized water to 50
mL of PEG in the purge chamber. Treat the blank as described in Sections
8.3.2 and 8.3.3. The purpose of the water blank is to insure that no
contaminants exist in the sampling and analytical apparatus which would
interfere with the quantitation of the target compounds. If contaminants
are present, locate the source of contamination, remove it, and repeat
the water blank analysis.
11.2 Sample Analysis. Sample analysis in the context of this method
refers to techniques to remove the target compounds from the sorbent
tubes, separate them using a chromatography technique, and quantify them
with an appropriate detector. Two types of sample extraction techniques
typically used for sorbents include solvent desorption or direct thermal
desorption of test compounds to a secondary focusing unit (either
sorbent or cryogen based). The test compounds are then typically
transferred to a GC system for analysis. Other analytical systems may be
used (e.g., HPLC) in lieu of GC systems as long as the recovery
efficiency criteria of this method are met.
11.2.1 Recover the test compounds from the sorbent tubes that
require solvent desorption by transferring the adsorbent material to a
sample vial containing the desorption solvent. The desorption solvent
shall be the same as the solvent used to prepare calibration standards.
The volume of solvent depends on the amount of adsorbed material to be
desorbed (1.0 mL per 100 mg of adsorbent material) and also on the
amount of test compounds present. Final volume adjustment and or
dilution can be made so that the concentration of test compounds in the
desorption solvent is bracketed by the concentration of the calibration
solutions. Ultrasonicate the desorption solvent for 15 min in an ice
bath. Allow the sample to sit for a period of time so that the adsorbent
material can settle to the bottom of the vial. Transfer the solvent with
a pasteur pipet (minimizing the amount of adsorbent material taken) to
another vial and store at 4 [deg]C (39.2 [deg]F).
11.2.2 Analyze the desorption solvent or direct thermal desorption
tubes from each sample using the same analytical parameters used for the
calibration standard. Calculate the total weight detected for each
compound (Equation 305-4, Section 12.5). The slope (area/amount) and y-
intercept are calculated from the line bracketed between the two closest
calibration points. Correct the concentration of each waste sample with
the appropriate recovery efficiency factor and the split flow ratio (if
used). The final concentration of each individual test compound is
calculated by dividing the corrected measured weight for that compound
by the weight of the original sample determined in Section 8.3.1
(Equation 305-5, Section 12.6).
11.2.3 Repeat the analysis for the three samples collected in
Section 8.3. Report the corrected concentration of each of the waste
samples, average waste concentration, and relative standard deviation
(Equation 305-6, Section 12.7).
12.0 Data Analysis and Calculations.
12.1 Nomenclature.
AS = Mean area counts of test compound in standard.
AU = Mean area counts of test compound in sample desorption
solvent.
b = Y-intercept of the line formed between the two closest calibration
standards that bracket the concentration of the sample.
CT = Amount of test compound ([micro]g) in calibration
standard.
CF = Correction for adjusting final amount of sample detected
for losses during individual sample runs.
FP = Nitrogen flow through the purge chamber (6 L/min).
FS = Nitrogen split flow directed to the sample recovery
system (use 6 L/min if split flow design was not used).
PPM = Final concentration of test compound in waste sample [[micro]g/g
(which is equivalent to parts per million by weight (ppmw))].
RE = Recovery efficiency for adjusting final amount of sample detected
for losses due to inefficient trapping and desorption techniques.
R.F. = Response factor for test compound, calculated from a calibration
standard.
S = Slope of the line (area counts/CT) formed between two
closest calibration points that bracket the concentration of the sample.
WC = Weight of test compound expected to be recovered in
spike solution based on theoretical amount ([micro]g).
WE = Weight of vial and PEG (g).
WF = Weight of vial, PEG and waste sample (g).
WS = Weight of original waste sample (g).
WT = Corrected weight of test compound measured ([micro]g) in
sample.
WX = Weight of test compound measured during analysis of
recovery efficiency spike samples ([micro]g).
12.2 Recovery efficiency for determining trapping/desorption
efficiency of individual test compounds in the spike solution, decimal
value.
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12.3 Weight of waste sample (g).
[GRAPHIC] [TIFF OMITTED] TR17OC00.564
12.4 Response factor for individual test compounds.
[GRAPHIC] [TIFF OMITTED] TR17OC00.565
12.5 Corrected weight of a test compound in the sample, in [micro]g.
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12.6 Final concentration of a test compound in the sample in ppmw.
[GRAPHIC] [TIFF OMITTED] TR17OC00.567
12.7 Relative standard deviation (RSD) calculation.
[GRAPHIC] [TIFF OMITTED] TR17OC00.568
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 References [Reserved]
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17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.569
[GRAPHIC] [TIFF OMITTED] TR17OC00.570
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[GRAPHIC] [TIFF OMITTED] TR17OC00.571
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Method 306--Determination of Chromium Emissions From Decorative and Hard
Chromium Electroplating and Chromium Anodizing Operations--Isokinetic
Method
Note: This method does not include all of the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical)
essential to its performance. Some material is incorporated by reference
from other methods in 40 CFR Part 60, Appendix A. Therefore, to obtain
reliable results, persons using this method should have a thorough
knowledge of at least Method 5.
1.0 Scope and Application
1.1 Analytes.
------------------------------------------------------------------------
Analyte CAS No. Sensitivity
------------------------------------------------------------------------
Chromium...................... 7440-47-3........ See Sec. 13.2.
------------------------------------------------------------------------
1.2 Applicability. This method applies to the determination of
chromium (Cr) in emissions from decorative and hard chrome
electroplating facilities, chromium anodizing operations, and continuous
chromium plating operations at iron and steel facilities.
1.3 Data Quality Objectives. [Reserved]
2.0 Summary of Method
2.1 Sampling. An emission sample is extracted isokinetically from
the source using an unheated Method 5 sampling train (40 CFR Part 60,
Appendix A), with a glass nozzle and probe liner, but with the filter
omitted. The sample time shall be at least two hours. The Cr emissions
are collected in an alkaline solution containing 0.1 N sodium hydroxide
(NaOH) or 0.1 N sodium bicarbonate (NaHCO3). The collected
samples are recovered using an alkaline solution and are then
transported to the laboratory for analysis.
2.2 Analysis.
2.2.1 Total chromium samples with high chromium concentrations
(=35 [micro]g/L) may be analyzed using inductively coupled
plasma emission spectrometry (ICP) at 267.72 nm.
Note: The ICP analysis is applicable for this method only when the
solution analyzed has a Cr concentration greater than or equal to 35
[micro]g/L or five times the method detection limit as determined
according to Appendix B in 40 CFR Part 136.
[[Page 191]]
2.2.2 Alternatively, when lower total chromium concentrations (<35
[micro]g/L) are encountered, a portion of the alkaline sample solution
may be digested with nitric acid and analyzed by graphite furnace atomic
absorption spectroscopy (GFAAS) at 357.9 nm.
2.2.3 If it is desirable to determine hexavalent chromium
(Cr+6) emissions, the samples may be analyzed using an ion
chromatograph equipped with a post-column reactor (IC/PCR) and a visible
wavelength detector. To increase sensitivity for trace levels of
Cr+6, a preconcentration system may be used in conjunction
with the IC/PCR.
3.0 Definitions
3.1 Total Chromium--measured chromium content that includes both
major chromium oxidation states (Cr+3, Cr+3).
3.2 May--Implies an optional operation.
3.3 Digestion--The analytical operation involving the complete (or
nearly complete) dissolution of the sample in order to ensure the
complete solubilization of the element (analyte) to be measured.
3.4 Interferences--Physical, chemical, or spectral phenomena that
may produce a high or low bias in the analytical result.
3.5 Analytical System--All components of the analytical process
including the sample digestion and measurement apparatus.
3.6 Sample Recovery--The quantitative transfer of sample from the
collection apparatus to the sample preparation (digestion, etc.)
apparatus. This term should not be confused with analytical recovery.
3.7 Matrix Modifier--A chemical modification to the sample during
GFAAS determinations to ensure that the analyte is not lost during the
measurement process (prior to the atomization stage)
3.8 Calibration Reference Standards--Quality control standards used
to check the accuracy of the instrument calibration curve prior to
sample analysis.
3.9 Continuing Check Standard--Quality control standards used to
verify that unacceptable drift in the measurement system has not
occurred.
3.10 Calibration Blank--A blank used to verify that there has been
no unacceptable shift in the baseline either immediately following
calibration or during the course of the analytical measurement.
3.11 Interference Check--An analytical/measurement operation that
ascertains whether a measurable interference in the sample exists.
3.12 Interelement Correction Factors--Factors used to correct for
interfering elements that produce a false signal (high bias).
3.13 Duplicate Sample Analysis--Either the repeat measurement of a
single solution or the measurement of duplicate preparations of the same
sample. It is important to be aware of which approach is required for a
particular type of measurement. For example, no digestion is required
for the ICP determination and the duplicate instrument measurement is
therefore adequate whereas duplicate digestion/instrument measurements
are required for GFAAS.
3.14 Matrix Spiking--Analytical spikes that have been added to the
actual sample matrix either before (Section 9.2.5.2) or after (Section
9.1.6). Spikes added to the sample prior to a preparation technique
(e.g., digestion) allow for the assessment of an overall method accuracy
while those added after only provide for the measurement accuracy
determination.
4.0 Interferences
4.1 ICP Interferences.
4.1.1 ICP Spectral Interferences. Spectral interferences are caused
by: overlap of a spectral line from another element; unresolved overlap
of molecular band spectra; background contribution from continuous or
recombination phenomena; and, stray light from the line emission of
high-concentrated elements. Spectral overlap may be compensated for by
correcting the raw data with a computer and measuring the interfering
element. At the 267.72 nm Cr analytical wavelength, iron, manganese, and
uranium are potential interfering elements. Background and stray light
interferences can usually be compensated for by a background correction
adjacent to the analytical line. Unresolved overlap requires the
selection of an alternative chromium wavelength. Consult the instrument
manufacturer's operation manual for interference correction procedures.
4.1.2 ICP Physical Interferences. High levels of dissolved solids in
the samples may cause significant inaccuracies due to salt buildup at
the nebulizer and torch tips. This problem can be controlled by diluting
the sample or by extending the rinse times between sample analyses.
Standards shall be prepared in the same solution matrix as the samples
(i.e., 0.1 N NaOH or 0.1 N NaHCO3).
4.1.3 ICP Chemical Interferences. These include molecular compound
formation, ionization effects and solute vaporization effects, and are
usually not significant in the ICP procedure, especially if the
standards and samples are matrix matched.
4.2 GFAAS Interferences.
4.2.1 GFAAS Chemical Interferences. Low concentrations of calcium
and/or phosphate may cause interferences; at concentrations above 200
[micro]g/L, calcium's effect is constant and eliminates the effect of
phosphate. Calcium nitrate is therefore added to the concentrated
analyte to ensure a known constant effect. Other matrix modifiers
recommended by the instrument manufacturer may also be considered.
4.2.2 GFAAS Cyanide Band Interferences. Nitrogen should not be used
as the purge gas due to cyanide band interference.
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4.2.3 GFAAS Spectral Interferences. Background correction may be
required because of possible significant levels of nonspecific
absorption and scattering at the 357.9 nm analytical wavelength.
4.2.4 GFAAS Background Interferences. Zeeman or Smith-Hieftje
background correction is recommended for interferences resulting from
high levels of dissolved solids in the alkaline impinger solutions.
4.3 IC/PCR Interferences.
4.3.1 IC/PCR Chemical Interferences. Components in the sample matrix
may cause Cr+6 to convert to trivalent chromium
(Cr+3) or cause Cr+3 to convert to
Cr+6. The chromatographic separation of Cr+6 using
ion chromatography reduces the potential for other metals to interfere
with the post column reaction. For the IC/PCR analysis, only compounds
that coelute with Cr+6 and affect the diphenylcarbazide
reaction will cause interference.
4.3.2 IC/PCR Background Interferences. Periodic analyses of reagent
water blanks are used to demonstrate that the analytical system is
essentially free of contamination. Sample cross-contamination can occur
when high-level and low-level samples or standards are analyzed
alternately and can be eliminated by thorough purging of the sample
loop. Purging of the sample can easily be achieved by increasing the
injection volume to ten times the size of the sample loop.
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of the
user to establish appropriate safety and health practices and to
determine the applicability of regulatory limitations prior to
performing this test method.
5.2 Hexavalent chromium compounds have been listed as carcinogens
although chromium (III) compounds show little or no toxicity. Chromium
can be a skin and respiratory irritant.
6.0 Equipment and Supplies
6.1 Sampling Train.
6.1.1 A schematic of the sampling train used in this method is shown
in Figure 306-1. The train is the same as shown in Method 5, Section 6.0
(40 CFR Part 60, Appendix A) except that the probe liner is unheated,
the particulate filter is omitted, and quartz or borosilicate glass must
be used for the probe nozzle and liner in place of stainless steel.
6.1.2 Probe fittings of plastic such as Teflon, polypropylene, etc.
are recommended over metal fittings to prevent contamination. If
desired, a single combined probe nozzle and liner may be used, but such
a single glass assembly is not a requirement of this methodology.
6.1.3 Use 0.1 N NaOH or 0.1 N NaHCO3 in the impingers in
place of water.
6.1.4 Operating and maintenance procedures for the sampling train
are described in APTD-0576 of Method 5. Users should read the APTD-0576
document and adopt the outlined procedures.
6.1.5 Similar collection systems which have been approved by the
Administrator may be used.
6.2 Sample Recovery. Same as Method 5, [40 CFR Part 60, Appendix A],
with the following exceptions:
6.2.1 Probe-Liner and Probe-Nozzle Brushes. Brushes are not
necessary for sample recovery. If a probe brush is used, it must be non-
metallic.
6.2.2 Sample Recovery Solution. Use 0.1 N NaOH or 0.1 N
NaHCO3, whichever is used as the impinger absorbing solution,
in place of acetone to recover the sample.
6.2.3 Sample Storage Containers. Polyethylene, with leak-free screw
cap, 250 mL, 500 mL or 1,000 mL.
6.3 Analysis.
6.3.1 General. For analysis, the following equipment is needed.
6.3.1.1 Phillips Beakers. (Phillips beakers are preferred, but
regular beakers may also be used.)
6.3.1.2 Hot Plate.
6.3.1.3 Volumetric Flasks. Class A, various sizes as appropriate.
6.3.1.4 Assorted Pipettes.
6.3.2 Analysis by ICP.
6.3.2.1 ICP Spectrometer. Computer-controlled emission spectrometer
with background correction and radio frequency generator.
6.3.2.2 Argon Gas Supply. Welding grade or better.
6.3.3 Analysis by GFAAS.
6.3.3.1 Chromium Hollow Cathode Lamp or Electrodeless Discharge
Lamp.
6.3.3.2 Graphite Furnace Atomic Absorption Spectrophotometer.
6.3.3.3 Furnace Autosampler.
6.3.4 Analysis by IC/PCR.
6.3.4.1 IC/PCR System. High performance liquid chromatograph pump,
sample injection valve, post-column reagent delivery and mixing system,
and a visible detector, capable of operating at 520 nm-540 nm, all with
a non-metallic (or inert) flow path. An electronic peak area mode is
recommended, but other recording devices and integration techniques are
acceptable provided the repeatability criteria and the linearity
criteria for the calibration curve described in Section 10.4 can be
satisfied. A sample loading system is required if preconcentration is
employed.
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6.3.4.2 Analytical Column. A high performance ion chromatograph
(HPIC) non-metallic column with anion separation characteristics and a
high loading capacity designed for separation of metal chelating
compounds to prevent metal interference. Resolution described in Section
11.6 must be obtained. A non-metallic guard column with the same ion-
exchange material is recommended.
6.3.4.3 Preconcentration Column (for older instruments). An HPIC
non-metallic column with acceptable anion retention characteristics and
sample loading rates must be used as described in Section 11.6.
6.3.4.4 Filtration Apparatus for IC/PCR.
6.3.4.4.1 Teflon, or equivalent, filter holder to accommodate 0.45-
[micro]m acetate, or equivalent, filter, if needed to remove insoluble
particulate matter.
6.3.4.4.2 0.45-[micro]m Filter Cartridge. For the removal of
insoluble material. To be used just prior to sample injection/analysis.
7.0 Reagents and Standards
Note: Unless otherwise indicated, all reagents should conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society (ACS reagent grade). Where such
specifications are not available, use the best available grade. Reagents
should be checked by the appropriate analysis prior to field use to
assure that contamination is below the analytical detection limit for
the ICP or GFAAS total chromium analysis; and that contamination is
below the analytical detection limit for Cr+6 using IC/PCR
for direct injection or, if selected, preconcentration.
7.1 Sampling.
7.1.1 Water. Reagent water that conforms to ASTM Specification
D1193-77 or 91 Type II (incorporated by reference see Sec. 63.14). All
references to water in the method refer to reagent water unless
otherwise specified. It is recommended that water blanks be checked
prior to preparing the sampling reagents to ensure that the Cr content
is less than three (3) times the anticipated detection limit of the
analytical method.
7.1.2 Sodium Hydroxide (NaOH) Absorbing Solution, 0.1 N. Dissolve
4.0 g of sodium hydroxide in 1 liter of water to obtain a pH of
approximately 8.5.
7.1.3 Sodium Bicarbonate (NaHCO3) Absorbing Solution, 0.1
N. Dissolve approximately 8.5 g of sodium bicarbonate in 1 liter of
water to obtain a pH of approximately 8.3.
7.1.4 Chromium Contamination.
7.1.4.1 The absorbing solution shall not exceed the QC criteria
noted in Section 7.1.1 (<= 3 times the instrument detection limit).
7.1.4.2 When the Cr+6 content in the field samples
exceeds the blank concentration by at least a factor of ten (10),
Cr+6 blank concentrations = 10 times the detection
limit will be allowed.
Note: At sources with high concentrations of acids and/or
SO2, the concentration of NaOH or NaHCO3 should be
= 0.5 N to insure that the pH of the solution remains at or
above 8.5 for NaOH and 8.0 for NaHCO3 during and after
sampling.
7.1.5 Silica Gel. Same as in Method 5.
7.2 Sample Recovery.
7.2.1 0.1 N NaOH or 0.1 N NaHCO3. Use the same solution
for the sample recovery that is used for the impinger absorbing
solution.
7.2.2 pH Indicator Strip, for IC/PCR. pH indicator capable of
determining the pH of solutions between the pH range of 7 and 12, at 0.5
pH increments.
7.3 Sample Preparation and Analysis.
7.3.1 Nitric Acid (HNO3), Concentrated, for GFAAS. Trace
metals grade or better HNO3 must be used for reagent
preparation. The ACS reagent grade HNO3 is acceptable for
cleaning glassware.
7.3.2 HNO3, 1.0% (v/v), for GFAAS. Prepare, by slowly
stirring, 10 mL of concentrated HNO3) into 800 mL of reagent
water. Dilute to 1,000 mL with reagent water. The solution shall contain
less than 0.001 mg Cr/L.
7.3.3 Calcium Nitrate Ca(NO3)2 Solution (10
[micro]g Ca/mL) for GFAAS analysis. Prepare the solution by weighing
40.9 mg of Ca(NO3)2 into a 1 liter volumetric
flask. Dilute with reagent water to 1 liter.
7.3.4 Matrix Modifier, for GFAAS. See instrument manufacturer's
manual for suggested matrix modifier.
7.3.5 Chromatographic Eluent, for IC/PCR. The eluent used in the
analytical system is ammonium sulfate based.
7.3.5.1 Prepare by adding 6.5 mL of 29 percent ammonium hydroxide
(NH4OH) and 33 g of ammonium sulfate
((NH4)2SO4) to 500 mL of reagent water.
Dilute to 1 liter with reagent water and mix well.
7.3.5.2 Other combinations of eluents and/or columns may be employed
provided peak resolution, repeatability, linearity, and analytical
sensitivity as described in Sections 9.3 and 11.6 are acceptable.
7.3.6 Post-Column Reagent, for IC/PCR. An effective post-column
reagent for use with the chromatographic eluent described in Section
7.3.5 is a diphenylcarbazide (DPC)-based system. Dissolve 0.5 g of 1,5-
diphenylcarbazide in 100 mL of ACS grade methanol. Add 500 mL of reagent
water containing 50 mL of 96 percent spectrophotometric grade sulfuric
acid. Dilute to 1 liter with reagent water.
7.3.7 Chromium Standard Stock Solution (1000 mg/L). Procure a
certified aqueous standard or dissolve 2.829 g of potassium dichromate
(K2Cr2O7), in reagent water and dilute
to 1 liter.
7.3.8 Calibration Standards for ICP or IC/PCR. Prepare calibration
standards for ICP or IC/PCR by diluting the Cr standard stock solution
(Section 7.3.7) with 0.1 N NaOH or
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0.1 N NaHCO3, whichever is used as the impinger absorbing
solution, to achieve a matrix similar to the actual field samples.
Suggested levels are 0, 50, 100, and 200 [micro]g Cr/L for ICP, and 0,
1, 5, and 10 [micro]g Cr+6/L for IC/PCR.
7.3.9 Calibration Standards for GFAAS. Chromium solutions for GFAAS
calibration shall contain 1.0 percent (v/v) HNO3. The zero
standard shall be 1.0 percent (v/v) HNO3. Calibration
standards should be prepared daily by diluting the Cr standard stock
solution (Section 7.3.7) with 1.0 percent HNO3. Use at least
four standards to make the calibration curve. Suggested levels are 0,
10, 50, and 100 [micro]g Cr/L.
7.4 Glassware Cleaning Reagents.
7.4.1 HNO3, Concentrated. ACS reagent grade or
equivalent.
7.4.2 Water. Reagent water that conforms to ASTM Specification
D1193-77 or 91 Type II.
7.4.3 HNO3, 10 percent (v/v). Add by stirring 500 mL of
concentrated HNO3 into a flask containing approximately 4,000
mL of reagent water. Dilute to 5,000 mL with reagent water. Mix well.
The reagent shall contain less than 2 [micro]g Cr/L.
7.5 Quality Assurance Audit Samples.
7.5.1 When making compliance determinations, and upon availability,
audit samples shall be obtained from the appropriate EPA regional Office
or from the responsible enforcement authority and analyzed in
conjunction with the field samples.
7.5.2 If EPA or National Institute of Standards and Technology
(NIST) reference audit sample are not available, a mid-range standard,
prepared from an independent commercial source, may be used.
Note: To order audit samples, contact the responsible enforcement
authority at least 30 days prior to the test date to allow sufficient
time for the audit sample to be delivered.
8.0 Sample Collection, Preservation, Holding Times, Storage, and
Transport
Note: Prior to sample collection, consideration should be given to
the type of analysis (Cr+6 or total Cr) that will be
performed. Which analysis option(s) will be performed will determine
which sample recovery and storage procedures will be required to process
the sample (See Figures 306-3 and 306-4).
8.1 Sample Collection. Same as Method 5 (40 CFR part 60, Appendix
A), with the following exceptions.
8.1.1 Omit the particulate filter and filter holder from the
sampling train. Use a glass nozzle and probe liner instead of stainless
steel. Do not heat the probe. Place 100 mL of 0.1 N NaOH or 0.1 N
NaHCO3 in each of the first two impingers, and record the
data for each run on a data sheet such as shown in Figure 306-2.
8.1.2 Clean all glassware prior to sampling in hot soapy water
designed for laboratory cleaning of glassware. Next, rinse the glassware
three times with tap water, followed by three additional rinses with
reagent water. Then soak the glassware in 10% (v/v) HNO3
solution for a minimum of 4 hours, rinse three times with reagent water,
and allow to air dry. Cover all glassware openings where contamination
can occur with Parafilm, or equivalent, until the sampling train is
assembled for sampling.
8.1.3 Train Operation. Follow the basic procedures outlined in
Method 5 in conjunction with the following instructions. Train sampling
rate shall not exceed 0.030 m\3\/min (1.0 cfm) during a run.
8.2 Sample Recovery. Follow the basic procedures of Method 5, with
the exceptions noted.
8.2.1 A particulate filter is not recovered from this train.
8.2.2 Tester shall select either the total Cr or Cr+6
sample recovery option.
8.2.3 Samples to be analyzed for both total Cr and Cr+6,
shall be recovered using the Cr+6 sample option (Section
8.2.6).
8.2.4 A field reagent blank shall be collected for either of the Cr
or the Cr+6 analysis. If both analyses (Cr and
Cr+6) are to be conducted on the samples, collect separate
reagent blanks for each analysis.
Note: Since particulate matter is not usually present at chromium
electroplating and/or chromium anodizing operations, it is not necessary
to filter the Cr+6 samples unless there is observed sediment
in the collected solutions. If it is necessary to filter the
Cr+6 solutions, please refer to Method 0061, Determination of
Hexavalent Chromium Emissions From Stationary Sources, Section 7.4,
Sample Preparation in SW-846 (see Reference 1).
8.2.5 Total Cr Sample Option.
8.2.5.1 Container No. 1. Measure the volume of the liquid in the
first, second, and third impingers and quantitatively transfer into a
labeled sample container.
8.2.5.2 Use approximately 200 to 300 mL of the 0.1 N NaOH or 0.1 N
NaHCO3 absorbing solution to rinse the probe nozzle, probe
liner, three impingers, and connecting glassware; add this rinse to
Container No. 1.
8.2.6 Cr+6 Sample Option.
8.2.6.1 Container No. 1. Measure and record the pH of the absorbing
solution contained in the first impinger at the end of the sampling run
using a pH indicator strip. The pH of the solution must be
=8.5 for NaOH and =8.0 for NaHCO3. If
it is not, discard the collected sample, increase the normality of the
NaOH or NaHCO3 impinger absorbing solution to 0.5 N or to a
solution normality approved by the Administrator and collect another air
emission sample.
8.2.6.2 After determining the pH of the first impinger solution,
combine and measure the volume of the liquid in the first, second, and
third impingers and quantitatively transfer into the labeled sample
container.
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Use approximately 200 to 300 mL of the 0.1 N NaOH or 0.1 N
NaHCO3 absorbing solution to rinse the probe nozzle, probe
liner, three impingers, and connecting glassware; add this rinse to
Container No. 1.
8.2.7 Field Reagent Blank.
8.2.7.1 Container No. 2.
8.2.7.2 Place approximately 500 mL of the 0.1 N NaOH or 0.1 N
NaHCO3 absorbing solution into a labeled sample container.
8.3 Sample Preservation, Storage, and Transport.
8.3.1 Total Cr Sample Option. Samples to be analyzed for total Cr
need not be refrigerated.
8.3.2 Cr+6 Sample Option. Samples to be analyzed for
Cr+6 must be shipped and stored at 4 [deg]C. Allow
Cr+6 samples to return to ambient temperature prior to
analysis.
8.4 Sample Holding Times.
8.4.1 Total Cr Sample Option. Samples to be analyzed for total Cr
shall be analyzed within 60 days of collection.
8.4.2 Cr+6 Sample Option. Samples to be analyzed for
Cr+6 shall be analyzed within 14 days of collection.
9.0 Quality Control
9.1 ICP Quality Control.
9.1.1 ICP Calibration Reference Standards. Prepare a calibration
reference standard using the same alkaline matrix as the calibration
standards; it should be at least 10 times the instrumental detection
limit.
9.1.1.1 This reference standard must be prepared from a different Cr
stock solution source than that used for preparation of the calibration
curve standards.
9.1.1.2 Prior to sample analysis, analyze at least one reference
standard.
9.1.1.3 The calibration reference standard must be measured within
10 percent of it's true value for the curve to be considered valid.
9.1.1.4 The curve must be validated before sample analyses are
performed.
9.1.2 ICP Continuing Check Standard.
9.1.2.1 Perform analysis of the check standard with the field
samples as described in Section 11.2 (at least after every 10 samples,
and at the end of the analytical run).
9.1.2.2 The check standard can either be the mid-range calibration
standard or the reference standard. The results of the check standard
shall agree within 10 percent of the expected value; if not, terminate
the analyses, correct the problem, recalibrate the instrument, and rerun
all samples analyzed subsequent to the last acceptable check standard
analysis.
9.1.3 ICP Calibration Blank.
9.1.3.1 Perform analysis of the calibration blank with the field
samples as described in Section 11.2 (at least after every 10 samples,
and at the end of the analytical run).
9.1.3.2 The results of the calibration blank shall agree within
three standard deviations of the mean blank value. If not, analyze the
calibration blank two more times and average the results. If the average
is not within three standard deviations of the background mean,
terminate the analyses, correct the problem, recalibrate, and reanalyze
all samples analyzed subsequent to the last acceptable calibration blank
analysis.
9.1.4 ICP Interference Check. Prepare an interference check solution
that contains known concentrations of interfering elements that will
provide an adequate test of the correction factors in the event of
potential spectral interferences.
9.1.4.1 Two potential interferences, iron and manganese, may be
prepared as 1000 [micro]g/mL and 200 [micro]g/mL solutions,
respectively. The solutions should be prepared in dilute HNO3
(1-5 percent). Particular care must be used to ensure that the solutions
and/or salts used to prepare the solutions are of ICP grade purity
(i.e., that no measurable Cr contamination exists in the salts/
solutions). Commercially prepared interfering element check standards
are available.
9.1.4.2 Verify the interelement correction factors every three
months by analyzing the interference check solution. The correction
factors are calculated according to the instrument manufacturer's
directions. If the interelement correction factors are used properly, no
false Cr should be detected.
9.1.4.3 Negative results with an absolute value greater than three
(3) times the detection limit are usually the results of the background
correction position being set incorrectly. Scan the spectral region to
ensure that the correction position has not been placed on an
interfering peak.
9.1.5 ICP Duplicate Sample Analysis. Perform one duplicate sample
analysis for each compliance sample batch (3 runs).
9.1.5.1 As there is no sample preparation required for the ICP
analysis, a duplicate analysis is defined as a repeat analysis of one of
the field samples. The selected sample shall be analyzed using the same
procedures that were used to analyze the original sample.
9.1.5.2 Duplicate sample analyses shall agree within 10 percent of
the original measurement value.
9.1.5.3 Report the original analysis value for the sample and report
the duplicate analysis value as the QC check value. If agreement is not
achieved, perform the duplicate analysis again. If agreement is not
achieved the second time, perform corrective action to identify and
correct the problem before analyzing the sample for a third time.
9.1.6 ICP Matrix Spiking. Spiked samples shall be prepared and
analyzed daily to ensure that there are no matrix effects, that samples
and standards have been matrix-matched, and that the laboratory
equipment is operating properly.
[[Page 196]]
9.1.6.1 Spiked sample recovery analyses should indicate a recovery
for the Cr spike of between 75 and 125 percent.
9.1.6.2 Cr levels in the spiked sample should provide final solution
concentrations that are within the linear portion of the calibration
curve, as well as, at a concentration level at least: equal to that of
the original sample; and, ten (10) times the detection limit.
9.1.6.3 If the spiked sample concentration meets the stated criteria
but exceeds the linear calibration range, the spiked sample must be
diluted with the field absorbing solution.
9.1.6.4 If the recoveries for the Cr spiked samples do not meet the
specified criteria, perform corrective action to identify and correct
the problem prior to reanalyzing the samples.
9.1.7 ICP Field Reagent Blank.
9.1.7.1 Analyze a minimum of one matrix-matched field reagent blank
(Section 8.2.4) per sample batch to determine if contamination or memory
effects are occurring.
9.1.7.2 If contamination or memory effects are observed, perform
corrective action to identify and correct the problem before reanalyzing
the samples.
9.1.8 Audit Sample Analysis.
9.1.8.1 When the method is used to analyze samples to demonstrate
compliance with a source emission regulation, an audit sample must be
analyzed, subject to availability.
9.1.8.2 Concurrently analyze the audit sample and the compliance
samples in the same manner to evaluate the technique of the analyst and
the standards preparation.
9.1.8.3 The same analyst, analytical reagents, and analytical system
shall be used for the compliance samples and the audit sample. If this
condition is met, duplicate auditing of subsequent compliance analyses
for the same enforcement agency within a 30-day period is waived. An
audit sample set may not be used to validate different sets of
compliance samples under the jurisdiction of separate enforcement
agencies, unless prior arrangements have been made with both enforcement
agencies.
9.1.9 Audit Sample Results.
9.1.9.1 Calculate the audit sample concentrations and submit results
using the instructions provided with the audit samples.
9.1.9.2 Report the results of the audit samples and the compliance
determination samples along with their identification numbers, and the
analyst's name to the responsible enforcement authority. Include this
information with reports of any subsequent compliance analyses for the
same enforcement authority during the 30-day period.
9.1.9.3 The concentrations of the audit samples obtained by the
analyst shall agree within the values specified by the compliance
auditor. If the specified range is not met, reanalyze the compliance and
audit samples, and include initial and reanalysis values in the test
report.
9.1.9.4 Failure to meet the specified range may require retests
unless the audit problems are resolved. However, if the audit results do
not affect the compliance or noncompliance status of the affected
facility, the Administrator may waive the reanalysis requirement,
further audits, or retests and accept the results of the compliance
test. While steps are being taken to resolve audit analysis problems,
the Administrator may also choose to use the data to determine the
compliance or noncompliance status of the affected facility.
9.2 GFAAS Quality Control.
9.2.1 GFAAS Calibration Reference Standards. The calibration curve
must be verified by using at least one calibration reference standard
(made from a reference material or other independent standard material)
at or near the mid-range of the calibration curve.
9.2.1.1 The calibration curve must be validated before sample
analyses are performed.
9.2.1.2 The calibration reference standard must be measured within
10 percent of its true value for the curve to be considered valid.
9.2.2 GFAAS Continuing Check Standard.
9.2.2.1 Perform analysis of the check standard with the field
samples as described in Section 11.4 (at least after every 10 samples,
and at the end of the analytical run).
9.2.2.2 These standards are analyzed, in part, to monitor the life
and performance of the graphite tube. Lack of reproducibility or a
significant change in the signal for the check standard may indicate
that the graphite tube should be replaced.
9.2.2.3 The check standard may be either the mid-range calibration
standard or the reference standard.
9.2.2.4 The results of the check standard shall agree within 10
percent of the expected value.
9.2.2.5 If not, terminate the analyses, correct the problem,
recalibrate the instrument, and reanalyze all samples analyzed
subsequent to the last acceptable check standard analysis.
9.2.3 GFAAS Calibration Blank.
9.2.3.1 Perform analysis of the calibration blank with the field
samples as described in Section 11.4 (at least after every 10 samples,
and at the end of the analytical run).
9.2.3.2 The calibration blank is analyzed to monitor the life and
performance of the graphite tube as well as the existence of any memory
effects. Lack of reproducibility or a significant change in the signal,
may indicate that the graphite tube should be replaced.
9.2.3.3 The results of the calibration blank shall agree within
three standard deviations of the mean blank value.
[[Page 197]]
9.2.3.4 If not, analyze the calibration blank two more times and
average the results. If the average is not within three standard
deviations of the background mean, terminate the analyses, correct the
problem, recalibrate, and reanalyze all samples analyzed subsequent to
the last acceptable calibration blank analysis.
9.2.4 GFAAS Duplicate Sample Analysis. Perform one duplicate sample
analysis for each compliance sample batch (3 runs).
9.2.4.1 A digested aliquot of the selected sample is processed and
analyzed using the identical procedures that were used for the whole
sample preparation and analytical efforts.
9.2.4.2 Duplicate sample analyses results incorporating duplicate
digestions shall agree within 20 percent for sample results exceeding
ten (10) times the detection limit.
9.2.4.3 Report the original analysis value for the sample and report
the duplicate analysis value as the QC check value.
9.2.4.4 If agreement is not achieved, perform the duplicate analysis
again. If agreement is not achieved the second time, perform corrective
action to identify and correct the problem before analyzing the sample
for a third time.
9.2.5 GFAAS Matrix Spiking.
9.2.5.1 Spiked samples shall be prepared and analyzed daily to
ensure that (1) correct procedures are being followed, (2) there are no
matrix effects and (3) all equipment is operating properly.
9.2.5.2 Cr spikes are added prior to any sample preparation.
9.2.5.3 Cr levels in the spiked sample should provide final solution
concentrations that are within the linear portion of the calibration
curve, as well as, at a concentration level at least: equal to that of
the original sample; and, ten (10) times the detection limit.
9.2.5.4 Spiked sample recovery analyses should indicate a recovery
for the Cr spike of between 75 and 125 percent.
9.2.5.5 If the recoveries for the Cr spiked samples do not meet the
specified criteria, perform corrective action to identify and correct
the problem prior to reanalyzing the samples.
9.2.6 GFAAS Method of Standard Additions.
9.2.6.1 Method of Standard Additions. Perform procedures in Section
5.4 of Method 12 (40 CFR Part 60, Appendix A)
9.2.6.2 Whenever sample matrix problems are suspected and standard/
sample matrix matching is not possible or whenever a new sample matrix
is being analyzed, perform referenced procedures to determine if the
method of standard additions is necessary.
9.2.7 GFAAS Field Reagent Blank.
9.2.7.1 Analyze a minimum of one matrix-matched field reagent blank
(Section 8.2.4) per sample batch to determine if contamination or memory
effects are occurring.
9.2.7.2 If contamination or memory effects are observed, perform
corrective action to identify and correct the problem before reanalyzing
the samples.
9.2.8 Audit Sample Analysis.
9.2.8.1 When the method is used to analyze samples to demonstrate
compliance with a source emission regulation, an audit sample must be
analyzed, subject to availability.
9.2.8.2 Concurrently analyze the audit sample and the compliance
samples in the same manner to evaluate the technique of the analyst and
the standards preparation.
9.2.8.3 The same analyst, analytical reagents, and analytical system
shall be used for the compliance samples and the audit sample. If this
condition is met, duplicate auditing of subsequent compliance analyses
for the same enforcement agency within a 30-day period is waived. An
audit sample set may not be used to validate different sets of
compliance samples under the jurisdiction of separate enforcement
agencies, unless prior arrangements have been made with both enforcement
agencies.
9.2.9 Audit Sample Results.
9.2.9.1 Calculate the audit sample concentrations and submit results
using the instructions provided with the audit samples.
9.2.9.2 Report the results of the audit samples and the compliance
determination samples along with their identification numbers, and the
analyst's name to the responsible enforcement authority. Include this
information with reports of any subsequent compliance analyses for the
same enforcement authority during the 30-day period.
9.2.9.3 The concentrations of the audit samples obtained by the
analyst shall agree within the values specified by the compliance
auditor. If the specified range is not met, reanalyze the compliance and
audit samples, and include initial and reanalysis values in the test
report.
9.2.9.4 Failure to meet the specified range may require retests
unless the audit problems are resolved. However, if the audit results do
not affect the compliance or noncompliance status of the affected
facility, the Administrator may waive the reanalysis requirement,
further audits, or retests and accept the results of the compliance
test. While steps are being taken to resolve audit analysis problems,
the Administrator may also choose to use the data to determine the
compliance or noncompliance status of the affected facility.
9.3 IC/PCR Quality Control.
9.3.1 IC/PCR Calibration Reference Standards.
9.3.1.1 Prepare a calibration reference standard at a concentration
that is at or near the mid-point of the calibration curve using the same
alkaline matrix as the calibration standards. This reference standard
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should be prepared from a different Cr stock solution than that used to
prepare the calibration curve standards. The reference standard is used
to verify the accuracy of the calibration curve.
9.3.1.2 The curve must be validated before sample analyses are
performed. Prior to sample analysis, analyze at least one reference
standard with an expected value within the calibration range.
9.3.1.3 The results of this reference standard analysis must be
within 10 percent of the true value of the reference standard for the
calibration curve to be considered valid.
9.3.2 IC/PCR Continuing Check Standard and Calibration Blank.
9.3.2.1 Perform analysis of the check standard and the calibration
blank with the field samples as described in Section 11.6 (at least
after every 10 samples, and at the end of the analytical run).
9.3.2.2 The result from the check standard must be within 10 percent
of the expected value.
9.3.2.3 If the 10 percent criteria is exceeded, excessive drift and/
or instrument degradation may have occurred, and must be corrected
before further analyses can be performed.
9.3.2.4 The results of the calibration blank analyses must agree
within three standard deviations of the mean blank value.
9.3.2.5 If not, analyze the calibration blank two more times and
average the results.
9.3.2.6 If the average is not within three standard deviations of
the background mean, terminate the analyses, correct the problem,
recalibrate, and reanalyze all samples analyzed subsequent to the last
acceptable calibration blank analysis.
9.3.3 IC/PCR Duplicate Sample Analysis.
9.3.3.1 Perform one duplicate sample analysis for each compliance
sample batch (3 runs).
9.3.3.2 An aliquot of the selected sample is prepared and analyzed
using procedures identical to those used for the emission samples (for
example, filtration and/or, if necessary, preconcentration).
9.3.3.3 Duplicate sample injection results shall agree within 10
percent for sample results exceeding ten (10) times the detection limit.
9.3.3.4 Report the original analysis value for the sample and report
the duplicate analysis value as the QC check value.
9.3.3.5 If agreement is not achieved, perform the duplicate analysis
again.
9.3.3.6 If agreement is not achieved the second time, perform
corrective action to identify and correct the problem prior to analyzing
the sample for a third time.
9.3.4 ICP/PCR Matrix Spiking. Spiked samples shall be prepared and
analyzed with each sample set to ensure that there are no matrix
effects, that samples and standards have been matrix-matched, and that
the equipment is operating properly.
9.3.4.1 Spiked sample recovery analysis should indicate a recovery
of the Cr+6 spike between 75 and 125 percent.
9.3.4.2 The spiked sample concentration should be within the linear
portion of the calibration curve and should be equal to or greater than
the concentration of the original sample. In addition, the spiked sample
concentration should be at least ten (10) times the detection limit.
9.3.4.3 If the recoveries for the Cr+6 spiked samples do
not meet the specified criteria, perform corrective action to identify
and correct the problem prior to reanalyzing the samples.
9.3.5 IC/PCR Field Reagent Blank.
9.3.5.1 Analyze a minimum of one matrix-matched field reagent blank
(Section 8.2.4) per sample batch to determine if contamination or memory
effects are occurring.
9.3.5.2 If contamination or memory effects are observed, perform
corrective action to identify and correct the problem before reanalyzing
the samples.
9.3.6 Audit Sample Analysis.
9.3.6.1 When the method is used to analyze samples to demonstrate
compliance with source emission regulation, an audit sample must be
analyzed, subject to availability.
9.3.6.2 Concurrently analyze the audit sample and the compliance
samples in the same manner to evaluate the technique of the analyst and
the standards preparation.
9.3.6.3 The same analyst, analytical reagents, and analytical system
shall be used for the compliance samples and the audit sample. If this
condition is met, duplicate auditing of subsequent compliance analyses
for the same enforcement agency within a 30-day period is waived. An
audit sample set may not be used to validate different sets of
compliance samples under the jurisdiction of separate enforcement
agencies, unless prior arrangements have been made with both enforcement
agencies.
9.3.7 Audit Sample Results.
9.3.7.1 Calculate the audit sample concentrations and submit results
using the instructions provided with the audit samples.
9.3.7.2 Report the results of the audit samples and the compliance
determination samples along with their identification numbers, and the
analyst's name to the responsible enforcement authority. Include this
information with reports of any subsequent compliance analyses for the
same enforcement authority during the 30-day period.
9.3.7.3 The concentrations of the audit samples obtained by the
analyst shall agree within the values specified by the compliance
auditor. If the specified range is not met, reanalyze the compliance and
audit samples, and include initial and reanalysis values in the test
report.
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9.3.7.4 Failure to meet the specified range may require retests
unless the audit problems are resolved. However, if the audit results do
not affect the compliance or noncompliance status of the affected
facility, the Administrator may waive the reanalysis requirement,
further audits, or retests and accept the results of the compliance
test. While steps are being taken to resolve audit analysis problems,
the Administrator may also choose to use the data to determine the
compliance or noncompliance status of the affected facility.
10.0 Calibration and Standardization
10.1 Sampling Train Calibration. Perform calibrations described in
Method 5, (40 CFR Part 60, Appendix A). The alternate calibration
procedures described in Method 5, may also be used.
10.2 ICP Calibration.
10.2.1 Calibrate the instrument according to the instrument
manufacturer's recommended procedures, using a calibration blank and
three standards for the initial calibration.
10.2.2 Calibration standards should be prepared fresh daily, as
described in Section 7.3.8. Be sure that samples and calibration
standards are matrix matched. Flush the system with the calibration
blank between each standard.
10.2.3 Use the average intensity of multiple exposures (3 or more)
for both standardization and sample analysis to reduce random error.
10.2.4 Employing linear regression, calculate the correlation
coefficient .
10.2.5 The correlation coefficient must equal or exceed 0.995.
10.2.6 If linearity is not acceptable, prepare and rerun another set
of calibration standards or reduce the range of the calibration
standards, as necessary.
10.3 GFAAS Calibration.
10.3.1 For instruments that measure directly in concentration, set
the instrument software to display the correct concentration, if
applicable.
10.3.2 Curve must be linear in order to correctly perform the method
of standard additions which is customarily performed automatically with
most instrument computer-based data systems.
10.3.3 The calibration curve (direct calibration or standard
additions) must be prepared daily with a minimum of a calibration blank
and three standards that are prepared fresh daily.
10.3.4 The calibration curve acceptance criteria must equal or
exceed 0.995.
10.3.5 If linearity is not acceptable, prepare and rerun another set
of calibration standards or reduce the range of calibration standards,
as necessary.
10.4 IC/PCR Calibration.
10.4.1 Prepare a calibration curve using the calibration blank and
three calibration standards prepared fresh daily as described in Section
7.3.8.
10.4.2 The calibration curve acceptance criteria must equal or
exceed 0.995.
10.4.3 If linearity is not acceptable, remake and/or rerun the
calibration standards. If the calibration curve is still unacceptable,
reduce the range of the curve.
10.4.4 Analyze the standards with the field samples as described in
Section 11.6.
11.0 Analytical Procedures
Note: The method determines the chromium concentration in [micro]g
Cr/mL. It is important that the analyst measure the field sample volume
prior to analyzing the sample. This will allow for conversion of
[micro]g Cr/mL to [micro]g Cr/sample.
11.1 ICP Sample Preparation.
11.1.1 The ICP analysis is performed directly on the alkaline
impinger solution; acid digestion is not necessary, provided the samples
and standards are matrix matched.
11.1.2 The ICP analysis should only be employed when the solution
analyzed has a Cr concentration greater than 35 [micro]g/L or five times
the method detection limit as determined according to Appendix B in 40
CFR Part 136 or by other commonly accepted analytical procedures.
11.2 ICP Sample Analysis.
11.2.1 The ICP analysis is applicable for the determination of total
chromium only.
11.2.2 ICP Blanks. Two types of blanks are required for the ICP
analysis.
11.2.2.1 Calibration Blank. The calibration blank is used in
establishing the calibration curve. For the calibration blank, use
either 0.1 N NaOH or 0.1 N NaHCO3, whichever is used for the
impinger absorbing solution. The calibration blank can be prepared fresh
in the laboratory; it does not have to be prepared from the same batch
of solution that was used in the field. A sufficient quantity should be
prepared to flush the system between standards and samples.
11.2.2.2 Field Reagent Blank. The field reagent blank is collected
in the field during the testing program. The field reagent blank
(Section 8.2.4) is an aliquot of the absorbing solution prepared in
Section 7.1.2. The reagent blank is used to assess possible
contamination resulting from sample processing.
11.2.3 ICP Instrument Adjustment.
11.2.3.1 Adjust the ICP instrument for proper operating parameters
including wavelength, background correction settings (if necessary), and
interfering element correction settings (if necessary).
11.2.3.2 The instrument must be allowed to become thermally stable
before beginning measurements (usually requiring at least 30
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min of operation prior to calibration). During this warmup period, the
optical calibration and torch position optimization may be performed
(consult the operator's manual).
11.2.4 ICP Instrument Calibration.
11.2.4.1 Calibrate the instrument according to the instrument
manufacturer's recommended procedures, and the procedures specified in
Section 10.2.
11.2.4.2 Prior to analyzing the field samples, reanalyze the highest
calibration standard as if it were a sample.
11.2.4.3 Concentration values obtained should not deviate from the
actual values or from the established control limits by more than 5
percent, whichever is lower (see Sections 9.1 and 10.2).
11.2.4.4 If they do, follow the recommendations of the instrument
manufacturer to correct the problem.
11.2.5 ICP Operational Quality Control Procedures.
11.2.5.1 Flush the system with the calibration blank solution for at
least 1 min before the analysis of each sample or standard.
11.2.5.2 Analyze the continuing check standard and the calibration
blank after each batch of 10 samples.
11.2.5.3 Use the average intensity of multiple exposures for both
standardization and sample analysis to reduce random error.
11.2.6 ICP Sample Dilution.
11.2.6.1 Dilute and reanalyze samples that are more concentrated
than the linear calibration limit or use an alternate, less sensitive Cr
wavelength for which quality control data have already been established.
11.2.6.2 When dilutions are performed, the appropriate factors must
be applied to sample measurement results.
11.2.7 Reporting Analytical Results. All analytical results should
be reported in [micro]g Cr/mL using three significant figures. Field
sample volumes (mL) must be reported also.
11.3 GFAAS Sample Preparation.
11.3.1 GFAAS Acid Digestion. An acid digestion of the alkaline
impinger solution is required for the GFAAS analysis.
11.3.1.1 In a beaker, add 10 mL of concentrated HNO3 to a
100 mL sample aliquot that has been well mixed. Cover the beaker with a
watch glass. Place the beaker on a hot plate and reflux the sample to
near dryness. Add another 5 mL of concentrated HNO3 to
complete the digestion. Again, carefully reflux the sample volume to
near dryness. Rinse the beaker walls and watch glass with reagent water.
11.3.1.2 The final concentration of HNO3 in the solution
should be 1 percent (v/v).
11.3.1.3 Transfer the digested sample to a 50-mL volumetric flask.
Add 0.5 mL of concentrated HNO3 and 1 mL of the 10 [micro]g/
mL of Ca(NO3)2. Dilute to 50 mL with reagent
water.
11.3.2 HNO3 Concentration. A different final volume may
be used based on the expected Cr concentration, but the HNO3
concentration must be maintained at 1 percent (v/v).
11.4 GFAAS Sample Analysis.
11.4.1 The GFAAS analysis is applicable for the determination of
total chromium only.
11.4.2 GFAAS Blanks. Two types of blanks are required for the GFAAS
analysis.
11.4.2.1 Calibration Blank. The 1.0 percent HNO3 is the
calibration blank which is used in establishing the calibration curve.
11.4.2.2 Field Reagent Blank. An aliquot of the 0.1 N NaOH solution
or the 0.1 N NaHCO3 prepared in Section 7.1.2 is collected
for the field reagent blank. The field reagent blank is used to assess
possible contamination resulting from processing the sample.
11.4.2.2.1 The reagent blank must be subjected to the entire series
of sample preparation and analytical procedures, including the acid
digestion.
11.4.2.2.2 The reagent blank's final solution must contain the same
acid concentration as the sample solutions.
11.4.3 GFAAS Instrument Adjustment.
11.4.3.1 The 357.9 nm wavelength line shall be used.
11.4.3.2 Follow the manufacturer's instructions for all other
spectrophotometer operating parameters.
11.4.4 Furnace Operational Parameters. Parameters suggested by the
manufacturer should be employed as guidelines.
11.4.4.1 Temperature-sensing mechanisms and temperature controllers
can vary between instruments and/or with time; the validity of the
furnace operating parameters must be periodically confirmed by
systematically altering the furnace parameters while analyzing a
standard. In this manner, losses of analyte due to higher-than-necessary
temperature settings or losses in sensitivity due to less than optimum
settings can be minimized.
11.4.4.2 Similar verification of furnace operating parameters may be
required for complex sample matrices (consult instrument manual for
additional information). Calibrate the GFAAS system following the
procedures specified in Section 10.3.
11.4.5 GFAAS Operational Quality Control Procedures.
11.4.5.1 Introduce a measured aliquot of digested sample into the
furnace and atomize.
11.4.5.2 If the measured concentration exceeds the calibration
range, the sample should be diluted with the calibration blank solution
(1.0 percent HNO3) and reanalyzed.
11.4.5.3 Consult the operator's manual for suggested injection
volumes. The use of multiple injections can improve accuracy and assist
in detecting furnace pipetting errors.
11.4.5.4 Analyze a minimum of one matrix-matched reagent blank per
sample batch
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to determine if contamination or any memory effects are occurring.
11.4.5.5 Analyze a calibration blank and a continuing check standard
after approximately every batch of 10 sample injections.
11.4.6 GFAAS Sample Dilution.
11.4.6.1 Dilute and reanalyze samples that are more concentrated
than the instrument calibration range.
11.4.6.2 If dilutions are performed, the appropriate factors must be
applied to sample measurement results.
11.4.7 Reporting Analytical Results.
11.4.7.1 Calculate the Cr concentrations by the method of standard
additions (see operator's manual) or, from direct calibration. All
dilution and/or concentration factors must be used when calculating the
results.
11.4.7.2 Analytical results should be reported in [micro]g Cr/mL
using three significant figures. Field sample volumes (mL) must be
reported also.
11.5 IC/PCR Sample Preparation.
11.5.1 Sample pH. Measure and record the sample pH prior to
analysis.
11.5.2 Sample Filtration. Prior to preconcentration and/or analysis,
filter all field samples through a 0.45-[micro]m filter. The filtration
step should be conducted just prior to sample injection/analysis.
11.5.2.1 Use a portion of the sample to rinse the syringe filtration
unit and acetate filter and then collect the required volume of
filtrate.
11.5.2.2 Retain the filter if total Cr is to be determined also.
11.5.3 Sample Preconcentration (older instruments).
11.5.3.1 For older instruments, a preconcentration system may be
used in conjunction with the IC/PCR to increase sensitivity for trace
levels of Cr+6.
11.5.3.2 The preconcentration is accomplished by selectively
retaining the analyte on a solid absorbent, followed by removal of the
analyte from the absorbent (consult instrument manual).
11.5.3.3 For a manual system, position the injection valve so that
the eluent displaces the concentrated Cr+6 sample,
transferring it from the preconcentration column and onto the IC anion
separation column.
11.6 IC/PCR Sample Analyses.
11.6.1 The IC/PCR analysis is applicable for hexavalent chromium
measurements only.
11.6.2 IC/PCR Blanks. Two types of blanks are required for the IC/
PCR analysis.
11.6.2.1 Calibration Blank. The calibration blank is used in
establishing the analytical curve. For the calibration blank, use either
0.1 N NaOH or 0.1 N NaHCO3, whichever is used for the
impinger solution. The calibration blank can be prepared fresh in the
laboratory; it does not have to be prepared from the same batch of
absorbing solution that is used in the field.
11.6.2.2 Field Reagent Blank. An aliquot of the 0.1 N NaOH solution
or the 0.1 N NaHCO3 solution prepared in Section 7.1.2 is
collected for the field reagent blank. The field reagent blank is used
to assess possible contamination resulting from processing the sample.
11.6.3 Stabilized Baseline. Prior to sample analysis, establish a
stable baseline with the detector set at the required attenuation by
setting the eluent and post-column reagent flow rates according to the
manufacturers recommendations.
Note: As long as the ratio of eluent flow rate to PCR flow rate
remains constant, the standard curve should remain linear. Inject a
sample of reagent water to ensure that no Cr+6 appears in the
water blank.
11.6.4 Sample Injection Loop. Size of injection loop is based on
standard/sample concentrations and the selected attenuator setting.
11.6.4.1 A 50-[micro]L loop is normally sufficient for most higher
concentrations.
11.6.4.2 The sample volume used to load the injection loop should be
at least 10 times the loop size so that all tubing in contact with the
sample is thoroughly flushed with the new sample to prevent cross
contamination.
11.6.5 IC/PCR Instrument Calibration.
11.6.5.1 First, inject the calibration standards prepared, as
described in Section 7.3.8 to correspond to the appropriate
concentration range, starting with the lowest standard first.
11.6.5.2 Check the performance of the instrument and verify the
calibration using data gathered from analyses of laboratory blanks,
calibration standards, and a quality control sample.
11.6.5.3 Verify the calibration by analyzing a calibration reference
standard. If the measured concentration exceeds the established value by
more than 10 percent, perform a second analysis. If the measured
concentration still exceeds the established value by more than 10
percent, terminate the analysis until the problem can be identified and
corrected.
11.6.6 IC/PCR Instrument Operation.
11.6.6.1 Inject the calibration reference standard (as described in
Section 9.3.1), followed by the field reagent blank (Section 8.2.4), and
the field samples.
11.6.6.1.1 Standards (and QC standards) and samples are injected
into the sample loop of the desired size (use a larger size loop for
greater sensitivity). The Cr+6 is collected on the resin bed
of the column.
11.6.6.1.2 After separation from other sample components, the
Cr+6 forms a specific complex in the post-column reactor with
the DPC reaction solution, and the complex is detected by visible
absorbance at a maximum wavelength of 540 nm.
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11.6.6.1.3 The amount of absorbance measured is proportional to the
concentration of the Cr+6 complex formed.
11.6.6.1.4 The IC retention time and the absorbance of the
Cr+6 complex with known Cr+6 standards analyzed
under identical conditions must be compared to provide both qualitative
and quantitative analyses.
11.6.6.1.5 If a sample peak appears near the expected retention time
of the Cr+6 ion, spike the sample according to Section 9.3.4
to verify peak identity.
11.6.7 IC/PCR Operational Quality Control Procedures.
11.6.7.1 Samples should be at a pH =8.5 for NaOH and
=8.0 if using NaHCO3; document any discrepancies.
11.6.7.2 Refrigerated samples should be allowed to equilibrate to
ambient temperature prior to preparation and analysis.
11.6.7.3 Repeat the injection of the calibration standards at the
end of the analytical run to assess instrument drift. Measure areas or
heights of the Cr+6/DPC complex chromatogram peaks.
11.6.7.4 To ensure the precision of the sample injection (manual or
autosampler), the response for the second set of injected standards must
be within 10 percent of the average response.
11.6.7.5 If the 10 percent criteria duplicate injection cannot be
achieved, identify the source of the problem and rerun the calibration
standards.
11.6.7.6 Use peak areas or peak heights from the injections of
calibration standards to generate a linear calibration curve. From the
calibration curve, determine the concentrations of the field samples.
11.6.8 IC/PCR Sample Dilution.
11.6.8.1 Samples having concentrations higher than the established
calibration range must be diluted into the calibration range and re-
analyzed.
11.6.8.2 If dilutions are performed, the appropriate factors must be
applied to sample measurement results.
11.6.9 Reporting Analytical Results. Results should be reported in
[micro]g Cr+6/mL using three significant figures. Field
sample volumes (mL) must be reported also.
12.0 Data Analysis and Calculations
12.1 Pretest Calculations.
12.1.1 Pretest Protocol (Site Test Plan).
12.1.1.1 The pretest protocol should define and address the test
data quality objectives (DQOs), with all assumptions, that will be
required by the end user (enforcement authority); what data are needed?
why are the data needed? how will the data be used? what are method
detection limits? and what are estimated target analyte levels for the
following test parameters.
12.1.1.1.1 Estimated source concentration for total chromium and/or
Cr+6.
12.1.1.1.2 Estimated minimum sampling time and/or volume required to
meet method detection limit requirements (Appendix B 40 CFR Part 136)
for measurement of total chromium and/or Cr+6.
12.1.1.1.3 Demonstrate that planned sampling parameters will meet
DQOs. The protocol must demonstrate that the planned sampling parameters
calculated by the tester will meet the needs of the source and the
enforcement authority.
12.1.1.2 The pre-test protocol should include information on
equipment, logistics, personnel, process operation, and other resources
necessary for an efficient and coordinated test.
12.1.1.3 At a minimum, the pre-test protocol should identify and be
approved by the source, the tester, the analytical laboratory, and the
regulatory enforcement authority. The tester should not proceed with the
compliance testing before obtaining approval from the enforcement
authority.
12.1.2 Post Test Calculations.
12.1.2.1 Perform the calculations, retaining one extra decimal
figure beyond that of the acquired data. Round off figures after final
calculations.
12.1.2.2 Nomenclature.
CS = Concentration of Cr in sample solution, [micro]g Cr/mL.
Ccr = Concentration of Cr in stack gas, dry basis, corrected
to standard conditions, mg/dscm.
D = Digestion factor, dimension less.
F = Dilution factor, dimension less.
MCr = Total Cr in each sample, [micro]g.
Vad = Volume of sample aliquot after digestion, mL.
Vaf = Volume of sample aliquot after dilution, mL.
Vbd = Volume of sample aliquot submitted to digestion, mL.
Vbf = Volume of sample aliquot before dilution, mL.
VmL = Volume of impinger contents plus rinses, mL.
Vm(std) = Volume of gas sample measured by the dry gas meter,
corrected to standard conditions, dscm.
12.1.2.3 Dilution Factor. The dilution factor is the ratio of the
volume of sample aliquot after dilution to the volume before dilution.
This ratio is given by the following equation:
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[GRAPHIC] [TIFF OMITTED] TR17OC00.573
12.1.2.4 Digestion Factor. The digestion factor is the ratio of the
volume of sample aliquot after digestion to the volume before digestion.
This ratio is given by Equation 306-2.
[GRAPHIC] [TIFF OMITTED] TR17OC00.574
12.1.2.5 Total Cr in Sample. Calculate MCr, the total [micro]g Cr in
each sample, using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.575
12.1.2.6 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. Same as Method 5.
12.1.2.7 Dry Gas Volume, Volume of Water Vapor, Moisture Content.
Same as Method 5.
12.1.2.8 Cr Emission Concentration (CCr). Calculate
CCr, the Cr concentration in the stack gas, in mg/dscm on a
dry basis, corrected to standard conditions using the following
equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.576
12.1.2.9 Isokinetic Variation, Acceptable Results. Same as Method 5.
13.0 Method Performance
13.1 Range. The recommended working range for all of the three
analytical techniques starts at five times the analytical detection
limit (see also Section 13.2.2). The upper limit of all three techniques
can be extended indefinitely by appropriate dilution.
13.2 Sensitivity.
13.2.1 Analytical Sensitivity. The estimated instrumental detection
limits listed are provided as a guide for an instrumental limit. The
actual method detection limits are sample and instrument dependent and
may vary as the sample matrix varies.
13.2.1.2 ICP Analytical Sensitivity. The minimum estimated detection
limits for ICP, as reported in Method 6010A and the recently revised
Method 6010B of SW-846 (Reference 1), are 7.0 [micro]g Cr/L and 4.7
[micro]g Cr/L, respectively.
13.2.1.3 GFAAS Analytical Sensitivity. The minimum estimated
detection limit for GFAAS, as reported in Methods 7000A and 7191 of SW-
846 (Reference 1), is 1 [micro]g Cr/L.
13.2.1.4 IC/PCR Analytical Sensitivity. The minimum detection limit
for IC/PCR with a preconcentrator, as reported in Methods 0061 and 7199
of SW-846 (Reference 1), is 0.05 [micro]g Cr\+6\/L.
1.3.2.1.5 Determination of Detection Limits. The laboratory
performing the Cr\+6\ measurements must determine the method detection
limit on a quarterly basis using a suitable procedure such as that found
in 40 CFR, Part 136, Appendix B. The determination should be made on
samples in the appropriate alkaline matrix. Normally this involves the
preparation (if applicable) and consecutive measurement of seven (7)
separate aliquots of a sample with a concentration <5 times the expected
detection limit. The detection limit is 3.14 times the standard
deviation of these results.
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13.2.2 In-stack Sensitivity. The in-stack sensitivity depends upon
the analytical detection limit, the volume of stack gas sampled, the
total volume of the impinger absorbing solution plus the rinses, and, in
some cases, dilution or concentration factors from sample preparation.
Using the analytical detection limits given in Sections 13.2.1.1,
13.2.1.2, and 13.2.1.3; a stack gas sample volume of 1.7 dscm; a total
liquid sample volume of 500 mL; and the digestion concentration factor
of 1/2 for the GFAAS analysis; the corresponding in-stack detection
limits are 0.0014 mg Cr/dscm to 0.0021 mg Cr/dscm for ICP, 0.00015 mg
Cr/dscm for GFAAS, and 0.000015 mg Cr\+6\/dscm for IC/PCR with
preconcentration.
Note: It is recommended that the concentration of Cr in the
analytical solutions be at least five times the analytical detection
limit to optimize sensitivity in the analyses. Using this guideline and
the same assumptions for impinger sample volume, stack gas sample
volume, and the digestion concentration factor for the GFAAS analysis
(500 mL,1.7 dscm, and 1/2, respectively), the recommended minimum stack
concentrations for optimum sensitivity are 0.0068 mg Cr/dscm to 0.0103
mg Cr/dscm for ICP, 0.00074 mg Cr/dscm for GFAAS, and 0.000074 mg
Cr\+6\/dscm for IC/PCR with preconcentration. If required, the in-stack
detection limits can be improved by either increasing the stack gas
sample volume, further reducing the volume of the digested sample for
GFAAS, improving the analytical detection limits, or any combination of
the three.
13.3 Precision.
13.3.1 The following precision data have been reported for the three
analytical methods. In each case, when the sampling precision is
combined with the reported analytical precision, the resulting overall
precision may decrease.
13.3.2 Bias data is also reported for GFAAS.
13.4 ICP Precision.
13.4.1 As reported in Method 6010B of SW-846 (Reference 1), in an
EPA round-robin Phase 1 study, seven laboratories applied the ICP
technique to acid/distilled water matrices that had been spiked with
various metal concentrates. For true values of 10, 50, and 150 [micro]g
Cr/L; the mean reported values were 10, 50, and 149 [micro]g Cr/L; and
the mean percent relative standard deviations were 18, 3.3, and 3.8
percent, respectively.
13.4.2 In another multi laboratory study cited in Method 6010B, a
mean relative standard of 8.2 percent was reported for an aqueous sample
concentration of approximately 3750 [micro]g Cr/L.
13.5 GFAAS Precision. As reported in Method 7191 of SW-846
(Reference 1), in a single laboratory (EMSL), using Cincinnati, Ohio tap
water spiked at concentrations of 19, 48, and 77 [micro]g Cr/L, the
standard deviations were 0.1, 0.2, and 0.8, respectively.
Recoveries at these levels were 97 percent, 101 percent, and 102
percent, respectively.
13.6 IC/PCR Precision. As reported in Methods 0061 and 7199 of SW-
846 (Reference 1), the precision of IC/PCR with sample preconcentration
is 5 to 10 percent. The overall precision for sewage sludge incinerators
emitting 120 ng/dscm of Cr+6 and 3.5 [micro]g/dscm of total
Cr was 25 percent and 9 percent, respectively; and for hazardous waste
incinerators emitting 300 ng/dscm of C+6 the precision was 20
percent.
14.0 Pollution Prevention
14.1 The only materials used in this method that could be considered
pollutants are the chromium standards used for instrument calibration
and acids used in the cleaning of the collection and measurement
containers/labware, in the preparation of standards, and in the acid
digestion of samples. Both reagents can be stored in the same waste
container.
14.2 Cleaning solutions containing acids should be prepared in
volumes consistent with use to minimize the disposal of excessive
volumes of acid.
14.3 To the extent possible, the containers/vessels used to collect
and prepare samples should be cleaned and reused to minimize the
generation of solid waste.
15.0 Waste Management
15.1 It is the responsibility of the laboratory and the sampling
team to comply with all federal, state, and local regulations governing
waste management, particularly the discharge regulations, hazardous
waste identification rules, and land disposal restrictions; and to
protect the air, water, and land by minimizing and controlling all
releases from field operations.
15.2 For further information on waste management, consult The Waste
Management Manual for Laboratory Personnel and Less is Better--
Laboratory Chemical Management for Waste Reduction, available from the
American Chemical Society's Department of Government Relations and
Science Policy, 1155 16th Street NW, Washington, DC 20036.
16.0 References
1. ``Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods, SW-846, Third Edition,'' as amended by Updates I, II, IIA, IIB,
and III. Document No. 955-001-000001. Available from Superintendent of
Documents, U.S. Government Printing Office, Washington, DC, November
1986.
2. Cox, X.B., R.W. Linton, and F.E. Butler. Determination of
Chromium Speciation in Environmental Particles--A Multi-technique
[[Page 205]]
Study of Ferrochrome Smelter Dust. Accepted for publication in
Environmental Science and Technology.
3. Same as Section 17.0 of Method 5, References 2, 3, 4, 5, and 7.
4. California Air Resources Board, ``Determination of Total Chromium
and Hexavalent Chromium Emissions from Stationary Sources.'' Method 425,
September 12, 1990.
5. The Merck Index. Eleventh Edition. Merck & Co., Inc., 1989.
6. Walpole, R.E., and R.H. Myers. ``Probability and Statistics for
Scientists and Engineering.'' 3rd Edition. MacMillan Publishing Co.,
NewYork, N.Y., 1985.
17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.577
[[Page 206]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.578
Method 306A--Determination of Chromium Emissions From Decorative and
Hard Chromium Electroplating and Chromium Anodizing Operations
Note: This method does not include all of the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical)
essential to its performance. Some material is incorporated by reference
from other methods in 40 CFR Part 60, Appendix A and in this part.
Therefore, to obtain reliable results, persons using this method should
have a thorough knowledge of at least Methods 5 and 306.
1.0 Scope and Application
1.1 Analyte. Chromium. CAS Number (7440-47-3).
1.2 Applicability.
1.2.1 This method applies to the determination of chromium (Cr) in
emissions from decorative and hard chromium electroplating facilities,
chromium anodizing operations, and continuous chromium plating at iron
and steel facilities. The method is less expensive and less complex to
conduct than Method 306. Correctly applied, the precision and bias of
the sample results should be comparable to those obtained with the
isokinetic Method 306. This method is applicable for the determination
of air emissions under nominal ambient moisture, temperature, and
pressure conditions.
1.2.2 The method is also applicable to electroplating and anodizing
sources controlled by wet scrubbers.
1.3 Data Quality Objectives.
1.3.1 Pretest Protocol.
[[Page 207]]
1.3.1.1 The pretest protocol should define and address the test data
quality objectives (DQOs), with all assumptions, that will be required
by the end user (enforcement authority); what data are needed? why are
the data needed? how will data be used? what are method detection
limits? and what are estimated target analyte levels for the following
test parameters.
1.3.1.1.1 Estimated source concentration for total chromium and/or
Cr\+6\.
1.3.1.1.2 Estimated minimum sampling time and/or volume required to
meet method detection limit requirements (Appendix B 40 CFR Part 136)
for measurement of total chromium and/or Cr\+6\.
1.3.1.1.3 Demonstrate that planned sampling parameters will meet
DQOs. The protocol must demonstrate that the planned sampling parameters
calculated by the tester will meet the needs of the source and the
enforcement authority.
1.3.1.2 The pre-test protocol should include information on
equipment, logistics, personnel, process operation, and other resources
necessary for an efficient and coordinated performance test.
1.3.1.3 At a minimum, the pre-test protocol should identify and be
approved by the source, the tester, the analytical laboratory, and the
regulatory enforcement authority. The tester should not proceed with the
compliance testing before obtaining approval from the enforcement
authority.
2.0 Summary of Method
2.1 Sampling.
2.1.1 An emission sample is extracted from the source at a constant
sampling rate determined by a critical orifice and collected in a
sampling train composed of a probe and impingers. The proportional
sampling time at the cross sectional traverse points is varied according
to the stack gas velocity at each point. The total sample time must be
at least two hours.
2.1.2 The chromium emission concentration is determined by the same
analytical procedures described in Method 306: inductively-coupled
plasma emission spectrometry (ICP), graphite furnace atomic absorption
spectrometry (GFAAS), or ion chromatography with a post-column reactor
(IC/PCR).
2.1.2.1 Total chromium samples with high chromium concentrations
(=35 [micro]g/L) may be analyzed using inductively coupled
plasma emission spectrometry (ICP) at 267.72 nm.
Note: The ICP analysis is applicable for this method only when the
solution analyzed has a Cr concentration greater than or equal to 35
[micro]g/L or five times the method detection limit as determined
according to Appendix B in 40 CFR Part 136.
2.1.2.2 Alternatively, when lower total chromium concentrations (<35
[micro]g/L) are encountered, a portion of the alkaline sample solution
may be digested with nitric acid and analyzed by graphite furnace atomic
absorption spectroscopy (GFAAS) at 357.9 nm.
2.1.2.3 If it is desirable to determine hexavalent chromium (Cr\+6\)
emissions, the samples may be analyzed using an ion chromatograph
equipped with a post-column reactor (IC/PCR) and a visible wavelength
detector. To increase sensitivity for trace levels of Cr\+6\, a
preconcentration system may be used in conjunction with the IC/PCR.
3.0 Definitions
3.1 Total Chromium--measured chromium content that includes both
major chromium oxidation states (Cr+3, Cr+6).
3.2 May--Implies an optional operation.
3.3 Digestion--The analytical operation involving the complete (or
nearly complete) dissolution of the sample in order to ensure the
complete solubilization of the element (analyte) to be measured.
3.4 Interferences--Physical, chemical, or spectral phenomena that
may produce a high or low bias in the analytical result.
3.5 Analytical System--All components of the analytical process
including the sample digestion and measurement apparatus.
3.6 Sample Recovery--The quantitative transfer of sample from the
collection apparatus to the sample preparation (digestion, etc.)
apparatus. This term should not be confused with analytical recovery.
4.0 Interferences
4.1 Same as in Method 306, Section 4.0.
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method does not purport to address
all of the safety issues associated with its use. It is the
responsibility of the user to establish appropriate safety and health
practices and to determine the applicability of regulatory limitations
prior to performing this test method.
5.2 Chromium and some chromium compounds have been listed as
carcinogens although Chromium (III) compounds show little or no
toxicity. Chromium is a skin and respiratory irritant.
6.0 Equipment and Supplies
Note: Mention of trade names or specific products does not
constitute endorsement by the Environmental Protection Agency.
6.1 Sampling Train. A schematic of the sampling train is shown in
Figure 306A-1. The individual components of the train are available
commercially, however, some fabrication and assembly are required.
6.1.1 Probe Nozzle/Tubing and Sheath.
6.1.1.1 Use approximately 6.4-mm (\1/4\-in.) inside diameter (ID)
glass or rigid plastic tubing approximately 20 cm (8 in.) in length
[[Page 208]]
with a short 90 degree bend at one end to form the sampling nozzle.
Grind a slight taper on the nozzle end before making the bend. Attach
the nozzle to flexible tubing of sufficient length to enable collection
of a sample from the stack.
6.1.1.2 Use a straight piece of larger diameter rigid tubing (such
as metal conduit or plastic water pipe) to form a sheath that begins
about 2.5 cm (1 in.) from the 90 [deg] bend on the nozzle and encases
and supports the flexible tubing.
6.1.2 Type S Pitot Tube. Same as Method 2, Section 6.1 (40 CFR Part
60, Appendix A).
6.1.3 Temperature Sensor.
6.1.3.1 A thermocouple, liquid-filled bulb thermometer, bimetallic
thermometer, mercury-in-glass thermometer, or other sensor capable of
measuring temperature to within 1.5 percent of the minimum absolute
stack temperature.
6.1.3.2 The temperature sensor shall either be positioned near the
center of the stack, or be attached to the pitot tube as directed in
Section 6.3 of Method 2.
6.1.4 Sample Train Connectors.
6.1.4.1 Use thick wall flexible plastic tubing (polyethylene,
polypropylene, or polyvinyl chloride) 6.4-mm (\1/4\-in.) to 9.5-mm (\3/
8\-in.) ID to connect the train components.
6.1.4.2 A combination of rigid plastic tubing and thin wall flexible
tubing may be used as long as tubing walls do not collapse when leak-
checking the train. Metal tubing cannot be used.
6.1.5 Impingers. Three, one-quart capacity, glass canning jars with
vacuum seal lids, or three Greenburg-Smith (GS) design impingers
connected in series, or equivalent, may be used.
6.1.5.1 One-quart glass canning jar. Three separate jar containers
are required: (1) the first jar contains the absorbing solution; (2) the
second is empty and is used to collect any reagent carried over from the
first container; and (3) the third contains the desiccant drying agent.
6.1.5.2 Canning Jar Connectors. The jar containers are connected by
leak-tight inlet and outlet tubes installed in the lids of each
container for assembly with the train. The tubes may be made of 6.4 mm
(\1/4\-in.) ID glass or rigid plastic tubing. For the inlet tube of the
first impinger, heat the glass or plastic tubing and draw until the
tubing separates. Fabricate the necked tip to form an orifice tip that
is approximately 2.4 mm (\3/32\-in.) ID.
6.1.5.2.1 When assembling the first container, place the orifice tip
end of the tube approximately 4.8 mm (\3/16\-in.) above the inside
bottom of the jar.
6.1.5.2.2 For the second container, the inlet tube need not be drawn
and sized, but the tip should be approximately 25 mm (1 in.) above the
bottom of the jar.
6.1.5.2.3 The inlet tube of the third container should extend to
approximately 12.7 mm (\1/2\-in.) above the bottom of the jar.
6.1.5.2.4 Extend the outlet tube for each container approximately 50
mm (2 in.) above the jar lid and downward through the lid, approximately
12.7 mm (\1/2\-in.) beneath the bottom of the lid.
6.1.5.3 Greenburg-Smith Impingers. Three separate impingers of the
Greenburg-Smith (GS) design as described in Section 6.0 of Method 5 are
required. The first GS impinger shall have a standard tip (orifice/
plate), and the second and third GS impingers shall be modified by
replacing the orifice/plate tube with a 13 mm (\1/2\-in.) ID glass tube,
having an unrestricted opening located 13 mm (\1/2\-in.) from the bottom
of the outer flask.
6.1.5.4 Greenburg-Smith Connectors. The GS impingers shall be
connected by leak-free ground glass ``U'' tube connectors or by leak-
free non-contaminating flexible tubing. The first impinger shall contain
the absorbing solution, the second is empty and the third contains the
desiccant drying agent.
6.1.6 Manometer. Inclined/vertical type, or equivalent device, as
described in Section 6.2 of Method 2 (40 CFR Part 60, Appendix A).
6.1.7 Critical Orifice. The critical orifice is a small restriction
in the sample line that is located upstream of the vacuum pump. The
orifice produces a constant sampling flow rate that is approximately
0.021 cubic meters per minute (m3/min) or 0.75 cubic feet per minute
(cfm).
6.1.7.1 The critical orifice can be constructed by sealing a 2.4-mm
(\3/32\-in.) ID brass tube approximately 14.3 mm (\9/16\-in.) in length
inside a second brass tube that is approximately 8 mm (\5/16\-in.) ID
and 14.3-mm (\9/16\-in.) in length .
6.1.7.2 Materials other than brass can be used to construct the
critical orifice as long as the flow through the sampling train can be
maintained at approximately 0.021 cubic meter per minute (0.75) cfm.
6.1.8 Connecting Hardware. Standard pipe and fittings, 9.5-mm (\3/
8\-in.), 6.4-mm (\1/4\-in.) or 3.2-mm (\1/8\-in.) ID, may be used to
assemble the vacuum pump, dry gas meter and other sampling train
components.
6.1.9 Vacuum Gauge. Capable of measuring approximately 760 mm
Hg (30 in. Hg) vacuum in 25.4 mm HG (1
in. Hg) increments. Locate vacuum gauge between the critical
orifice and the vacuum pump.
6.1.10 Pump Oiler. A glass oil reservoir with a wick mounted at the
vacuum pump inlet that lubricates the pump vanes. The oiler should be an
in-line type and not vented to the atmosphere. See EMTIC Guideline
Document No. GD-041.WPD for additional information.
6.1.11 Vacuum Pump. Gast Model 0522-V103-G18DX, or equivalent,
capable of delivering at least 1.5 cfm at 15 in. Hg vacuum.
[[Page 209]]
6.1.12 Oil Trap/Muffler. An empty glass oil reservoir without wick
mounted at the pump outlet to control the pump noise and prevent oil
from reaching the dry gas meter.
6.1.13 By-pass Fine Adjust Valve (Optional). Needle valve assembly
6.4-mm (\1/4\-in.), Whitey 1 RF 4-A, or equivalent, that allows for
adjustment of the train vacuum.
6.1.13.1 A fine-adjustment valve is positioned in the optional pump
by-pass system that allows the gas flow to recirculate through the pump.
This by-pass system allows the tester to control/reduce the maximum
leak-check vacuum pressure produced by the pump.
6.1.13.1.1 The tester must conduct the post test leak check at a
vacuum equal to or greater than the maximum vacuum encountered during
the sampling run.
6.1.13.1.2 The pump by-pass assembly is not required, but is
recommended if the tester intends to leak-check the 306A train at the
vacuum experienced during a run.
6.1.14 Dry Gas Meter. An Equimeter Model 110 test meter or,
equivalent with temperature sensor(s) installed (inlet/outlet) to
monitor the meter temperature. If only one temperature sensor is
installed, locate the sensor at the outlet side of the meter. The dry
gas meter must be capable of measuring the gaseous volume to within
2% of the true volume.
Note: The Method 306 sampling train is also commercially available
and may be used to perform the Method 306A tests. The sampling train may
be assembled as specified in Method 306A with the sampling rate being
operated at the delta H@ specified for the calibrated orifice
located in the meter box. The Method 306 train is then operated as
described in Method 306A.
6.2 Barometer. Mercury aneroid barometer, or other barometer
equivalent, capable of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
6.2.1 A preliminary check of the barometer shall be made against a
mercury-in-glass reference barometer or its equivalent.
6.2.2 Tester may elect to obtain the absolute barometric pressure
from a nearby National Weather Service station.
6.2.2.1 The station value (which is the absolute barometric
pressure) must be adjusted for elevation differences between the weather
station and the sampling location. Either subtract 2.5 mm Hg
(0.1 in. Hg) from the station value per 30 m (100 ft) of
elevation increase or add the same for an elevation decrease.
6.2.2.2 If the field barometer cannot be adjusted to agree within
0.1 in. Hg of the reference barometric, repair or discard the
unit. The barometer pressure measurement shall be recorded on the
sampling data sheet.
6.3 Sample Recovery. Same as Method 5, Section 6.2 (40 CFR Part 60,
Appendix A), with the following exceptions:
6.3.1 Probe-Liner and Probe-Nozzle Brushes. Brushes are not
necessary for sample recovery. If a probe brush is used, it must be non-
metallic.
6.3.2 Wash Bottles. Polyethylene wash bottle, for sample recovery
absorbing solution.
6.3.3 Sample Recovery Solution. Use 0.1 N NaOH or 0.1 N
NaHCO3, whichever is used as the impinger absorbing solution,
to replace the acetone.
6.3.4 Sample Storage Containers.
6.3.4.1 Glass Canning Jar. The first canning jar container of the
sampling train may serve as the sample shipping container. A new lid and
sealing plastic wrap shall be substituted for the container lid
assembly.
6.3.4.2 Polyethylene or Glass Containers. Transfer the Greenburg-
Smith impinger contents to precleaned polyethylene or glass containers.
The samples shall be stored and shipped in 250-mL, 500-mL or 1000-mL
polyethylene or glass containers with leak-free, non metal screw caps.
6.3.5 pH Indicator Strip, for Cr +6 Samples. pH indicator
strips, or equivalent, capable of determining the pH of solutions
between the range of 7 and 12, at 0.5 pH increments.
6.3.6 Plastic Storage Containers. Air tight containers to store
silica gel.
6.4 Analysis. Same as Method 306, Section 6.3.
7.0 Reagents and Standards.
Note: Unless otherwise indicated, all reagents shall conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society (ACS reagent grade). Where such
specifications are not available, use the best available grade. It is
recommended, but not required, that reagents be checked by the
appropriate analysis prior to field use to assure that contamination is
below the analytical detection limit for the ICP or GFAAS total chromium
analysis; and that contamination is below the analytical detection limit
for Cr+6 using IC/PCR for direct injection or, if selected,
preconcentration.
7.1 Sampling.
7.1.1 Water. Reagent water that conforms to ASTM Specification D1193
Type II (incorporated by reference see Sec. 63.14). All references to
water in the method refer to reagent water unless otherwise specified.
It is recommended that water blanks be checked prior to preparing the
sampling reagents to ensure that the Cr content is less than three (3)
times the anticipated detection limit of the analytical method.
7.1.2 Sodium Hydroxide (NaOH) Absorbing Solution, 0.1 N. Dissolve
4.0 g of sodium hydroxide in 1 liter of water to obtain a pH of
approximately 8.5.
[[Page 210]]
7.1.3 Sodium Bicarbonate (NaHCO3) Absorbing Solution, 0.1
N. Dissolve approximately 8.5 g of sodium bicarbonate in 1 liter of
water to obtain a pH of approximately 8.3.
7.1.4 Chromium Contamination.
7.1.4.1 The absorbing solution shall not exceed the QC criteria
noted in Method 306, Section 7.1.1 (<=3 times the instrument detection
limit).
7.1.4.2 When the Cr+6 content in the field samples
exceeds the blank concentration by at least a factor of ten (10),
Cr+6 blank levels <=10 times the detection limit will be
allowed.
Note: At sources with high concentrations of acids and/or
SO2, the concentration of NaOH or NaHCO3 should be
=0.5 N to insure that the pH of the solution remains at or
above 8.5 for NaOH and 8.0 for NaHCO3 during and after
sampling.
7.1.3 Desiccant. Silica Gel, 6-16 mesh, indicating type.
Alternatively, other types of desiccants may be used, subject to the
approval of the Administrator.
7.2 Sample Recovery. Same as Method 306, Section 7.2.
7.3 Sample Preparation and Analysis. Same as Method 306, Section
7.3.
7.4 Glassware Cleaning Reagents. Same as Method 306, Section 7.4.
7.5 Quality Assurance Audit Samples.
7.5.1 It is recommended, but not required, that a performance audit
sample be analyzed in conjunction with the field samples. The audit
sample should be in a suitable sample matrix at a concentration similar
to the actual field samples.
7.5.2 When making compliance determinations, and upon availability,
audit samples may be obtained from the appropriate EPA regional Office
or from the responsible enforcement authority and analyzed in
conjunction with the field samples.
Note: The responsible enforcement authority should be notified at
least 30 days prior to the test date to allow sufficient time for the
audit sample to be delivered.
8.0 Sample Collection, Recovery, Preservation, Holding Times, Storage,
and Transport
Note: Prior to sample collection, consideration should be given as
to the type of analysis (Cr+6 or total Cr) that will be
performed. Deciding which analysis will be performed will enable the
tester to determine which appropriate sample recovery and storage
procedures will be required to process the sample.
8.1 Sample Collection.
8.1.1 Pretest Preparation.
8.1.1.1 Selection of Measurement Site. Locate the sampling ports as
specified in Section 11.0 of Method 1 (40 CFR Part 60, Appendix A).
8.1.1.2 Location of Traverse Points.
8.1.1.2.1 Locate the traverse points as specified in Section 11.0 of
Method 1 (40 CFR Part 60, Appendix A). Use a total of 24 sampling points
for round ducts and 24 or 25 points for rectangular ducts. Mark the
pitot and sampling probe to identify the sample traversing points.
8.1.1.2.2 For round ducts less than 12 inches in diameter, use a
total of 16 points.
8.1.1.3 Velocity Pressure Traverse. Perform an initial velocity
traverse before obtaining samples. The Figure 306A-2 data sheet may be
used to record velocity traverse data.
8.1.1.3.1 To demonstrate that the flow rate is constant over several
days of testing, perform complete traverses at the beginning and end of
each day's test effort, and calculate the deviation of the flow rate for
each daily period. The beginning and end flow rates are considered
constant if the deviation does not exceed 10 percent. If the flow rate
exceeds the 10 percent criteria, either correct the inconsistent flow
rate problem, or obtain the Administrator's approval for the test
results.
8.1.1.3.2 Perform traverses as specified in Section 8.0 of Method 2,
but record only the [Delta]p (velocity pressure) values for each
sampling point. If a mass emission rate is desired, stack velocity
pressures shall be recorded before and after each test, and an average
stack velocity pressure determined for the testing period.
8.1.1.4 Verification of Absence of Cyclonic Flow. Check for cyclonic
flow during the initial traverse to verify that it does not exist.
Perform the cyclonic flow check as specified in Section 11.4 of Method 1
(40 CFR Part 60, Appendix A).
8.1.1.4.1 If cyclonic flow is present, verify that the absolute
average angle of the tangential flow does not exceed 20 degrees. If the
average value exceeds 20 degrees at the sampling location, the flow
condition in the stack is unacceptable for testing.
8.1.1.4.2 Alternative procedures, subject to approval of the
Administrator, e.g., installing straightening vanes to eliminate the
cyclonic flow, must be implemented prior to conducting the testing.
8.1.1.5 Stack Gas Moisture Measurements. Not required. Measuring the
moisture content is optional when a mass emission rate is to be
calculated.
8.1.1.5.1 The tester may elect to either measure the actual stack
gas moisture during the sampling run or utilize a nominal moisture value
of 2 percent.
8.1.1.5.2 For additional information on determining sampling train
moisture, please refer to Method 4 (40 CFR Part 60, Appendix A).
8.1.1.6 Stack Temperature Measurements. If a mass emission rate is
to be calculated, a temperature sensor must be placed either near the
center of the stack, or attached to the pitot tube as described in
Section 8.3 of Method 2. Stack temperature measurements,
[[Page 211]]
shall be recorded before and after each test, and an average stack
temperature determined for the testing period.
8.1.1.7 Point Sampling Times. Since the sampling rate of the train
(0.75 cfm) is maintained constant by the critical orifice, it is
necessary to calculate specific sampling times for each traverse point
in order to obtain a proportional sample.
8.1.1.7.1 If the sampling period (3 runs) is to be completed in a
single day, the point sampling times shall be calculated only once.
8.1.1.7.2 If the sampling period is to occur over several days, the
sampling times must be calculated daily using the initial velocity
pressure data recorded for that day. Determine the average of the
[Delta]p values obtained during the velocity traverse (Figure 306A-2).
8.1.1.7.3 If the stack diameter is less than 12 inches, use 7.5
minutes in place of 5 minutes in the equation and 16 sampling points
instead of 24 or 25 points. Calculate the sampling times for each
traverse point using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.579
Where:
n = Sampling point number.
[Delta]p = Average pressure differential across pitot tube, mm
H2O (in. H2O).
[Delta]Pavg = Average of [Delta]p values, mm H2O
(in. H2O).
Note: Convert the decimal fractions for minutes to seconds.
8.1.1.8 Pretest Preparation. It is recommended, but not required,
that all items which will be in contact with the sample be cleaned prior
to performing the testing to avoid possible sample contamination
(positive chromium bias). These items include, but are not limited to:
Sampling probe, connecting tubing, impingers, and jar containers.
8.1.1.8.1 Sample train components should be: (1) Rinsed with hot tap
water; (2) washed with hot soapy water; (3) rinsed with tap water; (4)
rinsed with reagent water; (5) soaked in a 10 percent (v/v) nitric acid
solution for at least four hours; and (6) rinsed throughly with reagent
water before use.
8.1.1.8.2 At a minimum, the tester should, rinse the probe,
connecting tubing, and first and second impingers twice with either 0.1
N sodium hydroxide (NaOH) or 0.1 N sodium bicarbonate
(NaHCO3) and discard the rinse solution.
8.1.1.8.3 If separate sample shipping containers are to be used,
these also should be precleaned using the specified cleaning procedures.
8.1.1.9 Preparation of Sampling Train. Assemble the sampling train
as shown in Figure 306A-1. Secure the nozzle-liner assembly to the outer
sheath to prevent movement when sampling.
8.1.1.9.1 Place 250 mL of 0.1 N NaOH or 0.1 N NaHCO3
absorbing solution into the first jar container or impinger. The second
jar/impinger is to remain empty. Place 6 to 16 mesh indicating silica
gel, or equivalent desiccant into the third jar/impinger until the
container is half full ( 300 to 400 g).
8.1.1.9.2 Place a small cotton ball in the outlet exit tube of the
third jar to collect small silica gel particles that may dislodge and
impair the pump and/or gas meter.
8.1.1.10 Pretest Leak-Check. A pretest leak-check is recommended,
but not required. If the tester opts to conduct the pretest leak-check,
the following procedures shall be performed: (1) Place the jar/impinger
containers into an ice bath and wait 10 minutes for the ice to cool the
containers before performing the leak check and/or start sampling; (2)
to perform the leak check, seal the nozzle using a piece of clear
plastic wrap placed over the end of a finger and switch on the pump; and
(3) the train system leak rate should not exceed 0.02 cfm at a vacuum of
380 mm Hg (15 in. Hg) or greater. If the leak rate does exceed the 0.02
cfm requirement, identify and repair the leak area and perform the leak
check again.
Note: Use caution when releasing the vacuum following the leak
check. Always allow air to slowly flow through the nozzle end of the
train system while the pump is still operating. Switching off the pump
with vacuum on the system may result in the silica gel being pulled into
the second jar container.
8.1.1.11 Leak-Checks During Sample Run. If, during the sampling run,
a component (e.g., jar container) exchange becomes necessary, a leak-
check shall be conducted immediately before the component exchange is
made. The leak-check shall be performed according to the procedure
outlined in Section 8.1.1.10 of this method. If the leakage rate is
found to be <= 0.02 cfm at the maximum operating vacuum, the results are
acceptable. If, however, a higher leak rate is obtained, either record
the leakage rate and correct the sample volume as shown in Section 12.3
of
[[Page 212]]
Method 5 or void the sample and initiate a replacement run. Following
the component change, leak-checks are optional, but are recommended as
are the pretest leak-checks.
8.1.1.12 Post Test Leak Check. Remove the probe assembly and
flexible tubing from the first jar/impinger container. Seal the inlet
tube of the first container using clear plastic wrap and switch on the
pump. The vacuum in the line between the pump and the critical orifice
must be =15 in. Hg. Record the vacuum gauge measurement along
with the leak rate observed on the train system.
8.1.1.12.1 If the leak rate does not exceed 0.02 cfm, the results
are acceptable and no sample volume correction is necessary.
8.1.1.12.2 If, however, a higher leak rate is obtained
(0.02 cfm), the tester shall either record the leakage rate
and correct the sample volume as shown in Section 12.3 of Method 5, or
void the sampling run and initiate a replacement run. After completing
the leak-check, slowly release the vacuum at the first container while
the pump is still operating. Afterwards, switch-off the pump.
8.1.2 Sample Train Operation.
8.1.2.1 Data Recording. Record all pertinent process and sampling
data on the data sheet (see Figure 306A-3). Ensure that the process
operation is suitable for sample collection.
8.1.2.2 Starting the Test. Place the probe/nozzle into the duct at
the first sampling point and switch on the pump. Start the sampling
using the time interval calculated for the first point. When the first
point sampling time has been completed, move to the second point and
continue to sample for the time interval calculated for that point;
sample each point on the traverse in this manner. Maintain ice around
the sample containers during the run.
8.1.2.3 Critical Flow. The sample line between the critical orifice
and the pump must operate at a vacuum of = 380 mm Hg
(=15 in. Hg) in order for critical flow to be maintained.
This vacuum must be monitored and documented using the vacuum gauge
located between the critical orifice and the pump.
Note: Theoretically, critical flow for air occurs when the ratio of
the orifice outlet absolute pressure to the orifice inlet absolute
pressure is less than a factor of 0.53. This means that the system
vacuum should be at least = 356 mm Hg (= 14 in.
Hg) at sea level and 305 mm Hg ( 12 in. Hg) at higher elevations.
8.1.2.4 Completion of Test.
8.1.2.4.1 Circular Stacks. Complete the first port traverse and
switch off the pump. Testers may opt to perform a leak-check between the
port changes to verify the leak rate however, this is not mandatory.
Move the sampling train to the next sampling port and repeat the
sequence. Be sure to record the final dry gas meter reading after
completing the test run. After performing the post test leak check,
disconnect the jar/impinger containers from the pump and meter assembly
and transport the probe, connecting tubing, and containers to the sample
recovery area.
8.1.2.4.2 Rectangle Stacks. Complete each port traverse as per the
instructions provided in 8.1.2.4.1.
Note: If an approximate mass emission rate is to be calculated,
measure and record the stack velocity pressure and temperature before
and after the test run.
8.2 Sample Recovery. After the train has been transferred to the
sample recovery area, disconnect the tubing that connects the jar/
impingers. The tester shall select either the total Cr or
Cr+6 sample recovery option. Samples to be analyzed for both
total Cr and Cr+6 shall be recovered using the
Cr+6 sample option (Section 8.2.2).
Note: Collect a reagent blank sample for each of the total Cr or the
Cr+6 analytical options. If both analyses (Cr and
Cr+6) are to be conducted on the samples, collect separate
reagent blanks for each analysis.
8.2.1 Total Cr Sample Option.
8.2.1.1 Shipping Container No. 1. The first jar container may either
be used to store and transport the sample, or if GS impingers are used,
samples may be stored and shipped in precleaned 250-mL, 500-mL or 1000-
mL polyethylene or glass bottles with leak-free, non-metal screw caps.
8.2.1.1.1 Unscrew the lid from the first jar/impinger container.
8.2.1.1.2 Lift the inner tube assembly almost out of the container,
and using the wash bottle containing fresh absorbing solution, rinse the
outside of the tube that was immersed in the container solution; rinse
the inside of the tube as well, by rinsing twice from the top of the
tube down through the inner tube into the container.
8.2.1.2 Recover the contents of the second jar/impinger container by
removing the lid and pouring any contents into the first shipping
container.
8.2.1.2.1 Rinse twice, using fresh absorbing solution, the inner
walls of the second container including the inside and outside of the
inner tube.
8.2.1.2.2 Rinse the connecting tubing between the first and second
sample containers with absorbing solution and place the rinses into the
first container.
8.2.1.3 Position the nozzle, probe and connecting plastic tubing in
a vertical position so that the tubing forms a ``U''.
8.2.1.3.1 Using the wash bottle, partially fill the tubing with
fresh absorbing solution. Raise and lower the end of the plastic tubing
several times to allow the solution to contact the internal surfaces. Do
not allow the solution to overflow or part of the sample will be lost.
Place the nozzle end of the probe
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over the mouth of the first container and elevate the plastic tubing so
that the solution flows into the sample container.
8.2.1.3.2 Repeat the probe/tubing sample recovery procedure but
allow the solution to flow out the opposite end of the plastic tubing
into the sample container. Repeat the entire sample recovery procedure
once again.
8.2.1.4 Use approximately 200 to 300 mL of the 0.1 N NaOH or 0.1 N
NaHCO3 absorbing solution during the rinsing of the probe
nozzle, probe liner, sample containers, and connecting tubing.
8.2.1.5 Place a piece of clear plastic wrap over the mouth of the
sample jar to seal the shipping container. Use a standard lid and band
assembly to seal and secure the sample in the jar.
8.2.1.5.1 Label the jar clearly to identify its contents, sample
number and date.
8.2.1.5.2 Mark the height of the liquid level on the container to
identify any losses during shipping and handling.
8.2.1.5.3 Prepare a chain-of-custody sheet to accompany the sample
to the laboratory.
8.2.2 Cr+6 Sample Option.
8.2.2.1 Shipping Container No. 1. The first jar container may either
be used to store and transport the sample, or if GS impingers are used,
samples may be stored and shipped in precleaned 250-mL, 500-mL or 1000-
mL polyethylene or glass bottles with leak-free non-metal screw caps.
8.2.2.1.1 Unscrew and remove the lid from the first jar container.
8.2.2.1.2 Measure and record the pH of the solution in the first
container by using a pH indicator strip. The pH of the solution must be
=8.5 for NaOH and =8.0 for NaHCO3. If
not, discard the collected sample, increase the concentration of the
NaOH or NaHCO3 absorbing solution to 0.5 M and collect another air
emission sample.
8.2.2.2 After measuring the pH of the first container, follow sample
recovery procedures described in Sections 8.2.1.1 through 8.2.1.5.
Note: Since particulate matter is not usually present at chromium
electroplating and/or chromium anodizing facilities, it is not necessary
to filter the Cr+6 samples unless there is observed sediment
in the collected solutions. If it is necessary to filter the
Cr+6 solutions, please refer to the EPA Method 0061,
Determination of Hexavalent Chromium Emissions from Stationary Sources,
Section 7.4, Sample Preparation in SW-846 (see Reference 5) for
procedure.
8.2.3 Silica Gel Container. Observe the color of the indicating
silica gel to determine if it has been completely spent and make a
notation of its condition/color on the field data sheet. Do not use
water or other liquids to remove and transfer the silica gel.
8.2.4 Total Cr and/or Cr+6 Reagent Blank.
8.2.4.1 Shipping Container No. 2. Place approximately 500 mL of the
0.1 N NaOH or 0.1 N NaHCO3 absorbing solution in a
precleaned, labeled sample container and include with the field samples
for analysis.
8.3 Sample Preservation, Storage, and Transport.
8.3.1 Total Cr Option. Samples that are to be analyzed for total Cr
need not be refrigerated.
8.3.2 Cr+6 Option. Samples that are to be analyzed for
Cr+6 must be shipped and stored at 4 [deg]C (40 [deg]F).
Note: Allow Cr+6 samples to return to ambient temperature
prior to analysis.
8.4 Sample Holding Times.
8.4.1 Total Cr Option. Samples that are to be analyzed for total
chromium must be analyzed within 60 days of collection.
8.4.2 Cr+6 Option. Samples that are to be analyzed for
Cr+6 must be analyzed within 14 days of collection.
9.0 Quality Control
9.1 Same as Method 306, Section 9.0.
10.0 Calibration and Standardization
Note: Tester shall maintain a performance log of all calibration
results.
10.1 Pitot Tube. The Type S pitot tube assembly shall be calibrated
according to the procedures outlined in Section 10.1 of Method 2.
10.2 Temperature Sensor. Use the procedure in Section 10.3 of Method
2 to calibrate the in-stack temperature sensor.
10.3 Metering System.
10.3.1 Sample Train Dry Gas Meter Calibration. Calibrations may be
performed as described in Section 16.2 of Method 5 by either the
manufacturer, a firm who provides calibration services, or the tester.
10.3.2 Dry Gas Meter Calibration Coefficient (Ym). The
meter calibration coefficient (Ym) must be determined prior
to the initial use of the meter, and following each field test program.
If the dry gas meter is new, the manufacturer will have specified the
Ym value for the meter. This Ym value can be used
as the pretest value for the first test. For subsequent tests, the
tester must use the Ym value established during the pretest
calibration.
10.3.3 Calibration Orifice. The manufacturer may have included a
calibration orifice and a summary spreadsheet with the meter that may be
used for calibration purposes. The spreadsheet will provide data
necessary to determine the calibration for the orifice and meter
(standard cubic feet volume, sample time, etc.). These data were
produced when the initial Ym value was determined for the
meter.
10.3.4 Ym Meter Value Verification or Meter Calibration.
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10.3.4.1 The Ym meter value may be determined by
replacing the sampling train critical orifice with the calibration
orifice. Replace the critical orifice assembly by installing the
calibration orifice in the same location. The inlet side of the
calibration orifice is to be left open to the atmosphere and is not to
be reconnected to the sample train during the calibration procedure.
10.3.4.2 If the vacuum pump is cold, switch on the pump and allow it
to operate (become warm) for several minutes prior to starting the
calibration. After stopping the pump, record the initial dry gas meter
volume and meter temperature.
10.3.4.3 Perform the calibration for the number of minutes specified
by the manufacturer's data sheet (usually 5 minutes). Stop the pump and
record the final dry gas meter volume and temperature. Subtract the
start volume from the stop volume to obtain the Vm and
average the meter temperatures (tm).
10.3.5 Ym Value Calculation. Ym is the
calculated value for the dry gas meter. Calculate Ym using
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.580
Where:
Pbar = Barometric pressure at meter, mm Hg, (in. Hg).
Pstd = Standard absolute pressure,
Metric = 760 mm Hg.
English = 29.92 in. Hg.
tm = Average dry gas meter temperature, [deg]C, ([deg]F).
Tm = Absolute average dry gas meter temperature,
Metric [deg]K = 273 + tm ([deg]C).
English [deg]R = 460 + tm([deg]F).
Tstd = Standard absolute temperature,
Metric = 293 [deg]K.
English = 528 [deg]R.
Vm = Volume of gas sample as measured (actual) by dry gas
meter, dcm,(dcf).
Vm(std),mfg = Volume of gas sample measured by manufacture's
calibrated orifice and dry gas meter, corrected to standard conditions
(pressure/temperature) dscm (dscf).
Ym = Dry gas meter calibration factor, (dimensionless).
10.3.6 Ym Comparison. Compare the Ym value
provided by the manufacturer (Section 10.3.3) or the pretest
Ym value to the post test Ym value using the
following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.581
10.3.6.1 If this ratio is between 0.95 and 1.05, the designated
Ym value for the meter is acceptable for use in later
calculations.
10.3.6.1.1 If the value is outside the specified range, the test
series shall either be: 1) voided and the samples discarded; or 2)
calculations for the test series shall be conducted using whichever
meter coefficient value (i.e., manufacturers's/pretest Ym
value or post test Ym value) produces the lowest sample
volume.
10.3.6.1.2 If the post test dry gas meter Ym value
differs by more than 5% as compared to the pretest value, either perform
the calibration again to determine acceptability or return the meter to
the manufacturer for recalibration.
10.3.6.1.3 The calibration may also be conducted as specified in
Section 10.3 or Section 16.0 of Method 5 (40 CFR Part 60, Appendix A),
except that it is only necessary to check the calibration at one flow
rate of 0.75 cfm.
10.3.6.1.4 The calibration of the dry gas meter must be verified
after each field test program using the same procedures.
Note: The tester may elect to use the Ym post test value
for the next pretest Ym value; e.g., Test 1 post test
Ym value and Test 2 pretest Ym value would be the
same.
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10.4 Barometer. Calibrate against a mercury barometer that has been
corrected for temperature and elevation.
10.5 ICP Spectrometer Calibration. Same as Method 306, Section 10.2.
10.6 GFAA Spectrometer Calibration. Same as Method 306, Section
10.3.
10.7 IC/PCR Calibration. Same as Method 306, Section 10.4.
11.0 Analytical Procedures
Note: The method determines the chromium concentration in [micro]g
Cr/mL. It is important that the analyst measure the volume of the field
sample prior to analyzing the sample. This will allow for conversion of
[micro]g Cr/mL to [micro]g Cr/sample.
11.1 Analysis. Refer to Method 306 for sample preparation and
analysis procedures.
12.0 Data Analysis and Calculations
12.1 Calculations. Perform the calculations, retaining one extra
decimal point beyond that of the acquired data. When reporting final
results, round number of figures consistent with the original data.
12.2 Nomenclature.
A = Cross-sectional area of stack, m2 (ft2).
Bws = Water vapor in gas stream, proportion by volume,
dimensionless (assume 2 percent moisture = 0.02).
Cp = Pitot tube coefficient; ``S'' type pitot coefficient
usually 0.840, dimensionless.
CS = Concentration of Cr in sample solution, [micro]g Cr/mL.
CCr = Concentration of Cr in stack gas, dry basis, corrected
to standard conditions [micro]g/dscm (gr/dscf).
d = Diameter of stack, m (ft).
D = Digestion factor, dimensionless.
ER = Approximate mass emission rate, mg/hr (lb/hr).
F = Dilution factor, dimensionless.
L = Length of a square or rectangular duct, m (ft).
MCr = Total Cr in each sample, [micro]g (gr).
Ms = Molecular weight of wet stack gas, wet basis, g/g-mole,
(lb/lb-mole); in a nominal gas stream at 2% moisture the value is 28.62.
Pbar = Barometric pressure at sampling site, mm Hg (in. Hg).
Ps = Absolute stack gas pressure; in this case, usually the
same value as the barometric pressure, mm Hg (in. Hg).
Pstd = Standard absolute pressure:
Metric = 760 mm Hg.
English = 29.92 in. Hg.
Qstd = Average stack gas volumetric flow, dry, corrected to
standard conditions, dscm/hr (dscf/hr).
tm = Average dry gas meter temperature, [deg]C ([deg]F).
Tm = Absolute average dry gas meter temperature:
Metric [deg]K = 273 + tm ([deg]C).
English [deg]R = 460 + tm([deg]F).
ts = Average stack temperature, [deg]C ([deg]F).
Ts = Absolute average stack gas temperature: Metric [deg]K =
273 + ts ([deg]C). English [deg]R = 460 +
ts([deg]F).
Tstd = Standard absolute temperature: Metric = 293 [deg]K.
English = 528 [deg]R.
Vad = Volume of sample aliquot after digestion (mL).
Vaf = Volume of sample aliquot after dilution (mL).
Vbd = Volume of sample aliquot submitted to digestion (mL).
Vbf = Volume of sample aliquot before dilution (mL).
Vm = Volume of gas sample as measured (actual, dry) by dry
gas meter, dcm (dcf).
VmL = Volume of impinger contents plus rinses (mL).
Vm(std) = Volume of gas sample measured by the dry gas meter,
corrected to standard conditions (temperature/pressure), dscm (dscf).
vs = Stack gas average velocity, calculated by Method 2,
Equation 2-9, m/sec (ft/sec).
W = Width of a square or rectangular duct, m (ft).
Ym = Dry gas meter calibration factor, (dimensionless).
[Delta]p = Velocity head measured by the Type S pitot tube, cm
H2O (in. H2O).
[Delta]pavg = Average of [Delta]p values, mm H2O
(in. H2O).
12.3 Dilution Factor. The dilution factor is the ratio of the volume
of sample aliquot after dilution to the volume before dilution. The
dilution factor is usually calculated by the laboratory. This ratio is
derived by the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.582
12.4 Digestion Factor. The digestion factor is the ratio of the
volume of sample aliquot after digestion to the volume before digestion.
The digestion factor is usually calculated by the laboratory. This ratio
is derived by the following equation.
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[GRAPHIC] [TIFF OMITTED] TR17OC00.583
12.5 Total Cr in Sample. Calculate MCr, the total
[micro]g Cr in each sample, using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.584
12.6 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 [deg]C, 760 mm Hg or 68 [deg]F,
29.92 in. Hg) using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.585
Where:
K1 = Metric units--0.3855 [deg]K/mm Hg.
English units--17.64 [deg]R/in. Hg.
12.7 Cr Emission Concentration (CCr). Calculate
CCr, the Cr concentration in the stack gas, in [micro]g/dscm
([micro]g/dscf) on a dry basis, corrected to standard conditions, using
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.586
Note: To convert [micro]g/dscm ([micro]g/dscf) to mg/dscm (mg/dscf),
divide by 1000.
12.8 Stack Gas Velocity.
12.8.1 Kp = Velocity equation constant:
[GRAPHIC] [TIFF OMITTED] TR17OC00.587
[GRAPHIC] [TIFF OMITTED] TR17OC00.588
12.8.2 Average Stack Gas Velocity.
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[GRAPHIC] [TIFF OMITTED] TR17OC00.589
12.9 Cross sectional area of stack.
[GRAPHIC] [TIFF OMITTED] TR17OC00.591
12.10 Average Stack Gas Dry Volumetric Flow Rate.
Note: The emission rate may be based on a nominal stack moisture
content of 2 percent (0.02). To calculate an emission rate, the tester
may elect to use either the nominal stack gas moisture value or the
actual stack gas moisture collected during the sampling run.
Volumetric Flow Rate Equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.592
Where:
3600 = Conversion factor, sec/hr.
[GRAPHIC] [TIFF OMITTED] TR17OC00.593
Note: To convert Qstd from dscm/hr (dscf/hr) to dscm/min
(dscf/min), divide Qstd by 60.
12.11 Mass emission rate, mg/hr (lb/hr):
[GRAPHIC] [TIFF OMITTED] TR17OC00.594
[GRAPHIC] [TIFF OMITTED] TR17OC00.595
13.0 Method Performance
13.1 Range. The recommended working range for all of the three
analytical techniques starts at five times the analytical detection
limit (see also Method 306, Section 13.2.2). The upper limit of all
three techniques can be extended indefinitely by appropriate dilution.
13.2 Sensitivity.
13.2.1 Analytical Sensitivity. The estimated instrumental detection
limits listed are provided as a guide for an instrumental limit. The
actual method detection limits
[[Page 218]]
are sample and instrument dependent and may vary as the sample matrix
varies.
13.2.1.1 ICP Analytical Sensitivity. The minimum estimated detection
limits for ICP, as reported in Method 6010A and the recently revised
Method 6010B of SW-846 (Reference 1), are 7.0 [micro]g Cr/L and 4.7
[micro]g Cr/L, respectively.
13.2.1.2 GFAAS Analytical Sensitivity. The minimum estimated
detection limit for GFAAS, as reported in Methods 7000A and 7191 of SW-
846 (Reference 1), is 1.0 [micro]g Cr/L.
13.2.1.3 IC/PCR Analytical Sensitivity. The minimum detection limit
for IC/PCR with a preconcentrator, as reported in Methods 0061 and 7199
of SW-846 (Reference 1), is 0.05 [micro]g Cr+6/L.
13.2.2 In-stack Sensitivity. The in-stack sensitivity depends upon
the analytical detection limit, the volume of stack gas sampled, and the
total volume of the impinger absorbing solution plus the rinses. Using
the analytical detection limits given in Sections 13.2.1.1, 13.2.1.2,
and 13.2.1.3; a stack gas sample volume of 1.7 dscm; and a total liquid
sample volume of 500 mL; the corresponding in-stack detection limits are
0.0014 mg Cr/dscm to 0.0021 mg Cr/dscm for ICP, 0.00029 mg Cr/dscm for
GFAAS, and 0.000015 mg Cr+36/dscm for IC/PCR with
preconcentration.
Note: It is recommended that the concentration of Cr in the
analytical solutions be at least five times the analytical detection
limit to optimize sensitivity in the analyses. Using this guideline and
the same assumptions for impinger sample volume and stack gas sample
volume (500 mL and 1.7 dscm, respectively), the recommended minimum
stack concentrations for optimum sensitivity are 0.0068 mg Cr/dscm to
0.0103 mg Cr/dscm for ICP, 0.0015 mg Cr/dscm for GFAAS, and 0.000074 mg
Cr+6 dscm for IC/PCR with preconcentration. If required, the
in-stack detection limits can be improved by either increasing the
sampling time, the stack gas sample volume, reducing the volume of the
digested sample for GFAAS, improving the analytical detection limits, or
any combination of the three.
13.3 Precision.
13.3.1 The following precision data have been reported for the three
analytical methods. In each case, when the sampling precision is
combined with the reported analytical precision, the resulting overall
precision may decrease.
13.3.2 Bias data is also reported for GFAAS.
13.4 ICP Precision.
13.4.1 As reported in Method 6010B of SW-846 (Reference 1), in an
EPA round-robin Phase 1 study, seven laboratories applied the ICP
technique to acid/distilled water matrices that had been spiked with
various metal concentrates. For true values of 10, 50, and 150 [micro]g
Cr/L; the mean reported values were 10, 50, and 149 [micro]g Cr/L; and
the mean percent relative standard deviations were 18, 3.3, and 3.8
percent, respectively.
13.4.2 In another multilaboratory study cited in Method 6010B, a
mean relative standard of 8.2 percent was reported for an aqueous sample
concentration of approximately 3750 [micro]g Cr/L.
13.5 GFAAS Precision. As reported in Method 7191 of SW-846
(Reference 1), in a single laboratory (EMSL), using Cincinnati, Ohio tap
water spiked at concentrations of 19, 48, and 77 [micro]g Cr/L, the
standard deviations were 0.1, 0.2, and 0.8, respectively.
Recoveries at these levels were 97 percent, 101 percent, and 102
percent, respectively.
13.6 IC/PCR Precision. As reported in Methods 0061 and 7199 of SW-
846 (Reference 1), the precision of IC/PCR with sample preconcentration
is 5 to 10 percent; the overall precision for sewage sludge incinerators
emitting 120 ng/dscm of Cr+6 and 3.5 [micro]g/dscm of total
Cr is 25 percent and 9 percent, respectively; and for hazardous waste
incinerators emitting 300 ng/dscm of Cr+6 the precision is 20
percent.
14.0 Pollution Prevention
14.1 The only materials used in this method that could be considered
pollutants are the chromium standards used for instrument calibration
and acids used in the cleaning of the collection and measurement
containers/labware, in the preparation of standards, and in the acid
digestion of samples. Both reagents can be stored in the same waste
container.
14.2 Cleaning solutions containing acids should be prepared in
volumes consistent with use to minimize the disposal of excessive
volumes of acid.
14.3 To the extent possible, the containers/vessels used to collect
and prepare samples should be cleaned and reused to minimize the
generation of solid waste.
15.0 Waste Management
15.1 It is the responsibility of the laboratory and the sampling
team to comply with all federal, state, and local regulations governing
waste management, particularly the discharge regulations, hazardous
waste identification rules, and land disposal restrictions; and to
protect the air, water, and land by minimizing and controlling all
releases from field operations.
15.2 For further information on waste management, consult The Waste
Management Manual for Laboratory Personnel and Less is Better-Laboratory
Chemical Management for Waste Reduction, available from the American
Chemical Society's Department of Government Relations and Science
Policy, 1155 16th Street NW, Washington, DC 20036.
[[Page 219]]
16.0 References
1. F.R. Clay, Memo, Impinger Collection Efficiency--Mason Jars vs.
Greenburg-Smith Impingers, Dec. 1989.
2. Segall, R.R., W.G. DeWees, F.R. Clay, and J.W. Brown. Development
of Screening Methods for Use in Chromium Emissions Measurement and
Regulations Enforcement. In: Proceedings of the 1989 EPA/A&WMA
International Symposium-Measurement of Toxic and Related Air Pollutants,
A&WMA Publication VIP-13, EPA Report No. 600/9-89-060, p. 785.
3. Clay, F.R., Chromium Sampling Method. In: Proceedings of the 1990
EPA/A&WMA International Symposium-Measurement of Toxic and Related Air
Pollutants, A&WMA Publication VIP-17, EPA Report No. 600/9-90-026, p.
576.
4. Clay, F.R., Proposed Sampling Method 306A for the Determination
of Hexavalent Chromium Emissions from Electroplating and Anodizing
Facilities. In: Proceedings of the 1992 EPA/A&WMA International
Symposium-Measurement of Toxic and Related Air Pollutants, A&WMA
Publication VIP-25, EPA Report No. 600/R-92/131, p. 209.
5. Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods, SW-846, Third Edition as amended by Updates I, II, IIA, IIB,
and III. Document No. 955-001-000001. Available from Superintendent of
Documents, U.S. Government Printing Office, Washington, DC, November
1986.
17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.596
[[Page 220]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.597
[[Page 221]]
[GRAPHIC] [TIFF OMITTED] TR17OC00.598
Method 306B--Surface Tension Measurement for Tanks Used at Decorative
Chromium Electroplating and Chromium Anodizing Facilities
Note: This method does not include all of the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical)
essential to its performance. Some material is incorporated by reference
from other methods in 40 CFR Part 60, Appendix A and in this part.
Therefore, to obtain reliable results, persons using this method should
have a thorough knowledge of at least Methods 5 and 306.
1.0 Scope and Application
1.1 Analyte. Not applicable.
1.2 Applicability. This method is applicable to all decorative
chromium plating and chromium anodizing operations, and continuous
chromium plating at iron and steel facilities where a wetting agent is
used in the tank as the primary mechanism for reducing emissions from
the surface of the plating solution.
2.0 Summary of Method
2.1 During an electroplating or anodizing operation, gas bubbles
generated during the process rise to the surface of the liquid and
burst. Upon bursting, tiny droplets of chromic acid become entrained in
ambient air. The addition of a wetting agent to the tank bath reduces
the surface tension of the liquid and diminishes the formation of these
droplets.
2.2 This method determines the surface tension of the bath using a
stalagmometer or
[[Page 222]]
a tensiometer to confirm that there is sufficient wetting agent present.
3.0 Definitions [Reserved]
4.0 Interferences [Reserved]
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of the
user to establish appropriate safety and health practices and to
determine the applicability of regulatory limitations prior to
performing this test method.
6.0 Equipment and Supplies
6.1 Stalagmometer. Any commercially available stalagmometer or
equivalent surface tension measuring device may be used to measure the
surface tension of the plating or anodizing tank liquid.
6.2 Tensiometer. A tensiometer may be used to measure the surface
tension of the tank liquid provided the procedures specified in ASTM
Method D 1331-89, Standard Test Methods for Surface and Interfacial
Tension of Solutions of Surface Active Agents (incorporated by
reference--see Sec. 63.14) are followed.
7.0 Reagents and Standards [Reserved]
8.0 Sample Collection, Sample Recovery, Sample Preservation, Sample
Holding Times, Storage, and Transport [Reserved]
9.0 Quality Control [Reserved]
10.0 Calibration and Standardization [Reserved]
11.0 Analytical Procedure
11.1 Procedure. The surface tension of the tank bath may be measured
by using a tensiometer, a stalagmometer or any other equivalent surface
tension measuring device approved by the Administrator for measuring
surface tension in dynes per centimeter. If the tensiometer is used, the
procedures specified in ASTM Method D 1331-89 must be followed. If a
stalagmometer or other device is used to measure surface tension, the
instructions provided with the measuring device must be followed.
11.2 Frequency of Measurements.
11.2.1 Measurements of the bath surface tension are performed using
a progressive system which decreases the frequency of surface tension
measurements required when the proper surface tension is maintained.
11.2.1.1 Initially, following the compliance date, surface tension
measurements must be conducted once every 4 hours of tank operation for
the first 40 hours of tank operation.
11.2.1.2 Once there are no exceedances during a period of 40 hours
of tank operation, measurements may be conducted once every 8 hours of
tank operation.
11.2.1.3 Once there are no exceedances during a second period of 40
consecutive hours of tank operation, measurements may be conducted once
every 40 hours of tank operation on an on-going basis, until an
exceedance occurs. The maximum time interval for measurements is once
every 40 hours of tank operation.
11.2.2 If a measurement of the surface tension of the solution is
above the 45 dynes per centimeter limit, or above an alternate surface
tension limit established during the performance test, the time interval
shall revert back to the original monitoring schedule of once every 4
hours. A subsequent decrease in frequency would then be allowed
according to Section 11.2.1.
12.0 Data Analysis and Calculations
12.1 Log Book of Surface Tension Measurements and Fume Suppressant
Additions.
12.1.1 The surface tension of the plating or anodizing tank bath
must be measured as specified in Section 11.2.
12.1.2 The measurements must be recorded in the log book. In
addition to the record of surface tension measurements, the frequency of
fume suppressant maintenance additions and the amount of fume
suppressant added during each maintenance addition must be recorded in
the log book.
12.1.3 The log book will be readily available for inspection by
regulatory personnel.
12.2 Instructions for Apparatus Used in Measuring Surface Tension.
12.2.1 Included with the log book must be a copy of the instructions
for the apparatus used for measuring the surface tension of the plating
or anodizing bath.
12.2.2 If a tensiometer is used, a copy of ASTM Method D 1331-89
must be included with the log book.
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 References [Reserved]
17.0 Tables, Diagrams, Flowcharts, and Validation Data [Reserved]
Method 307--Determination of Emissions From Halogenated Solvent Vapor
Cleaning Machines Using a Liquid Level Procedure
1. Applicability and Principle
1.1 Applicability. This method is applicable to the determination of
the halogenated solvent emissions from solvent vapor cleaners in the
idling mode.
[[Page 223]]
1.2 Principle. The solvent level in the solvent cleaning machine is
measured using inclined liquid level indicators. The change in liquid
level corresponds directly to the amount of solvent lost from the
solvent cleaning machine.
2. Apparatus
Note: Mention of trade names or specific products does not
constitute endorsement by the Environmental Protection Agency.
2.1 Inclined Liquid Level Indicator. A schematic of the inclined
liquid level indicators used in this method is shown in figure 307-1;
two inclined liquid level indicators having 0.05 centimeters divisions
or smaller shall be used. The liquid level indicators shall be made of
glass, Teflon, or any similar material that will not react with the
solvent being used. A 6-inch by 1-inch slope is recommended; however the
slope may vary depending on the size and design of the solvent cleaning
machine.
Note: It is important that the inclined liquid level indicators be
constructed with ease of reading in mind. The inclined liquid level
indicators should also be mounted so that they can be raised or lowered
if necessary to suit the solvent cleaning machine size.
[GRAPHIC] [TIFF OMITTED] TC01MY92.075
2.2 Horizontal Indicator. Device to check the inclined liquid level
indicators orientation relative to horizontal.
2.3 Velocity Meter. Hotwire and vane anemometers, or other devices
capable of measuring the flow rates ranging from 0 to 15.2 meters per
minute across the solvent cleaning machine.
3. Procedure
3.1 Connection of the Inclined Liquid Level Indicator. Connect one
of the inclined liquid level indicators to the boiling sump drain and
the other inclined liquid level indicator to the immersion sump drain
using Teflon tubing and the appropriate fittings. A schematic diagram is
shown in figure 307-2.
[GRAPHIC] [TIFF OMITTED] TC01MY92.076
3.2 Positioning of Velocity Meter. Position the velocity meter so
that it measures the flow rate of the air passing directly across the
solvent cleaning machine.
3.3 Level the Inclined Liquid Level Indicators.
3.4 Initial Inclined Liquid Level Indicator Readings. Open the sump
drainage valves. Allow the solvent cleaning machine to operate long
enough for the vapor zone to form and the system to stabilize (check
with manufacturer). Record the inclined liquid level
[[Page 224]]
indicators readings and the starting time on the data sheet. A sample
data sheet is provided in figure 307-3.
Date____________________________________________________________________
Run_____________________________________________________________________
Solvent type____________________________________________________________
Solvent density, g/m \3\ (lb/ft \3\)____________________________________
Length of boiling sump (SB), m (ft)__________________________
Width of boiling sump (WB), m (ft)___________________________
Length of immersion sump (SI), m (ft)________________________
Width of immersion sump (WI), m (ft)_________________________
Length of solvent vapor/air interface (SV), m (ft) ----------
--
Width of solvent vapor/air interface (WV), m (ft) ----------
--
------------------------------------------------------------------------
Boiling Immersion
Clock time sump sump Flow rate
reading reading reading
------------------------------------------------------------------------
------------------------------------------------------------------------
Figure 307-3. Data sheet.
3.5 Final Inclined Liquid Level Indicator Readings. At the end of
the 16-hour test run, check to make sure the inclined liquid level
indicators are level; if not, make the necessary adjustments. Record the
final inclined liquid level indicators readings and time.
3.6 Determination of Solvent Vapor/Air Interface Area for Each Sump.
Determine the area of the solvent/air interface of the individual sumps.
Whenever possible, physically measure these dimensions, rather than
using factory specifications. A schematic of the dimensions of a solvent
cleaning machine is provided in figure 307-4.
[GRAPHIC] [TIFF OMITTED] TC01MY92.077
4. Calculations
4.1 Nomenclature.
AB = area of boiling sump interface, m\2\ (ft\2\).
AI = area of immersion sump interface, m\2\ (ft\2\).
AV = area of solvent/air interface, m\2\ (ft\2\).
E = emission rate, kg/m\2\-hr (lb/ft\2\-hr).
K = 100,000 cm . g/m . kg for metric units.
= 12 in./ft for English units.
LBF = final boiling sump inclined liquid level indicators
reading, cm (in.).
LBi = initial boiling sump inclined liquid level indicators
reading, cm (in.).
LIf = final immersion sump inclined liquid level indicators
reading, cm (in.).
LIi = initial immersion sump inclined liquid level indicators
reading, cm (in.).
SB = length of the boiling sump, m (ft).
SI = length of the immersion sump, m (ft).
SV = length of the solvent vapor/air interface, m (ft).
WB = width of the boiling sump, m (ft).
WI = width of the immersion sump, m (ft).
WV = width of the solvent vapor/air interface, m (ft).
[rho] = density of solvent, g/m3 (lb/ft3).
[thetas] = test time, hr.
4.2 Area of Sump Interfaces. Calculate the areas of the boiling and
immersion sump interfaces as follows:
AB = SB WB Eq. 307-1
AI = SI WI Eq. 307-2
4.3 Area of Solvent/Air Interface. Calculate the area of the solvent
vapor/air interface as follows:
AV = SV WV Eq. 307-3
4.4 Emission Rate. Calculate the emission rate as follows:
[GRAPHIC] [TIFF OMITTED] TR02DE94.007
[[Page 225]]
Method 308--Procedure for Determination of Methanol Emission From
Stationary Sources
1.0 Scope and Application
1.1 Analyte. Methanol. Chemical Abstract Service (CAS) No. 67-56-1.
1.2 Applicability. This method applies to the measurement of
methanol emissions from specified stationary sources.
2.0 Summary of Method
A gas sample is extracted from the sampling point in the stack. The
methanol is collected in deionized distilled water and adsorbed on
silica gel. The sample is returned to the laboratory where the methanol
in the water fraction is separated from other organic compounds with a
gas chromatograph (GC) and is then measured by a flame ionization
detector (FID). The fraction adsorbed on silica gel is extracted with an
aqueous solution of n-propanol and is then separated and measured by GC/
FID.
3.0 Definitions [Reserved]
4.0 Interferences [Reserved]
5.0 Safety
5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method does not purport to address
all of the safety problems associated with its use. It is the
responsibility of the user of this test method to establish appropriate
safety and health practices and to determine the applicability of
regulatory limitations before performing this test method.
5.2 Methanol Characteristics. Methanol is flammable and a dangerous
fire and explosion risk. It is moderately toxic by ingestion and
inhalation.
6.0 Equipment and Supplies
6.1 Sample Collection. The following items are required for sample
collection:
6.1.1 Sampling Train. The sampling train is shown in Figure 308-1
and component parts are discussed below.
6.1.1.1 Probe. Teflon[reg], approximately 6-millimeter
(mm) (0.24 inch) outside diameter.
6.1.1.2 Impinger. A 30-milliliter (ml) midget impinger. The impinger
must be connected with leak-free glass connectors. Silicone grease may
not be used to lubricate the connectors.
6.1.1.3 Adsorbent Tube. Glass tubes packed with the required amount
of the specified adsorbent.
6.1.1.4 Valve. Needle valve, to regulate sample gas flow rate.
6.1.1.5 Pump. Leak-free diaphragm pump, or equivalent, to pull gas
through the sampling train. Install a small surge tank between the pump
and rate meter to eliminate the pulsation effect of the diaphragm pump
on the rotameter.
6.1.1.6 Rate Meter. Rotameter, or equivalent, capable of measuring
flow rate to within 2 percent of the selected flow rate of up to 1000
milliliter per minute (ml/min). Alternatively, the tester may use a
critical orifice to set the flow rate.
6.1.1.7 Volume Meter. Dry gas meter (DGM), sufficiently accurate to
measure the sample volume to within 2 percent, calibrated at the
selected flow rate and conditions actually encountered during sampling,
and equipped with a temperature sensor (dial thermometer, or equivalent)
capable of measuring temperature accurately to within 3 [deg]C (5.4
[deg]F).
6.1.1.8 Barometer. Mercury (Hg), aneroid, or other barometer capable
of measuring atmospheric pressure to within 2.5 mm (0.1 inch) Hg. See
the NOTE in Method 5 (40 CFR part 60, appendix A), section 6.1.2.
6.1.1.9 Vacuum Gauge and Rotameter. At least 760-mm (30-inch) Hg
gauge and 0- to 40-ml/min rotameter, to be used for leak-check of the
sampling train.
6.2 Sample Recovery. The following items are required for sample
recovery:
6.2.1 Wash Bottles. Polyethylene or glass, 500-ml, two.
6.2.2 Sample Vials. Glass, 40-ml, with Teflon[reg]-lined
septa, to store impinger samples (one per sample).
6.2.3 Graduated Cylinder. 100-ml size.
6.3 Analysis. The following are required for analysis:
6.3.1 Gas Chromatograph. GC with an FID, programmable temperature
control, and heated liquid injection port.
6.3.2 Pump. Capable of pumping 100 ml/min. For flushing sample loop.
6.3.3 Flow Meter. To monitor accurately sample loop flow rate of 100
ml/min.
6.3.4 Regulators. Two-stage regulators used on gas cylinders for GC
and for cylinder standards.
6.3.5 Recorder. To record, integrate, and store chromatograms.
6.3.6 Syringes. 1.0- and 10-microliter (l) size, calibrated, for
injecting samples.
6.3.7 Tubing Fittings. Stainless steel, to plumb GC and gas
cylinders.
6.3.8 Vials. Two 5.0-ml glass vials with screw caps fitted with
Teflon[reg]-lined septa for each sample.
6.3.9 Pipettes. Volumetric type, assorted sizes for preparing
calibration standards.
6.3.10 Volumetric Flasks. Assorted sizes for preparing calibration
standards.
6.3.11 Vials. Glass 40-ml with Teflon[reg]-lined septa,
to store calibration standards (one per standard).
7.0 Reagents and Standards
Note: Unless otherwise indicated, all reagents must conform to the
specifications
[[Page 226]]
established by the Committee on Analytical Reagents of the American
Chemical Society. Where such specifications are not available, use the
best available grade.
7.1 Sampling. The following are required for sampling:
7.1.1 Water. Deionized distilled to conform to the American Society
for Testing and Materials (ASTM) Specification D 1193-77, Type 3. At the
option of the analyst, the potassium permanganate (KMnO4)
test for oxidizable organic matter may be omitted when high
concentrations of organic matter are not expected to be present.
7.1.2 Silica Gel. Deactivated chromatographic grade 20/40 mesh
silica gel packed in glass adsorbent tubes. The silica gel is packed in
two sections. The front section contains 520 milligrams (mg) of silica
gel, and the back section contains 260 mg.
7.2 Analysis. The following are required for analysis:
7.2.1 Water. Same as specified in section 7.1.1.
7.2.2 n-Propanol, 3 Percent. Mix 3 ml of n-propanol with 97 ml of
water.
7.2.3 Methanol Stock Standard. Prepare a methanol stock standard by
weighing 1 gram of methanol into a 100-ml volumetric flask. Dilute to
100 ml with water.
7.2.3.1 Methanol Working Standard. Prepare a methanol working
standard by pipetting 1 ml of the methanol stock standard into a 100-ml
volumetric flask. Dilute the solution to 100 ml with water.
7.2.3.2 Methanol Standards For Impinger Samples. Prepare a series of
methanol standards by pipetting 1, 2, 5, 10, and 25 ml of methanol
working standard solution respectively into five 50-ml volumetric
flasks. Dilute the solutions to 50 ml with water. These standards will
have 2, 4, 10, 20, and 50 [micro]g/ml of methanol, respectively. After
preparation, transfer the solutions to 40-ml glass vials capped with
Teflon[reg] septa and store the vials under refrigeration.
Discard any excess solution.
7.2.3.3 Methanol Standards for Adsorbent Tube Samples. Prepare a
series of methanol standards by first pipetting 10 ml of the methanol
working standard into a 100-ml volumetric flask and diluting the
contents to exactly 100 ml with 3 percent n-propanol solution. This
standard will contain 10 [micro]g/ml of methanol. Pipette 5, 15, and 25
ml of this standard, respectively, into four 50-ml volumetric flasks.
Dilute each solution to 50 ml with 3 percent n-propanol solution. These
standards will have 1, 3, and 5 [micro]g/ml of methanol, respectively.
Transfer all four standards into 40-ml glass vials capped with
Teflon[reg]-lined septa and store under refrigeration.
Discard any excess solution.
7.2.4 GC Column. Capillary column, 30 meters (100 feet) long with an
inside diameter (ID) of 0.53 mm (0.02 inch), coated with DB 624 to a
film thickness of 3.0 micrometers, ([micro]m) or an equivalent column.
Alternatively, a 30-meter capillary column coated with polyethylene
glycol to a film thickness of 1 [micro]m such as AT-WAX or its
equivalent.
7.2.5 Helium. Ultra high purity.
7.2.6 Hydrogen. Zero grade.
7.2.7 Oxygen. Zero grade.
8.0 Procedure
8.1 Sampling. The following items are required for sampling:
8.1.1 Preparation of Collection Train. Measure 20 ml of water into
the midget impinger. The adsorbent tube must contain 520 mg of silica
gel in the front section and 260 mg of silica gel in the backup section.
Assemble the train as shown in Figure 308-1. An optional, second
impinger that is left empty may be placed in front of the water-
containing impinger to act as a condensate trap. Place crushed ice and
water around the impinger.
[[Page 227]]
[GRAPHIC] [TIFF OMITTED] TR15AP98.014
8.1.2 Leak Check. A leak check prior to the sampling run is
optional; however, a leak check after the sampling run is mandatory. The
leak-check procedure is as follows:
Temporarily attach a suitable (e.g., 0-to 40-ml/min) rotameter to
the outlet of the DGM, and place a vacuum gauge at or near the probe
inlet. Plug the probe inlet, pull a vacuum of at least 250 mm (10 inch)
Hg, and note the flow rate as indicated by the rotameter. A leakage rate
not in excess of 2 percent of the average sampling rate is acceptable.
Note: Carefully release the probe inlet plug before turning off the
pump.
8.1.3 Sample Collection. Record the initial DGM reading and
barometric pressure. To begin sampling, position the tip of the
Teflon[reg] tubing at the sampling point, connect the tubing
to the impinger, and start the pump. Adjust the sample flow to a
constant rate between 200 and 1000 ml/min as indicated by the rotameter.
Maintain this constant rate (10 percent) during
the entire sampling run. Take readings (DGM, temperatures at DGM and at
impinger outlet, and rate meter) at least every 5 minutes. Add more ice
during the run to keep the temperature of the gases leaving the last
impinger at 20 [deg]C (68 [deg]F) or less. At the conclusion of each
run,
[[Page 228]]
turn off the pump, remove the Teflon[reg] tubing from the
stack, and record the final readings. Conduct a leak check as in section
8.1.2. (This leak check is mandatory.) If a leak is found, void the test
run or use procedures acceptable to the Administrator to adjust the
sample volume for the leakage.
8.2 Sample Recovery. The following items are required for sample
recovery:
8.2.1 Impinger. Disconnect the impinger. Pour the contents of the
midget impinger into a graduated cylinder. Rinse the midget impinger and
the connecting tubes with water, and add the rinses to the graduated
cylinder. Record the sample volume. Transfer the sample to a glass vial
and cap with a Teflon[reg] septum. Discard any excess sample.
Place the samples in an ice chest for shipment to the laboratory.
8.2.2. Adsorbent Tubes. Seal the silica gel adsorbent tubes and
place them in an ice chest for shipment to the laboratory.
9.0 Quality Control
9.1 Miscellaneous Quality Control Measures. The following quality
control measures are required:
------------------------------------------------------------------------
Section Quality control measure Effect
------------------------------------------------------------------------
8.1.2, 8.1.3, 10.1.. Sampling equipment leak Ensures accurate
check and calibration. measurement of sample
volume.
10.2................ GC calibration.......... Ensures precision of GC
analysis.
------------------------------------------------------------------------
9.2 Applicability. When the method is used to analyze samples to
demonstrate compliance with a source emission regulation, an audit
sample must be analyzed, subject to availability.
9.3 Audit Procedure. Analyze an audit sample with each set of
compliance samples. Concurrently analyze the audit sample and a set of
compliance samples in the same manner to evaluate the technique of the
analyst and the standards preparation. The same analyst, analytical
reagents, and analytical system shall be used both for the compliance
samples and the EPA audit sample.
9.4 Audit Sample Availability. Audit samples will be supplied only
to enforcement agencies for compliance tests. Audit samples may be
obtained by writing: Source Test Audit Coordinator (MD-77B), Air
Measurement Research Division, National Exposure Research Laboratory,
U.S. Environmental Protection Agency, Research Triangle Park, NC 27711;
or by calling the Source Test Audit Coordinator (STAC) at (919) 541-
7834. The audit sample request must be made at least 30 days prior to
the scheduled compliance sample analysis.
9.5 Audit Results. Calculate the audit sample concentration
according to the calculation procedure provided in the audit
instructions included with the audit sample. Fill in the audit sample
concentration and the analyst's name on the audit response form included
with the audit instructions. Send one copy to the EPA Regional Office or
the appropriate enforcement agency and a second copy to the STAC. The
EPA Regional office or the appropriate enforcement agency will report
the results of the audit to the laboratory being audited. Include this
response with the results of the compliance samples in relevant reports
to the EPA Regional Office or the appropriate enforcement agency.
10.0 Calibration and Standardization
10.1 Metering System. The following items are required for the
metering system:
10.1.1 Initial Calibration.
10.1.1.1 Before its initial use in the field, first leak-check the
metering system (drying tube, needle valve, pump, rotameter, and DGM) as
follows: Place a vacuum gauge at the inlet to the drying tube, and pull
a vacuum of 250 mm (10 inch) Hg; plug or pinch off the outlet of the
flow meter, and then turn off the pump. The vacuum shall remain stable
for at least 30 seconds. Carefully release the vacuum gauge before
releasing the flow meter end.
10.1.1.2 Next, remove the drying tube, and calibrate the metering
system (at the sampling flow rate specified by the method) as follows:
Connect an appropriately sized wet test meter (e.g., 1 liter per
revolution (0.035 cubic feet per revolution)) to the inlet of the drying
tube. Make three independent calibrations runs, using at least five
revolutions of the DGM per run. Calculate the calibration factor, Y (wet
test meter calibration volume divided by the DGM volume, both volumes
adjusted to the same reference temperature and pressure), for each run,
and average the results. If any Y-value deviates by more than 2 percent
from the average, the metering system is unacceptable for use.
Otherwise, use the average as the calibration factor for subsequent test
runs.
10.1.2 Posttest Calibration Check. After each field test series,
conduct a calibration check as in section 10.1.1 above, except for the
following variations: (a) The leak check is not to be conducted, (b)
three, or more revolutions of the DGM may be used, and (c) only two
independent runs need be made. If the calibration factor does not
deviate by more than 5 percent from the initial calibration factor
(determined in section 10.1.1), then the DGM volumes obtained during the
test series are acceptable. If the calibration factor deviates by more
than 5 percent, recalibrate the metering system as in section 10.1.1,
and for the calculations, use the calibration factor (initial or
recalibration) that yields the lower gas volume for each test run.
10.1.3 Temperature Sensors. Calibrate against mercury-in-glass
thermometers.
[[Page 229]]
10.1.4 Rotameter. The rotameter need not be calibrated, but should
be cleaned and maintained according to the manufacturer's instruction.
10.1.5 Barometer. Calibrate against a mercury barometer.
10.2 Gas Chromatograph. The following procedures are required for
the gas chromatograph:
10.2.1 Initial Calibration. Inject 1 [micro]l of each of the
standards prepared in sections 7.2.3.3 and 7.2.3.4 into the GC and
record the response. Repeat the injections for each standard until two
successive injections agree within 5 percent. Using the mean response
for each calibration standard, prepare a linear least squares equation
relating the response to the mass of methanol in the sample. Perform the
calibration before analyzing each set of samples.
10.2.2 Continuing Calibration. At the beginning of each day, analyze
the mid level calibration standard as described in section 10.5.1. The
response from the daily analysis must agree with the response from the
initial calibration within 10 percent. If it does not, the initial
calibration must be repeated.
11.0 Analytical Procedure
11.1 Gas Chromatograph Operating Conditions. The following operating
conditions are required for the GC:
11.1.1 Injector. Configured for capillary column, splitless, 200
[deg]C (392 [deg]F).
11.1.2 Carrier. Helium at 10 ml/min.
11.1.3 Oven. Initially at 45 [deg]C for 3 minutes; then raise by 10
[deg]C to 70 [deg]C; then raise by 70 [deg]C/min to 200 [deg]C.
11.2 Impinger Sample. Inject 1 [micro]l of the stored sample into
the GC. Repeat the injection and average the results. If the sample
response is above that of the highest calibration standard, either
dilute the sample until it is in the measurement range of the
calibration line or prepare additional calibration standards. If the
sample response is below that of the lowest calibration standard,
prepare additional calibration standards. If additional calibration
standards are prepared, there shall be at least two that bracket the
response of the sample. These standards should produce approximately 50
percent and 150 percent of the response of the sample.
11.3 Silica Gel Adsorbent Sample. The following items are required
for the silica gel adsorbent samples:
11.3.1 Preparation of Samples. Extract the front and backup sections
of the adsorbent tube separately. With a file, score the glass adsorbent
tube in front of the first section of silica gel. Break the tube open.
Remove and discard the glass wool. Transfer the first section of the
silica gel to a 5-ml glass vial and stopper the vial. Remove the spacer
between the first and second section of the adsorbent tube and discard
it. Transfer the second section of silica gel to a separate 5-ml glass
vial and stopper the vial.
11.3.2 Desorption of Samples. Add 3 ml of the 10 percent n-propanol
solution to each of the stoppered vials and shake or vibrate the vials
for 30 minutes.
11.3.3 Inject a 1-[micro]l aliquot of the diluted sample from each
vial into the GC. Repeat the injection and average the results. If the
sample response is above that of the highest calibration standard,
either dilute the sample until it is in the measurement range of the
calibration line or prepare additional calibration standards. If the
sample response is below that of the lowest calibration standard,
prepare additional calibration standards. If additional calibration
standards are prepared, there shall be at least two that bracket the
response of the sample. These standards should produce approximately 50
percent and 150 percent of the response of the sample.
12.0 Data Analysis and Calculations
12.1 Nomenclature.
Caf=Concentration of methanol in the front of the adsorbent
tube, [micro]g/ml.
Cab=Concentration of methanol in the back of the adsorbent
tube, [micro]g/ml.
Ci=Concentration of methanol in the impinger portion of the
sample train, [micro]g/ml.
E=Mass emission rate of methanol, [micro]g/hr (lb/hr).
Mtot=Total mass of methanol collected in the sample train,
[micro]g.
Pbar=Barometric pressure at the exit orifice of the DGM, mm
Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qstd=Dry volumetric stack gas flow rate corrected to standard
conditions, dscm/hr (dscf/hr).
Tm=Average DGM absolute temperature, degrees K ([deg]R).
Tstd=Standard absolute temperature, 293 degrees K (528
[deg]R).
Vaf=Volume of front half adsorbent sample, ml.
Vab=Volume of back half adsorbent sample, ml.
Vi=Volume of impinger sample, ml.
Vm=Dry gas volume as measured by the DGM, dry cubic meters
(dcm), dry cubic feet (dcf).
Vm(std)=Dry gas volume measured by the DGM, corrected to
standard conditions, dry standard cubic meters (dscm), dry standard
cubic feet (dscf).
12.2 Mass of Methanol. Calculate the total mass of methanol
collected in the sampling train using Equation 308-1.
[[Page 230]]
[GRAPHIC] [TIFF OMITTED] TR15AP98.015
12.3 Dry Sample Gas Volume, Corrected to Standard Conditions.
Calculate the volume of gas sampled at standard conditions using
Equation 308-2.
[GRAPHIC] [TIFF OMITTED] TR15AP98.016
12.4 Mass Emission Rate of Methanol. Calculate the mass emission
rate of methanol using Equation 308-3.
[GRAPHIC] [TIFF OMITTED] TR15AP98.017
13.0 Method Performance [Reserved]
14.0 Pollution Prevention [Reserved]
15.0 Waste Management [Reserved]
16.0 Bibliography
1. Rom, J.J. ``Maintenance, Calibration, and Operation of Isokinetic
Source Sampling Equipment.'' Office of Air Programs, Environmental
Protection Agency. Research Triangle Park, NC. APTD-0576 March 1972.
2. Annual Book of ASTM Standards. Part 31; Water, Atmospheric
Analysis. American Society for Testing and Materials. Philadelphia, PA.
1974. pp. 40-42.
3. Westlin, P.R. and R.T. Shigehara. ``Procedure for Calibrating and
Using Dry Gas Volume Meters as Calibration Standards.'' Source
Evaluation Society Newsletter. 3(1) :17-30. February 1978.
4. Yu, K.K. ``Evaluation of Moisture Effect on Dry Gas Meter
Calibration.'' Source Evaluation Society Newsletter. 5(1) :24-28.
February 1980.
5. NIOSH Manual of Analytical Methods, Volume 2. U.S. Department of
Health and Human Services National Institute for Occupational Safety and
Health. Center for Disease Control. 4676 Columbia Parkway, Cincinnati,
OH 45226. (available from the Superintendent of Documents, Government
Printing Office, Washington, DC 20402.)
6. Pinkerton, J.E. ``Method for Measuring Methanol in Pulp Mill Vent
Gases.'' National Council of the Pulp and Paper Industry for Air and
Stream Improvement, Inc., New York, NY.
17.0 Tables, Diagrams, Flowcharts, and Validation Data [Reserved]
Method 310A--Determination of Residual Hexane Through Gas Chromatography
1.0 Scope and Application
1.1 This method is used to analyze any crumb rubber or water samples
for residual hexane content.
1.2 The sample is heated in a sealed bottle with an internal
standard and the vapor is analyzed by gas chromatography.
2.0 Summary of Method
2.1 This method, utilizing a capillary column gas chromatograph with
a flame ionization detector, determines the concentration of residual
hexane in rubber crumb samples.
3.0 Definitions
3.1 The definitions are included in the text as needed.
4.0 Interferences
4.1 There are no known interferences.
5.0 Safety
5.1 It is the responsibility of the user of this procedure to
establish safety and health practices applicable to their specific
operation.
6.0 Equipment and Supplies
6.1 Gas Chromatograph with a flame ionization detector and data
handling station equipped with a capillary column 30 meters long.
[[Page 231]]
6.2 Chromatograph conditions for Sigma 1:
6.2.1 Helium pressure: 50 inlet A, 14 aux
6.2.2 Carrier flow: 25 cc/min
6.2.3 Range switch: 100x
6.2.4 DB: 1 capillary column
6.3 Chromatograph conditions for Hewlett-Packard GC:
6.3.1 Initial temperature: 40 [deg]C
6.3.2 Initial time: 8 min
6.3.3 Rate: 0
6.3.4 Range: 2
6.3.5 DB: 1705 capillary column
6.4 Septum bottles and stoppers
6.5 Gas Syringe--0.5 cc
7.0 Reagents and Standards
7.1 Chloroform, 99.9+%, A.S.C. HPLC grade
8.0 Sample Collection, Preservation, and Storage
8.1 A representative sample should be caught in a clean 8 oz.
container with a secure lid.
8.2 The container should be labeled with sample identification, date
and time.
9.0 Quality Control
9.1 The instrument is calibrated by injecting calibration solution
(Section 10.2 of this method) five times.
9.2 The retention time for components of interest and relative
response of monomer to the internal standard is determined.
9.3 Recovery efficiency must be determined once for each sample type
and whenever modifications are made to the method.
9.3.1 Determine the percent hexane in three separate dried rubber
crumb samples.
9.3.2 Weigh a portion of each crumb sample into separate sample
bottles and add a known amount of hexane (10 microliters) by microliter
syringe and 20 microliters of internal standard. Analyze each by the
described procedure and calculate the percent recovery of the known
added hexane.
9.3.3 Repeat the previous step using twice the hexane level (20
microliters), analyze and calculate the percent recovery of the known
added hexane.
9.3.4 Set up two additional sets of samples using 10 microliters and
20 microliters of hexane as before, but add an amount of water equal to
the dry crumb used. Analyze and calculate percent recovery to show the
effect of free water on the results obtained.
9.3.5 A value of R between 0.70 and 1.30 is acceptable.
9.3.6 R shall be used to correct all reported results for each
compound by dividing the measured results of each compound by the R for
that compound for the same sample type.
10.0 Calibration and Instrument Settings
10.1 Calibrate the chromatograph using a standard made by injecting
10 [micro]l of fresh hexane and 20 [micro]l of chloroform into a sealed
septum bottle. This standard will be 0.6 wt.% total hexane based on 1
gram of dry rubber.
10.2 Analyze the hexane used and calculate the percentage of each
hexane isomer (2-methylpentane, 3-methylpentane, n-hexane, and
methylcyclo-pentane). Enter these percentages into the method
calibration table.
10.3 Heat the standard bottle for 30 minutes in a 105 [deg]C oven.
10.4 Inject about 0.25 cc of vapor into the gas chromatograph and
after the analysis is finished, calibrate according to the procedures
described by the instrument manufacturer.
11.0 Procedure
11.1 Using a cold mill set at a wide roller gap (125-150 mm), mill
about 250 grams of crumb two times to homogenize the sample.
11.2 Weigh about 2 grams of wet crumb into a septum bottle and cap
with a septum ring. Add 20 [micro]l of chloroform with a syringe and
place in a 105 [deg]C oven for 45 minutes.
11.3 Run the moisture content on a separate portion of the sample
and calculate the grams of dry rubber put into the septum bottle.
11.4 Set up the data station on the required method and enter the
dry rubber weight in the sample weight field.
11.5 Inject a 0.25 cc vapor sample into the chromatograph and push
the start button.
11.6 At the end of the analysis, the data station will print a
report listing the concentration of each identified component.
11.7 To analyze water samples, pipet 5 ml of sample into the septum
bottle, cap and add 20 [micro]l of chloroform. Place in a 105 [deg]C
oven for 30 minutes.
11.8 Enter 5 grams into the sample weight field.
11.9 Inject a 0.25 cc vapor sample into the chromatograph and push
the start button.
11.10 At the end of the analysis, the data station will print a
report listing the concentration of each identified component.
12.0 Data Analysis and Calculation
12.1 For samples that are prepared as in section 11 of this method,
ppm n-hexane is read directly from the computer.
12.2 The formulas for calculation of the results are as follows:
ppmhexane=(AhexanexRhexane)/
(AisxRis)
Where:
Ahexane=area of hexane
Rhexane=response of hexane
Ais=area of the internal standard
Ris=response of the internal standard
[[Page 232]]
% hexane in crumb=(ppmhexane/sample amount)100
12.3 Correct the results by the value of R (as determined in
sections 9.3.4, 9.3.5, and 9.3.6 of this method).
13.0 Method Performance
13.1 The test has a standard deviation of 0.14 wt% at 0.66 wt%
hexane. Spike recovery of 12 samples at two levels of hexane averaged
102.3%. Note: Recovery must be determined for each type of sample. The
values given here are meant to be examples of method performance.
14.0 Pollution Prevention
14.1 Waste generation should be minimized where possible. Sample
size should be an amount necessary to adequately run the analysis.
15.0 Waste Management
15.1 All waste shall be handled in accordance with federal and state
environmental regulations.
16.0 References and Publications
16.1 DSM Copolymer Test Method T-3380.
Method 310B--Determination of Residual Hexane Through Gas Chromatography
1.0 Scope and Application
----------------------------------------------------------------------------------------------------------------
Method sensitivity (5.5g
Analyte CAS No. Matrix sample size)
----------------------------------------------------------------------------------------------------------------
Hexane................................... 110-54-3 Rubber crumb............. .01 wt%.
Applicable Termonomer.................... .............. Rubber crumb............. .001 wt%.
----------------------------------------------------------------------------------------------------------------
1.1 Data Quality Objectives:
In the production of ethylene-propylene terpolymer crumb rubber, the
polymer is recovered from solution by flashing off the solvent with
steam and hot water. The resulting water-crumb slurry is then pumped to
the finishing units. Certain amounts of solvent (hexane being the most
commonly used solvent) and diene monomer remain in the crumb. The
analyst uses the following procedure to determine those amounts.
2.0 Summary of Method
2.1 The crumb rubber sample is dissolved in toluene to which heptane
has been added as an internal standard. Acetone is then added to this
solution to precipitate the crumb, and the supernatant is analyzed for
hexane and diene by a gas chromatograph equipped with a flame ionization
detector (FID).
3.0 Definitions
3.1 Included in text as needed.
4.0 Interferences
4.1 None known.
4.2 Benzene, introduced as a contaminant in the toluene solvent,
elutes between methyl cyclopentane and cyclohexane. However, the benzene
peak is completely resolved.
4.3 2,2-dimethyl pentane, a minor component of the hexane used in
our process, elutes just prior to methyl cyclopentane. It is included as
``hexane'' in the analysis whether it is integrated separately or
included in the methyl cyclopentane peak.
5.0 Safety
5.1 This procedure does not purport to address all of the safety
concerns associated with its use. It is the responsibility of the user
of this procedure to establish appropriate safety and health practices
and determine the applicability of regulatory limitations prior to use.
5.2 Chemicals used in this analysis are flammable and hazardous (see
specific toxicity information below). Avoid contact with sources of
ignition during sample prep. All handling should be done beneath a hood.
Playtex or nitrile gloves recommended.
5.3 Hexane is toxic by ingestion and inhalation. Vapor inhalation
causes irritation of nasal and respiratory passages, headache,
dizziness, nausea, central nervous system depression. Chronic
overexposure can cause severe nerve damage. May cause irritation on
contact with skin or eyes. May cause damage to kidneys.
5.4 Termonomer may be harmful by inhalation, ingestion, or skin
absorption. Vapor or mist is irritating to the eyes, mucous membranes,
and upper respiratory tract. Causes skin irritation.
5.5 Toluene is harmful or fatal if swallowed. Vapor harmful if
inhaled. Symptoms: headache, dizziness, hallucinations, distorted
perceptions, changes in motor activity, nausea, diarrhea, respiratory
irritation, central nervous system depression, unconsciousness, liver,
kidney and lung damage. Contact can cause severe eye irritation. May
cause skin irritation. Causes irritation of eyes, nose, and throat.
[[Page 233]]
5.6 Acetone, at high concentrations or prolonged overexposure, may
cause headache, dizziness, irritation of eyes and respiratory tract,
loss of strength, and narcosis. Eye contact causes severe irritation;
skin contact may cause mild irritation. Concentrations of 20,000 ppm are
immediately dangerous to life and health.
5.7 Heptane is harmful if inhaled or swallowed. May be harmful if
absorbed through the skin. Vapor or mist is irritating to the eyes,
mucous membranes, and upper respiratory tract. Prolonged or repeated
exposure to skin causes defatting and dermatitis.
5.8 The steam oven used to dry the polymer in this procedure is set
at 110 [deg]C. Wear leather gloves when removing bottles from the oven.
6.0 Equipment and Supplies
6.1 4000-ml volumetric flask
6.2 100-ml volumetric pipette
6.3 1000-ml volumetric flask
6.4 8-oz. French Square sample bottles with plastic-lined caps
6.5 Top-loading balance
6.6 Laboratory shaker
6.7 Laboratory oven set at 110 [deg]C (steam oven)
6.8 Gas chromatograph, Hewlett-Packard 5890A, or equivalent,
interfaced with HP 7673A (or equivalent) autosampler (equipped with
nanoliter adapter and robotic arm), and HP 3396 series II or 3392A (or
equivalent) integrator/controller.
6.9 GC column, capillary type, 50m x 0.53mm, methyl silicone, 5
micron film thickness, Quadrex, or equivalent.
6.10 Computerized data acquisition system, such as CIS/CALS
6.11 Crimp-top sample vials and HP p/n 5181-1211 crimp caps, or
screw-top autosampler vials and screw tops.
6.12 Glass syringes, 5-ml, with ``Luer-lock'' fitting
6.13 Filters, PTFE, .45 [micro]m pore size, Gelman Acrodisc or
equivalent, to fit on Luer-lock syringes (in 6.12, above).
7.0 Reagents and Standards
7.1 Reagent toluene, EM Science Omnisolv (or equivalent)
Purity Check: Prior to using any bottle of reagent toluene, analyze
it according to section 11.2 of this method. Use the bottle only if
hexane, heptane, and termonomer peak areas are less than 15 each (note
that an area of 15 is equivalent to less than 0.01 wt% in a 10g sample).
7.2 Reagent acetone, EM Science Omnisolv HR-GC (or equivalent)
Purity Check: Prior to using any bottle of reagent acetone, analyze
it according to section 11.2 of this method. Use the bottle only if
hexane, heptane, and termonomer peak areas are less than 15 each.
7.3 Reagent heptane, Aldrich Chemical Gold Label, Cat
15,487-3 (or equivalent)
Purity Check: Prior to using any bottle of reagent heptane, analyze
it according to section 11.2 of this method. Use the bottle only if
hexane and termonomer peak areas are less than 5 each.
7.4 Internal standard solution--used as a concentrate for
preparation of the more dilute Polymer Dissolving Solution. It contains
12.00g heptane/100ml of solution which is 120.0g per liter.
Preparation of internal standard solution (polymer dissolving stock
solution):
------------------------------------------------------------------------
Action Notes
------------------------------------------------------------------------
7.4.1 Tare a clean, dry 1-liter If the 1-liter volumetric flask
volumetric flask on the balance. is too tall to fit in the
Record the weight to three places. balance case, you can shield
the flask from drafts by
inverting a paint bucket with
a hole cut in the bottom over
the balance cover. Allow the
neck of the flask to project
through the hole in the
bucket.
7.4.2 Weigh 120.00 g of n-heptane into Use 99+% n-heptane from Aldrich
the flask. Record the total weight of or Janssen Chimica.
the flask and heptane as well as the
weight of heptane added.
7.4.3 Fill the flask close to the mark Use EM Science Omnisolve
with toluene, about 1 to 2 toluene, Grade TX0737-1, or
below the mark. equivalent.
7.4.4 Shake the flask vigorously to mix Allow any bubbles to clear
the contents. before proceeding to the next
step.
7.4.5 Top off the flask to the mark
with toluene. Shake vigorously, as in
section 7.4.4 of this method, to mix
well.
7.4.6 Weigh the flask containing the
solution on the three place balance
record the weight
7.4.7 Transfer the contents of the Discard any excess solution
flask to a 1 qt Boston round bottle.
7.4.8 Label the bottle with the Be sure to include the words
identity of the contents, the weights ``Hexane in Crumb Polymer
of heptane and toluene used, the date Dissolving Stock Solution'' on
of preparation and the preparer's name. the label.
7.4.9 Refrigerate the completed blend
for the use of the routine Technicians.
------------------------------------------------------------------------
[[Page 234]]
7.5 Polymer Dissolving Solution (``PDS'')--Heptane (as internal
standard) in toluene. This solution contains 0.3g of heptane internal
standard per 100 ml of solution.
7.5.1 Preparation of Polymer Dissolving Solution. Fill a 4,000-ml
volumetric flask about \3/4\ full with toluene.
7.5.2 Add 100 ml of the internal standard solution (section 7.4 of
this method) to the flask using the 100ml pipette.
7.5.3 Fill the flask to the mark with toluene. Discard any excess.
7.5.4 Add a large magnetic stirring bar to the flask and mix by
stirring.
7.5.5 Transfer the polymer solvent solution to the one-gallon
labeled container with 50ml volumetric dispenser attached.
7.5.6 Purity Check: Analyze according to section 11.2. NOTE: You
must ``precipitate'' the sample with an equal part of acetone (thus
duplicating actual test conditions--see section 11.1 of this method,
sample prep) before analyzing. Analyze the reagent 3 times to quantify
the C6 and termonomer interferences. Inspect the results to
ensure good agreement among the three runs (within 10%).
7.5.7 Tag the bottle with the following information:
POLYMER DISSOLVING SOLUTION FOR C6 IN CRUMB ANALYSIS
PREPARER'S NAME
DATE
CALS FILE ID'S OF THE THREE ANALYSES FOR PURITY (from section 7.5.6
of this method)
7.6 Quality Control Solution: the quality control solution is
prepared by adding specific amounts of mixed hexanes (barge hexane), n-
nonane and termonomer to some polymer dissolving solution. Nonane elutes
in the same approximate time region as termonomer and is used to
quantify in that region because it has a longer shelf life. Termonomer,
having a high tendency to polymerize, is used in the QC solution only to
ensure that both termonomer isomers elute at the proper time.
First, a concentrated stock solution is prepared; the final QC
solution can then be prepared by diluting the stock solution.
7.6.1 In preparation of stock solution, fill a 1-liter volumetric
flask partially with polymer dissolving solution (PDS)--see section 7.5
of this method. Add 20.0 ml barge hexane, 5.0 ml n-nonane, and 3 ml
termonomer. Finish filling the volumetric to the mark with PDS.
7.6.2 In preparation of quality control solution, dilute the quality
control stock solution (above) precisely 1:10 with PDS, i.e. 10 ml of
stock solution made up to 100 ml (volumetric flask) with PDS. Pour the
solution into a 4 oz. Boston round bottle and store in the refrigerator.
8.0 Sample Collection, Preservation and Storage
8.1 Line up facility to catch crumb samples. The facility is a
special facility where the sample is drawn.
8.1.1 Ensure that the cock valve beneath facility is closed.
8.1.2 Line up the system from the slurry line cock valve to the cock
valve at the nozzle on the stripper.
8.1.3 Allow the system to flush through facility for a period of 30
seconds.
8.2 Catch a slurry crumb sample.
8.2.1 Simultaneously close the cock valves upstream and downstream
of facility.
8.2.2 Close the cock valve beneath the slurry line in service.
8.2.3 Line up the cooling tower water through the sample bomb water
jacket to the sewer for a minimum of 30 minutes.
8.2.4 Place the sample catching basket beneath facility and open the
cock valve underneath the bomb to retrieve the rubber crumb.
8.2.5 If no rubber falls by gravity into the basket, line up
nitrogen to the bleeder upstream of the sample bomb and force the rubber
into the basket.
8.2.6 Close the cock valve underneath the sample bomb.
8.3 Fill a plastic ``Whirl-pak'' sample bag with slurry crumb and
send it to the lab immediately.
8.4 Once the sample reaches the lab, it should be prepped as soon as
possible to avoid hexane loss through evaporation. Samples which have
lain untouched for more than 30 minutes should be discarded.
9.0 Quality Control
Quality control is monitored via a computer program that tracks
analyses of a prepared QC sample (from section 7.6.2 of this method).
The QC sample result is entered daily into the program, which plots the
result as a data point on a statistical chart. If the data point does
not satisfy the ``in-control'' criteria (as defined by the lab quality
facilitator), an ``out-of-control'' flag appears, mandating corrective
action.
In addition, the area of the n-heptane peak is monitored so that any
errors in making up the polymer dissolving solution will be caught and
corrected. Refer to section 12.4 of this method.
9.1 Fill an autosampler vial with the quality control solution (from
section 7.6.2 of this method) and analyze on the GC as normal (per
section 11 of this method).
9.2 Add the concentrations of the 5 hexane isomers as they appear on
the CALS printout. Also include the 2,2-dimethyl-pentane peak just ahead
of the methyl cyclopentane (the fourth major isomer) peak in the event
that the peak integration split this peak out. Do not include the
benzene peak in the sum.
[[Page 235]]
Note the nonane concentration. Record both results (total hexane and
nonane) in the QC computer program. If out of control, and GC appears to
be functioning within normal parameters, reanalyze a fresh control
sample. If the fresh QC is not in control, check stock solution for
contaminants or make up a new QC sample with the toluene currently in
use. If instrument remains out-of-control, more thorough GC
troubleshooting may be needed.
Also, verify that the instrument has detected both isomers of
termonomer (quantification not necessary--see section 7.0 of this
method).
9.3 Recovery efficiency must be determined for high ethylene
concentration, low ethylene concentration, E-P terpolymer, or oil
extended samples and whenever modifications are made to the method.
Recovery shall be between 70 and 130 percent. All test results must be
corrected by the recovery efficiency value (R).
9.3.1 Approximately 10 grams of wet EPDM crumb (equivalent to about
5 grams of dry rubber) shall be added to six sample bottles containing
100 ml of hexane in crumb polymer dissolving solution (toluene
containing 0.3 gram n-heptane/100 ml solution). The polymer shall be
dissolved by agitating the bottles on a shaker for 4 hours. The polymer
shall be precipitated using 100 ml acetone.
9.3.2 The supernatant liquid shall be decanted from the polymer.
Care shall be taken to remove as much of the liquid phase from the
sample as possible to minimize the effect of retained liquid phase upon
the next cycle of the analysis. The supernatant liquid shall be analyzed
by gas chromatography using an internal standard quantitation method
with heptane as the internal standard.
9.3.3 The precipitated polymer from the steps described above shall
be redissolved using toluene as the solvent. No heptane shall be added
to the sample in the second dissolving step. The toluene solvent and
acetone precipitant shall be determined to be free of interfering
compounds.
9.3.4 The rubber which was dissolved in the toluene shall be
precipitated with acetone as before, and the supernatant liquid decanted
from the precipitated polymer. The liquid shall be analyzed by gas
chromatography and the rubber phase dried in a steam-oven to determine
the final polymer weight.
9.3.5 The ratios of the areas of the hexane peaks and of the heptane
internal standard peak shall be calculated for each of the six samples
in the two analysis cycles outlined above. The area ratios of the total
hexane to heptane (R1) shall be determined for the two analysis cycles
of the sample set. The ratio of the values of R1 from the second
analysis cycle to the first cycle shall be determined to give a second
ratio (R2).
10.0 Calibration and Standardization
The procedure for preparing a Quality Control sample with the
internal standard in it is outlined in section 7.6 of this method.
10.1 The relative FID response factors for n-heptane, the internal
standard, versus the various hexane isomers and termonomer are
relatively constant and should seldom need to be altered. However
Baseline construction is a most critical factor in the production of
good data. For this reason, close attention should be paid to peak
integration. Procedures for handling peak integration will depend upon
the data system used.
10.2 If recalibration of the analysis is needed, make up a
calibration blend of the internal standard and the analytes as detailed
below and analyze it using the analytical method used for the samples.
10.2.1 Weigh 5 g heptane into a tared scintillation vial to five
places.
10.2.2 Add 0.2 ml termonomer to the vial and reweigh.
10.2.3 Add 0.5 ml hexane to the vial and reweigh.
10.2.4 Cap, and shake vigorously to mix.
10.2.5 Calculate the weights of termonomer and of hexane added and
divide their weights by the weight of the n-heptane added. The result is
the known of given value for the calibration.
10.2.6 Add 0.4 ml of this mixture to a mixture of 100 ml toluene and
100 ml of acetone. Cap and shake vigorously to mix.
10.2.7 Analyze the sample.
10.2.8 Divide the termonomer area and the total areas of the hexane
peaks by the n-heptane area. This result is the ``found'' value for the
calibration.
10.2.9 Divide the appropriate ``known'' value from 10.2.5 by the
found value from 10.2.8. The result is the response factor for the
analyte in question. Previous work has shown that the standard deviation
of the calibration method is about 1% relative.
11.0 Procedure
11.1 SAMPLE PREPARATION
11.1.1 Tare an 8oz sample bottle--Tag attached, cap off; record
weight and sample ID on tag in pencil.
11.1.2 Place crumb sample in bottle: RLA-3: 10 g (gives a dry wt. of
5.5 g).
11.1.3 Dispense 100ml of PDS into each bottle. SAMPLE SHOULD BE
PLACED INTO SOLUTION ASAP TO AVOID HEXANE LOSS--Using ``Dispensette''
pipettor. Before dispensing, ``purge'' the dispensette (25% of its
volume) into a waste bottle to eliminate any voids.
11.1.4 Tightly cap bottles and load samples into shaker.
11.1.5 Insure that ``ON-OFF'' switch on the shaker itself is ``ON.''
11.1.6 Locate shaker timer. Insure that toggle switch atop timer
control box is in
[[Page 236]]
the middle (``off'') position. If display reads ``04:00'' (4 hours),
move toggle switch to the left position. Shaker should begin operating.
11.1.7 After shaker stops, add 100 ml acetone to each sample to
precipitate polymer. Shake minimum of 5 minutes on shaker--Vistalon
sample may not have fully dissolved; nevertheless, for purposes of
consistency, 4 hours is the agreed-upon dissolving time.
11.1.8 Using a 5-ml glass Luer-lock syringe and Acrodisc filter,
filter some of the supernatant liquid into an autosampler vial; crimp
the vial and load it into the GC autosampler for analysis (section 11.2
of this method)--The samples are filtered to prevent polymer buildup in
the GC. Clean the syringes in toluene.
11.1.9 Decant remaining supernatant into a hydrocarbon waste sink,
being careful not to discard any of the polymer. Place bottle of
precipitate into the steam oven and dry for six hours--Some grades of
Vistalon produce very small particles in the precipitate, thus making
complete decanting impossible without discarding some polymer. In this
case, decant as much as possible and put into the oven as is, allowing
the oven to drive off remaining supernatant (this practice is avoided
for environmental reasons). WARNING: OVEN IS HOT--110 [deg]C (230
[deg]F).
11.1.10 Cool, weigh and record final weight of bottle.
11.2 GC ANALYSIS
11.2.1 Initiate the CALS computer channel.
11.2.2 Enter the correct instrument method into the GC's integrator.
11.2.3 Load sample vial(s) into autosampler.
11.2.4 Start the integrator.
11.2.5 When analysis is complete, plot CALS run to check baseline
skim.
12.0 Data Analysis and Calculations
12.1 Add the concentrations of the hexane peaks as they appear on
the CALS printout. Do not include the benzene peak in the sum.
12.2 Subtract any hexane interferences found in the PDS (see section
7.5.6 of this method); record the result.
12.3 Note the termonomer concentration on the CALS printout.
Subtract any termonomer interference found in the PDS and record this
result in a ``% termonomer by GC'' column in a logbook.
12.4 Record the area (from CALS printout) of the heptane internal
standard peak in a ``C7 area'' column in the logbook. This helps track
instrument performance over the long term.
12.5 After obtaining the final dry weight of polymer used (Section
11.1.10 of this method), record that result in a ``dry wt.'' column of
the logbook (for oil extended polymer, the amount of oil extracted is
added to the dry rubber weight).
12.6 Divide the %C6 by the dry weight to obtain the total PHR hexane
in crumb. Similarly, divide the % termonomer by the dry weight to obtain
the total PHR termonomer in crumb. Note that PHR is an abbreviation for
``parts per hundred''. Record both the hexane and termonomer results in
the logbook.
12.7 Correct all results by the recovery efficiency value (R).
13.0 Method Performance
13.1 The method has been shown to provide 100% recovery of the
hexane analyte. The method was found to give a 6% relative standard
deviation when the same six portions of the same sample were carried
through the procedure. Note: These values are examples; each sample
type, as specified in Section 9.3, must be tested for sample recovery.
14.0 Pollution Prevention
14.1 Dispose of all hydrocarbon liquids in the appropriate disposal
sink system; never pour hydrocarbons down a water sink.
14.2 As discussed in section 11.1.9 of this method, the analyst can
minimize venting hydrocarbon vapor to the atmosphere by decanting as
much hydrocarbon liquid as possible before oven drying.
15.0 Waste Management
15.1 The Technician conducting the analysis should follow the proper
waste management practices for their laboratory location.
16.0 References
16.1 Baton Rouge Chemical Plant Analytical Procedure no. BRCP 1302
16.2 Material Safety Data Sheets (from chemical vendors) for hexane,
ENB, toluene, acetone, and heptane
Method 310C--Determination of Residual N-Hexane in EPDM Rubber Through
Gas Chromatography
1.0 Scope and Application
1.1 This method describes a procedure for the determination of
residual hexane in EPDM wet crumb rubber in the 0.01--2% range by
solvent extraction of the hexane followed by gas chromatographic
analysis where the hexane is detected by flame ionization and quantified
via an internal standard.
1.2 This method may involve hazardous materials operations and
equipment. This method does not purport to address all the safety
problems associated with it use, if any. It is the responsibility of the
user to consult and establish appropriate safety and health practices
and determine the applicability of regulatory limitations prior to use.
[[Page 237]]
2.0 Summary
2.1 Residual hexane contained in wet pieces of EPDM polymer is
extracted with MIBK. A known amount of an internal standard (IS) is
added to the extract which is subsequently analyzed via gas
chromatography where the hexane and IS are separated and detected
utilizing a megabore column and flame ionization detection (FID). From
the response to the hexane and the IS, the amount of hexane in the EPDM
polymer is calculated.
3.0 Definitions
3.1 Hexane--refers to n-hexane
3.2 Heptane--refers to n-heptane
3.3 MIBK--methyl isobutyl ketone (4 methyl 2--Pentanone)
4.0 Interferences
4.1 Material eluting at or near the hexane and/or the IS will cause
erroneous results. Prior to extraction, solvent blanks must be analyzed
to confirm the absence of interfering peaks.
5.0 Safety
5.1 Review Material Safety Data Sheets of the chemicals used in this
method.
6.0 Equipment and Supplies
6.1 4 oz round glass jar with a wide mouth screw cap lid.
6.2 Vacuum oven.
6.3 50 ml pipettes.
6.4 A gas chromatograph with an auto sampler and a 50 meter, 0.53
ID, methyl silicone column with 5 micron phase thickness.
6.5 Shaker, large enough to hold 10, 4 oz. jars.
6.6 1000 and 4000 ml volumetric flasks.
6.7 Electronic integrator or equivalent data system.
6.8 GC autosampler vials.
6.9 50 uL syringe.
7.0 Reagents and Standards
7.1 Reagent grade Methyl-Iso-Butyl-Ketone (MIBK)
7.2 n-heptane, 99% + purity
7.3 n-hexane, 99% + purity
8.0 Sample Collection
8.1 Trap a sample of the EPDM crumb slurry in the sampling
apparatus. Allow the crumb slurry to circulate through the sampling
apparatus for 5 minutes; then close off the values at the bottom and top
of the sampling apparatus, trapping the crumb slurry. Run cooling water
through the water jacket for a minimum of 30 minutes. Expel the cooled
crumb slurry into a sample catching basket. If the crumb does not fall
by gravity, force it out with demineralized water or nitrogen. Send the
crumb slurry to the lab for analysis.
9.0 Quality Control
9.1 The Royalene crumb sample is extracted three times with MIBK
containing an internal standard. The hexane from each extraction is
added together to obtain a total hexane content. The percent hexane in
the first extraction is then calculated and used as the recovery factor
for the analysis.
9.2 Follow this test method through section 11.4 of the method.
After removing the sample of the first extraction to be run on the gas
chromatograph, drain off the remainder of the extraction solvent,
retaining the crumb sample in the sample jar. Rinse the crumb with
demineralized water to remove any MIBK left on the surface of the crumb.
Repeat the extraction procedure with fresh MIBK with internal standard
two more times.
9.3 After the third extraction, proceed to section 11.5 of this
method and obtain the percent hexane in each extraction. Use the sample
weight obtained in section 12.1 of this method to calculate the percent
hexane in each of the extracts.
9.4 Add the percent hexane obtained from the three extractions for a
total percent hexane in the sample.
9.5 Use the following equations to determine the recovery factor
(R):
% Recovery of the first extraction=(% hexane in the first extract/
total % hexane)x100
Recovery Factor (R)=(% Hexane Recovered in the first extract)/100
10.0 Calibration
10.1 Preparation of Internal Standard (IS) solution:
Accuracy weigh 30 grams of n-heptane into a 1000 ml volumetric
flask. Dilute to the mark with reagent grade MIBK. Label this Solution
``A''. Pipette 100 mls. of Solution A into a 4 liter volumetric flask.
Fill the flask to the mark with reagent MIBK. Label this Solution ``B''.
Solution ``B'' will have a concentration of 0.75 mg/ml of heptane.
10.2 Preparation of Hexane Standard Solution (HS):
Using a 50 uL syringe, weigh by difference, 20 mg of n-hexane into a
50 ml volumetric flask containing approximately 40 ml of Solution B.
Fill the flask to the mark with Solution B and mix well.
10.3 Conditions for GC analysis of standards and samples:
Temperature:
Initial=40 [deg]C
Final=150 [deg]C
Injector=160 [deg]C
Detector=280 [deg]C
Program Rate=5.0 [deg]C/min
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Initial Time=5 minutes Final Time=6 minutes
Flow Rate=5.0 ml/min
Sensitivity=detector response must be adjusted to keep the hexane
and IS on scale.
10.4 Fill an autosampler vial with the HS, analyze it three times
and calculate a Hexane Relative Response Factor (RF) as follows:
RF=(AIS x CHS x PHS)/(AHS x
CIS x PIS) (1)
Where:
AIS=Area of IS peak (Heptane)
AHS=Area of peak (Hexane Standard)
CHS=Mg of Hexane/50 ml HS
CIS=Mg of Heptane/50 ml IS Solution B
PIS=Purity of the IS n-heptane
PHS=Purity of the HS n-hexane
11.0 Procedure
11.1 Weight 10 grams of wet crumb into a tared (W1), wide mouth 4
oz. jar.
11.2 Pipette 50 ml of Solution B into the jar with the wet crumb
rubber.
11.3 Screw the cap on tightly and place it on a shaker for 4 hours.
11.4 Remove the sample from the shaker and fill an autosampler vial
with the MIBK extract.
11.5 Analyze the sample two times.
11.6 Analyze the HS twice, followed by the samples. Inject the HS
twice at the end of each 10 samples or at the end of the run.
12.0 Calculations
12.1 Drain off the remainder of the MIBK extract from the polymer in
the 4 oz. jar. Retain all the polymer in the jar. Place the uncovered
jar and polymer in a heated vacuum oven until the polymer is dry.
Reweigh the jar and polymer (W2) and calculate the dried sample weight
of the polymer as follows:
Dried SW=W2--W1 (2)
12.2 Should the polymer be oil extended, pipette 10 ml of the MIBK
extract into a tared evaporating dish (W1) and evaporate to dryness on a
steam plate.
Reweigh the evaporating dish containing the extracted oil (W2).
Calculate the oil content of the polymer as follows:
Gram of oil extracted =5 (W2--W1) (3)
% Hexane in polymer=(AsxRFxCISxPIS)/
(AISxSW) (4)
Where:
As=Area of sample hexane sample peak.
AIS=Area of IS peak in sample.
CIS=Concentration of IS in 50 ml.
PIS=Purity of IS.
SW=Weight of dried rubber after extraction. (For oil extended polymer,
the amount of oil extracted is added to the dry rubber weight).
% Corrected Hexane=(% Hexane in Polymer)/R (5)
R=Recovery factor determined in section 9 of this method.
13.0 Method Performance
13.1 Performance must be determined for each sample type by
following the procedures in section 9 of this method.
14.0 Waste Generation
14.1 Waste generation should be minimized where possible.
15.0 Waste Management
15.1 All waste shall be handled in accordance with Federal and State
environmental regulations.
16.0 References [Reserved]
Method 311--Analysis of Hazardous Air Pollutant Compounds in Paints and
Coatings by Direct Injection Into a Gas Chromatograph
1. Scope and Application
1.1 Applicability. This method is applicable for determination of
most compounds designated by the U.S. Environmental Protection Agency as
volatile hazardous air pollutants (HAP's) (See Reference 1) that are
contained in paints and coatings. Styrene, ethyl acrylate, and methyl
methacrylate can be measured by ASTM D 4827-93 or ASTM D 4747-87.
Formaldehyde can be measured by ASTM PS 9-94 or ASTM D 1979-91. Toluene
diisocyanate can be measured in urethane prepolymers by ASTM D 3432-89.
Method 311 applies only to those volatile HAP's which are added to the
coating when it is manufactured, not to those which may form as the
coating cures (reaction products or cure volatiles). A separate or
modified test procedure must be used to measure these reaction products
or cure volatiles in order to determine the total volatile HAP emissions
from a coating. Cure volatiles are a significant component of the total
HAP content of some coatings. The term ``coating'' used in this method
shall be understood to mean paints and coatings.
1.2 Principle. The method uses the principle of gas chromatographic
separation and quantification using a detector that responds to
concentration differences. Because there are many potential analytical
systems or sets of operating conditions that may represent useable
methods for determining the concentrations of the compounds cited in
Section 1.1 in the applicable matrices, all systems that employ this
principle, but differ only in details of equipment and operation, may be
used as alternative methods, provided that the prescribed quality
control, calibration, and method performance requirements are met.
Certified product data sheets (CPDS) may also include information
relevant to the analysis of the coating sample including, but not
limited to, separation
[[Page 239]]
column, oven temperature, carrier gas, injection port temperature,
extraction solvent, and internal standard.
2. Summary of Method
Whole coating is added to dimethylformamide and a suitable internal
standard compound is added. An aliquot of the sample mixture is injected
onto a chromatographic column containing a stationary phase that
separates the analytes from each other and from other volatile compounds
contained in the sample. The concentrations of the analytes are
determined by comparing the detector responses for the sample to the
responses obtained using known concentrations of the analytes.
3. Definitions [Reserved]
4. Interferences
4.1 Coating samples of unknown composition may contain the compound
used as the internal standard. Whether or not this is the case may be
determined by following the procedures of Section 11 and deleting the
addition of the internal standard specified in Section 11.5.3. If
necessary, a different internal standard may be used.
4.2 The GC column and operating conditions developed for one coating
formulation may not ensure adequate resolution of target analytes for
other coating formulations. Some formulations may contain nontarget
analytes that coelute with target analytes. If there is any doubt about
the identification or resolution of any gas chromatograph (GC) peak, it
may be necessary to analyze the sample using a different GC column or
different GC operating conditions.
4.3 Cross-contamination may occur whenever high-level and low-level
samples are analyzed sequentially. The order of sample analyses
specified in Section 11.7 is designed to minimize this problem.
4.4 Cross-contamination may also occur if the devices used to
transfer coating during the sample preparation process or for injecting
the sample into the GC are not adequately cleaned between uses. All such
devices should be cleaned with acetone or other suitable solvent and
checked for plugs or cracks before and after each use.
5. Safety
5.1 Many solvents used in coatings are hazardous. Precautions should
be taken to avoid unnecessary inhalation and skin or eye contact. This
method may involve hazardous materials, operations, and equipment. This
test method does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this
test method to establish appropriate safety and health practices and to
determine the applicability of regulatory limitations in regards to the
performance of this test method.
5.2 Dimethylformamide is harmful if inhaled or absorbed through the
skin. The user should obtain relevant health and safety information from
the manufacturer. Dimethylformamide should be used only with adequate
ventilation. Avoid contact with skin, eyes, and clothing. In case of
contact, immediately flush skin or eyes with plenty of water for at
least 15 minutes. If eyes are affected, consult a physician. Remove and
wash contaminated clothing before reuse.
5.3 User's manuals for the gas chromatograph and other related
equipment should be consulted for specific precautions to be taken
related to their use.
6. Equipment and Supplies
Note: Certified product data sheets (CPDS) may also include
information relevant to the analysis of the coating sample including,
but not limited to, separation column, oven temperature, carrier gas,
injection port temperature, extraction solvent, and internal standard.
6.1 Sample Collection.
6.1.1 Sampling Containers. Dual-seal sampling containers, four to
eight fluid ounce capacity, should be used to collect the samples. Glass
sample bottles or plastic containers with volatile organic compound
(VOC) impermeable walls must be used for corrosive substances (e.g.,
etch primers and certain coating catalysts such as methyl ethyl ketone
(MEK) peroxide). Sample containers, caps, and inner seal liners must be
inert to the compounds in the sample and must be selected on a case-by-
case basis.
6.1.1.1 Other routine sampling supplies needed include waterproof
marking pens, tubing, scrappers/spatulas, clean rags, paper towels,
cooler/ice, long handle tongs, and mixing/stirring paddles.
6.1.2 Personal safety equipment needed includes eye protection,
respiratory protection, a hard hat, gloves, steel toe shoes, etc.
6.1.3 Shipping supplies needed include shipping boxes, packing
material, shipping labels, strapping tape, etc.
6.1.4 Data recording forms and labels needed include coating data
sheets and sample can labels.
Note: The actual requirements will depend upon the conditions
existing at the source sampled.
6.2 Laboratory Equipment and Supplies.
6.2.1 Gas Chromatograph (GC). Any instrument equipped with a flame
ionization detector and capable of being temperature programmed may be
used. Optionally, other types of detectors (e.g., a mass spectrometer),
and any necessary interfaces, may be used provided that the detector
system
[[Page 240]]
yields an appropriate and reproducible response to the analytes in the
injected sample. Autosampler injection may be used, if available.
6.2.2 Recorder. If available, an electronic data station or
integrator may be used to record the gas chromatogram and associated
data. If a strip chart recorder is used, it must meet the following
criteria: A 1 to 10 millivolt (mV) linear response with a full scale
response time of 2 seconds or less and a maximum noise level of 0.03 percent of full scale. Other types of recorders may
be used as appropriate to the specific detector installed provided that
the recorder has a full scale response time of 2 seconds or less and a
maximum noise level of 0.03 percent of full scale.
6.2.3 Column. The column must be constructed of materials that do
not react with components of the sample (e.g., fused silica, stainless
steel, glass). The column should be of appropriate physical dimensions
(e.g., length, internal diameter) and contain sufficient suitable
stationary phase to allow separation of the analytes. DB-5, DB-Wax, and
FFAP columns are commonly used for paint analysis; however, it is the
responsibility of each analyst to select appropriate columns and
stationary phases.
6.2.4 Tube and Tube Fittings. Supplies to connect the GC and gas
cylinders.
6.2.5 Pressure Regulators. Devices used to regulate the pressure
between gas cylinders and the GC.
6.2.6 Flow Meter. A device used to determine the carrier gas flow
rate through the GC. Either a digital flow meter or a soap film bubble
meter may be used to measure gas flow rates.
6.2.7 Septa. Seals on the GC injection port through which liquid or
gas samples can be injected using a syringe.
6.2.8 Liquid Charging Devices. Devices used to inject samples into
the GC such as clean and graduated 1, 5, and 10 microliter ([micro]l)
capacity syringes.
6.2.9 Vials. Containers that can be sealed with a septum in which
samples may be prepared or stored. The recommended size is 25 ml
capacity. Mininert[reg] valves have been found satisfactory
and are available from Pierce Chemical Company, Rockford, Illinois.
6.2.10 Balance. Device used to determine the weights of standards
and samples. An analytical balance capable of accurately weighing to
0.0001 g is required.
7. Reagents and Standards
7.1 Purity of Reagents. Reagent grade chemicals shall be used in all
tests. Unless otherwise specified, all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the American
Chemical Society, where such specifications are available. Other grades
may be used provided it is first ascertained that the reagent is of
sufficient purity to permit its use without lessening the accuracy of
determination.
7.2 Carrier Gas. Helium carrier gas shall have a purity of 99.995
percent or higher. High purity nitrogen may also be used. Other carrier
gases that are appropriate for the column system and analyte may also be
used. Ultra-high purity grade hydrogen gas and zero-grade air shall be
used for the flame ionization detector.
7.3 Dimethylformamide (DMF). Solvent for all standards and samples.
Some other suitable solvent may be used if DMF is not compatible with
the sample or coelutes with a target analyte.
Note: DMF may coelute with ethylbenzene or p-xylene under the
conditions described in the note under Section 6.2.3.
7.4 Internal Standard Materials. The internal standard material is
used in the quantitation of the analytes for this method. It shall be
gas chromatography spectrophotometric quality or, if this grade is not
available, the highest quality available. Obtain the assay for the
internal standard material and maintain at that purity during use. The
recommended internal standard material is 1-propanol; however, selection
of an appropriate internal standard material for the particular coating
and GC conditions used is the responsibility of each analyst.
7.5 Reference Standard Materials. The reference standard materials
are the chemicals cited in Section 1.1 which are of known identity and
purity and which are used to assist in the identification and
quantification of the analytes of this method. They shall be the highest
quality available. Obtain the assays for the reference standard
materials and maintain at those purities during use.
7.6 Stock Reference Standards. Stock reference standards are
dilutions of the reference standard materials that may be used on a
daily basis to prepare calibration standards, calibration check
standards, and quality control check standards. Stock reference
standards may be prepared from the reference standard materials or
purchased as certified solutions.
7.6.1 Stock reference standards should be prepared in
dimethylformamide for each analyte expected in the coating samples to be
analyzed. The concentrations of analytes in the stock reference
standards are not specified but must be adequate to prepare the
calibration standards required in the method. A stock reference standard
may contain more than one analyte provided all analytes are chemically
compatible and no analytes coelute. The actual concentrations prepared
must be known to within 0.1 percent (e.g., 0.1000 0.0001 g/g solution). The following procedure is
suggested. Place about 35 ml of dimethylformamide into a tared
[[Page 241]]
ground-glass stoppered 50 ml volumetric flask. Weigh the flask to the
nearest 0.1 mg. Add 12.5 g of the reference standard material and
reweigh the flask. Dilute to volume with dimethylformamide and reweigh.
Stopper the flask and mix the contents by inverting the flask several
times. Calculate the concentration in grams per gram of solution from
the net gain in weights, correcting for the assayed purity of the
reference standard material.
Note: Although a glass-stoppered volumetric flask is convenient, any
suitable glass container may be used because stock reference standards
are prepared by weight.
7.6.2 Transfer the stock reference standard solution into one or
more Teflon-sealed screw-cap bottles. Store, with minimal headspace, at
-10 [deg]C to 0 [deg]C and protect from light.
7.6.3 Prepare fresh stock reference standards every six months, or
sooner if analysis results from daily calibration check standards
indicate a problem. Fresh stock reference standards for very volatile
HAP's may have to be prepared more frequently.
7.7 Calibration Standards. Calibration standards are used to
determine the response of the detector to known amounts of reference
material. Calibration standards must be prepared at a minimum of three
concentration levels from the stock reference standards (see Section
7.6). Prepare the calibration standards in dimethylformamide (see
Section 7.3). The lowest concentration standard should contain a
concentration of analyte equivalent either to a concentration of no more
than 0.01% of the analyte in a coating or to a concentration that is
lower than the actual concentration of the analyte in the coating,
whichever concentration is higher. The highest concentration standard
should contain a concentration of analyte equivalent to slightly more
than the highest concentration expected for the analyte in a coating.
The remaining calibration standard should contain a concentration of
analyte roughly at the midpoint of the range defined by the lowest and
highest concentration calibration standards. The concentration range of
the standards should thus correspond to the expected range of analyte
concentrations in the prepared coating samples (see Section 11.5). Each
calibration standard should contain each analyte for detection by this
method expected in the actual coating samples (e.g., some or all of the
compounds listed in Section 1.1 may be included). Each calibration
standard should also contain an appropriate amount of internal standard
material (response for the internal standard material is within 25 to 75
percent of full scale on the attenuation setting for the particular
reference standard concentration level). Calibration Standards should be
stored for 1 week only in sealed vials with minimal headspace. If the
stock reference standards were prepared as specified in Section 7.6, the
calibration standards may be prepared by either weighing each addition
of the stock reference standard or by adding known volumes of the stock
reference standard and calculating the mass of the standard reference
material added. Alternative 1 (Section 7.7.1) specifies the procedure to
be followed when the stock reference standard is added by volume.
Alternative 2 (Section 7.7.2) specifies the procedure to be followed
when the stock reference standard is added by weight.
Note: To assist with determining the appropriate amount of internal
standard to add, as required here and in other sections of this method,
the analyst may find it advantageous to prepare a curve showing the area
response versus the amount of internal standard injected into the GC.
7.7.1 Preparation Alternative 1. Determine the amount of each stock
reference standard and dimethylformamide solvent needed to prepare
approximately 25 ml of the specific calibration concentration level
desired. To a tared 25 ml vial that can be sealed with a crimp-on or
Mininert[reg] valve, add the total amount of
dimethylformamide calculated to be needed. As quickly as practical, add
the calculated amount of each stock reference standard using new pipets
(or pipet tips) for each stock reference standard. Reweigh the vial and
seal it. Using the known weights of the standard reference materials per
ml in the stock reference standards, the volumes added, and the total
weight of all reagents added to the vial, calculate the weight percent
of each standard reference material in the calibration standard
prepared. Repeat this process for each calibration standard to be
prepared.
7.7.2 Preparation Alternative 2. Determine the amount of each stock
reference standard and dimethylformamide solvent needed to prepare
approximately 25 ml of the specific calibration concentration level
desired. To a tared 25 ml vial that can be sealed with a crimp-on or
Mininert[reg] valve, add the total amount of
dimethylformamide calculated to be needed. As quickly as practical, add
the calculated amount of a stock reference standard using a new pipet
(or pipet tip) and reweigh the vial. Repeat this process for each stock
reference standard to be added. Seal the vial after obtaining the final
weight. Using the known weight percents of the standard reference
materials in the stock reference standards, the weights of the stock
reference standards added, and the total weight of all reagents added to
the vial, calculate the weight percent of each standard reference
material in the calibration standard prepared. Repeat this process for
each calibration standard to be prepared.
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8. Sample Collection, Preservation, Transport, and Storage
8.1 Copies of material safety data sheets (MSDS's) for each sample
should be obtained prior to sampling. The MSDS's contain information on
the ingredients, and physical and chemical properties data. The MSDS's
also contain recommendations for proper handling or required safety
precautions. Certified product data sheets (CPDS) may also include
information relevant to the analysis of the coating sample including,
but not limited to, separation column, oven temperature, carrier gas,
injection port temperature, extraction solvent, and internal standard.
8.2 A copy of the blender's worksheet can be requested to obtain
data on the exact coating being sampled. A blank coating data sheet form
(see Section 18) may also be used. The manufacturer's formulation
information from the product data sheet should also be obtained.
8.3 Prior to sample collection, thoroughly mix the coating to ensure
that a representative, homogeneous sample is obtained. It is preferred
that this be accomplished using a coating can shaker or similar device;
however, when necessary, this may be accomplished using mechanical
agitation or circulation systems.
8.3.1 Water-thinned coatings tend to incorporate or entrain air
bubbles if stirred too vigorously; mix these types of coatings slowly
and only as long as necessary to homogenize.
8.3.2 Each component of multicomponent coatings that harden when
mixed must be sampled separately. The component mix ratios must be
obtained at the facility at the time of sampling and submitted to the
analytical laboratory.
8.4 Sample Collection. Samples must be collected in a manner that
prevents or minimizes loss of volatile components and that does not
contaminate the coating reservoir. A suggested procedure is as follows.
Select a sample collection container which has a capacity at least 25
percent greater than the container in which the sample is to be
transported. Make sure both sample containers are clean and dry. Using
clean, long-handled tongs, turn the sample collection container upside
down and lower it into the coating reservoir. The mouth of the sample
collection container should be at approximately the midpoint of the
reservoir (do not take the sample from the top surface). Turn the sample
collection container over and slowly bring it to the top of the coating
reservoir. Rapidly pour the collected coating into the sample container,
filling it completely. It is important to fill the sample container
completely to avoid any loss of volatiles due to volatilization into the
headspace. Return any unused coating to the reservoir or dispose as
appropriate.
Note: If a company requests a set of samples for its own analysis, a
separate set of samples, using new sample containers, should be taken at
the same time.
8.5 Once the sample is collected, place the sample container on a
firm surface and insert the inner seal in the container by placing the
seal inside the rim of the container, inverting a screw cap, and
pressing down on the screw cap which will evenly force the inner seal
into the container for a tight fit. Using clean towels or rags, remove
all residual coating material from the outside of the sample container
after inserting the inner seal. Screw the cap onto the container.
8.5.1 Affix a sample label (see Section 18) clearly identifying the
sample, date collected, and person collecting the sample.
8.5.2 Prepare the sample for transportation to the laboratory. The
sample should be maintained at the coating's recommended storage
temperature specified on the Material Safety Data Sheet, or, if no
temperature is specified, the sample should be maintained within the
range of 5 [deg]C to 38 [deg]C.
8.9 The shipping container should adhere to U.S. Department of
Transportation specification DOT 12-B. Coating samples are considered
hazardous materials; appropriate shipping procedures should be followed.
9. Quality Control
9.1 Laboratories using this method should operate a formal quality
control program. The minimum requirements of the program should consist
of an initial demonstration of laboratory capability and an ongoing
analysis of blanks and quality control samples to evaluate and document
quality data. The laboratory must maintain records to document the
quality of the data generated. When results indicate atypical method
performance, a quality control check standard (see Section 9.4) must be
analyzed to confirm that the measurements were performed in an in-
control mode of operation.
9.2 Before processing any samples, the analyst must demonstrate,
through analysis of a reagent blank, that there are no interferences
from the analytical system, glassware, and reagents that would bias the
sample analysis results. Each time a set of analytical samples is
processed or there is a change in reagents, a reagent blank should be
processed as a safeguard against chronic laboratory contamination. The
blank samples should be carried through all stages of the sample
preparation and measurement steps.
9.3 Required instrument quality control parameters are found in the
following sections:
9.3.1 Baseline stability must be demonstrated to be <=5 percent of
full scale using the procedures given in Section 10.1.
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9.3.2 The GC calibration is not valid unless the retention time (RT)
for each analyte at each concentration is within 0.05 min of the retention time measured for that analyte
in the stock standard.
9.3.3 The retention time (RT) of any sample analyte must be within
0.05 min of the average RT of the analyte in the
calibration standards for the analyte to be considered tentatively
identified.
9.3.4 The GC system must be calibrated as specified in Section 10.2.
9.3.5 A one-point daily calibration check must be performed as
specified in Section 10.3.
9.4 To establish the ability to generate results having acceptable
accuracy and precision, the analyst must perform the following
operations.
9.4.1 Prepare a quality control check standard (QCCS) containing
each analyte expected in the coating samples at a concentration expected
to result in a response between 25 percent and 75 percent of the limits
of the calibration curve when the sample is prepared as described in
Section 11.5. The QCCS may be prepared from reference standard materials
or purchased as certified solutions. If prepared in the laboratory, the
QCCS must be prepared independently from the calibration standards.
9.4.2 Analyze three aliquots of the QCCS according to the method
beginning in Section 11.5.3 and calculate the weight percent of each
analyte using Equation 1, Section 12.
9.4.3 Calculate the mean weight percent (X) for each analyte from
the three results obtained in Section 9.4.2.
9.4.4 Calculate the percent accuracy for each analyte using the
known concentrations (Ti) in the QCCS using Equation 3, Section 12.
9.4.5 Calculate the percent relative standard deviation (percent
RSD) for each analyte using Equation 7, Section 12, substituting the
appropriate values for the relative response factors (RRF's) in said
equation.
9.4.6 If the percent accuracy (Section 9.4.4) for all analytes is
within the range 90 percent to 110 percent and the percent RSD (Section
9.4.5) for all analytes is <=20 percent, system performance is
acceptable and sample analysis may begin. If these criteria are not met
for any analyte, then system performance is not acceptable for that
analyte and the test must be repeated for those analytes only. Repeated
failures indicate a general problem with the measurement system that
must be located and corrected. In this case, the entire test, beginning
at Section 9.4.1, must be repeated after the problem is corrected.
9.5 Great care must be exercised to maintain the integrity of all
standards. It is recommended that all standards be stored at -10 [deg]C
to 0 [deg]C in screw-cap amber glass bottles with Teflon liners.
9.6 Unless otherwise specified, all weights are to be recorded
within 0.1 mg.
10. Calibration and Standardization.
10.1 Column Baseline Drift. Before each calibration and series of
determinations and before the daily calibration check, condition the
column using procedures developed by the laboratory or as specified by
the column supplier. Operate the GC at initial (i.e., before sample
injection) conditions on the lowest attenuation to be used during sample
analysis. Adjust the recorder pen to zero on the chart and obtain a
baseline for at least one minute. Initiate the GC operating cycle that
would be used for sample analysis. On the recorder chart, mark the pen
position at the end of the simulated sample analysis cycle. Baseline
drift is defined as the absolute difference in the pen positions at the
beginning and end of the cycle in the direction perpendicular to the
chart movement. Calculate the percent baseline drift by dividing the
baseline drift by the chart width representing full-scale deflection and
multiply the result by 100.
10.2 Calibration of GC. Bring all stock standards and calibration
standards to room temperature while establishing the GC at the
determined operating conditions.
10.2.1 Retention Times (RT's) for Individual Compounds.
Note: The procedures of this subsection are required only for the
initial calibration. However, it is good laboratory practice to follow
these procedures for some or all analytes before each calibration. The
procedures were written for chromatograms output to a strip chart
recorder. More modern instruments (e.g., integrators and electronic data
stations) determine and print out or display retention times
automatically.
The RT for each analyte should be determined before calibration.
This provides a positive identification for each peak observed from the
calibration standards. Inject an appropriate volume (see Note in Section
11.5.2) of one of the stock reference standards into the gas
chromatograph and record on the chart the pen position at the time of
the injection (see Section 7.6.1). Dilute an aliquot of the stock
reference standard as required in dimethylformamide to achieve a
concentration that will result in an on-scale response. Operate the gas
chromatograph according to the determined procedures. Select the peak(s)
that correspond to the analyte(s) [and internal standard, if used] and
measure the retention time(s). If a chart recorder is used, measure the
distance(s) on the chart from the injection point to the peak maxima.
These distances, divided by the chart speed, are defined as the RT's of
the analytes in question. Repeat this process for each of the stock
reference standard solutions.
[[Page 244]]
Note: If gas chromatography with mass spectrometer detection (GC-MS)
is used, a stock reference standard may contain a group of analytes,
provided all analytes are adequately separated during the analysis. Mass
spectral library matching can be used to identify the analyte associated
with each peak in the gas chromatogram. The retention time for the
analyte then becomes the retention time of its peak in the chromatogram.
10.2.2 Calibration. The GC must be calibrated using a minimum of
three concentration levels of each potential analyte. (See Section 7.7
for instructions on preparation of the calibration standards.) Beginning
with the lowest concentration level calibration standard, carry out the
analysis procedure as described beginning in Section 11.7. Repeat the
procedure for each progressively higher concentration level until all
calibration standards have been analyzed.
10.2.2.1 Calculate the RT's for the internal standard and for each
analyte in the calibration standards at each concentration level as
described in Section 10.2.1. The RT's for the internal standard must not
vary by more than 0.10 minutes. Identify each analyte by comparison of
the RT's for peak maxima to the RT's determined in Section 10.2.1.
10.2.2.2 Compare the retention times (RT's) for each potential
analyte in the calibration standards for each concentration level to the
retention times determined in Section 10.2.1. The calibration is not
valid unless all RT's for all analytes meet the criteria given in
Section 9.3.2.
10.2.2.3 Tabulate the area responses and the concentrations for the
internal standard and each analyte in the calibration standards.
Calculate the response factor for the internal standard
(RFis) and the response factor for each compound relative to
the internal standard (RRF) for each concentration level using Equations
5 and 6, Section 12.
10.2.2.4 Using the RRF's from the calibration, calculate the percent
relative standard deviation (percent RSD) for each analyte in the
calibration standard using Equation 7, Section 12. The percent RSD for
each individual calibration analyte must be less than 15 percent. This
criterion must be met in order for the calibration to be valid. If the
criterion is met, the mean RRF's determined above are to be used until
the next calibration.
10.3 Daily Calibration Checks. The calibration curve (Section
10.2.2) must be checked and verified at least once each day that samples
are analyzed. This is accomplished by analyzing a calibration standard
that is at a concentration near the midpoint of the working range and
performing the checks in Sections 10.3.1, 10.3.2, and 10.3.3.
10.3.1 For each analyte in the calibration standard, calculate the
percent difference in the RRF from the last calibration using Equation
8, Section 12. If the percent difference for each calibration analyte is
less than 10 percent, the last calibration curve is assumed to be valid.
If the percent difference for any analyte is greater than 5 percent, the
analyst should consider this a warning limit. If the percent difference
for any one calibration analyte exceeds 10 percent, corrective action
must be taken. If no source of the problem can be determined after
corrective action has been taken, a new three-point (minimum)
calibration must be generated. This criterion must be met before
quantitative analysis begins.
10.3.2 If the RFis for the internal standard changes by
more than 20 percent from the last daily
calibration check, the system must be inspected for malfunctions and
corrections made as appropriate.
10.3.3 The retention times for the internal standard and all
calibration check analytes must be evaluated. If the retention time for
the internal standard or for any calibration check analyte changes by
more than 0.10 min from the last calibration, the system must be
inspected for malfunctions and corrections made as required.
11. Procedure
11.1 All samples and standards must be allowed to warm to room
temperature before analysis. Observe the given order of ingredient
addition to minimize loss of volatiles.
11.2 Bring the GC system to the determined operating conditions and
condition the column as described in Section 10.1.
Note: The temperature of the injection port may be an especially
critical parameter.Information about the proper temperature may be found
on the CPDS.
11.3 Perform the daily calibration checks as described in Section
10.3. Samples are not to be analyzed until the criteria in Section 10.3
are met.
11.4 Place the as-received coating sample on a paint shaker, or
similar device, and shake the sample for a minimum of 5 minutes to
achieve homogenization.
11.5 Note: The steps in this section must be performed rapidly and
without interruption to avoid loss of volatile organics. These steps
must be performed in a laboratory hood free from solvent vapors. All
weights must be recorded to the nearest 0.1 mg.
11.5.1 Add 16 g of dimethylformamide to each of two tared vials (A
and B) capable of being septum sealed.
11.5.2 To each vial add a weight of coating that will result in the
response for the major constituent being in the upper half of the linear
range of the calibration curve.
Note: The magnitude of the response obviously depends on the amount
of sample injected into the GC as specified in Section 11.8. This volume
must be the same as used
[[Page 245]]
for preparation of the calibration curve, otherwise shifts in compound
retention times may occur. If a sample is prepared that results in a
response outside the limits of the calibration curve, new samples must
be prepared; changing the volume injected to bring the response within
the calibration curve limits is not permitted.
11.5.3 Add a weight of internal standard to each vial (A and B)
that will result in the response for the internal standard being between
25 percent and 75 percent of the linear range of the calibration curve.
11.5.4 Seal the vials with crimp-on or Mininert[reg]
septum seals.
11.6 Shake the vials containing the prepared coating samples for 60
seconds. Allow the vials to stand undisturbed for ten minutes. If solids
have not settled out on the bottom after 10 minutes, then centrifuge at
1,000 rpm for 5 minutes. The analyst also has the option of injecting
the sample without allowing the solids to settle.
11.7 Analyses should be conducted in the following order: daily
calibration check sample, method blank, up to 10 injections from sample
vials (i.e., one injection each from up to five pairs of vials, which
corresponds to analysis of 5 coating samples).
11.8 Inject the prescribed volume of supernatant from the
calibration check sample, the method blank, and the sample vials onto
the chromatographic column and record the chromatograms while operating
the system under the specified operating conditions.
Note: The analyst has the option of injecting the unseparated
sample.
12. Data Analysis and Calculations
12.1 Qualitative Analysis. An analyte (e.g., those cited in Section
1.1) is considered tentatively identified if two criteria are satisfied:
(1) elution of the sample analyte within 0.05 min
of the average GC retention time of the same analyte in the calibration
standard; and (2) either (a) confirmation of the identity of the
compound by spectral matching on a gas chromatograph equipped with a
mass selective detector or (b) elution of the sample analyte within
0.05 min of the average GC retention time of the
same analyte in the calibration standard analyzed on a dissimilar GC
column.
12.1.1 The RT of the sample analyte must meet the criteria specified
in Section 9.3.3.
12.1.2 When doubt exists as to the identification of a peak or the
resolution of two or more components possibly comprising one peak,
additional confirmatory techniques (listed in Section 12.1) must be
used.
12.2 Quantitative Analysis. When an analyte has been identified, the
quantification of that compound will be based on the internal standard
technique.
12.2.1 A single analysis consists of one injection from each of two
sample vials (A and B) prepared using the same coating. Calculate the
concentration of each identified analyte in the sample as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.003
12.2.2 Report results for duplicate analysis (sample vials A and B)
without correction.
12.3 Precision Data. Calculate the percent difference between the
measured concentrations of each analyte in vials A and B as follows.
12.3.1 Calculate the weight percent of the analyte in each of the
two sample vials as described in Section 12.2.1.
12.3.2 Calculate the percent difference for each analyte as:
[GRAPHIC] [TIFF OMITTED] TR07DE95.004
[[Page 246]]
where Ai and Bi are the measured concentrations of
the analyte in vials A and B.
12.4 Calculate the percent accuracy for analytes in the QCCS (See
Section 9.4) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.005
where Xx is the mean measured value and Tx is the
known true value of the analyte in the QCCS.
12.5 Obtain retention times (RT's) from data station or integrator
or, for chromatograms from a chart recorder, calculate the RT's for
analytes in the calibration standards (See Section 10.2.2.2) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.006
12.6 Calculate the response factor for the internal standard (See
Section 10.2.2.3) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.007
where:
Ais = Area response of the internal standard.
Cis = Weight percent of the internal standard.
12.7 Calculate the relative response factors for analytes in the
calibration standards (See Section 10.2.2.3) as follows:
where:
[GRAPHIC] [TIFF OMITTED] TR07DE95.008
RRFx = Relative response factor for an individual
analyte.
Ax = Area response of the analyte being measured.
Cx = Weight percent of the analyte being measured.
12.8 Calculate the percent relative standard deviation of the
relative response factors for analytes in the calibration standards (See
Section 10.2.2.4) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.009
12.9 Calculate the percent difference in the relative response
factors between the calibration curve and the daily calibration checks
(See Section 10.3) as follows:
[[Page 247]]
[GRAPHIC] [TIFF OMITTED] TR07DE95.010
13. Measurement of Reaction Byproducts That are HAP [Reserved]
14. Method Performance [Reserved]
15. Pollution Prevention [Reserved]
16. Waste Management
16.1 The coating samples and laboratory standards and reagents may
contain compounds which require management as hazardous waste. It is the
laboratory's responsibility to ensure all wastes are managed in
accordance with all applicable laws and regulations.
16.2 To avoid excessive laboratory waste, obtain only enough sample
for laboratory analysis.
16.3 It is recommended that discarded waste coating solids, used
rags, used paper towels, and other nonglass or nonsharp waste materials
be placed in a plastic bag before disposal. A separate container,
designated ``For Sharp Objects Only,'' is recommended for collection of
discarded glassware and other sharp-edge items used in the laboratory.
It is recommended that unused or excess samples and reagents be placed
in a solvent-resistant plastic or metal container with a lid or cover
designed for flammable liquids. This container should not be stored in
the area where analytical work is performed. It is recommended that a
record be kept of all compounds placed in the container for
identification of the contents upon disposal.
17. References
1. Clean Air Act Amendments, Public Law 101-549, Titles I-XI,
November, 1990.
2. Standard Test Method for Water Content of Water-Reducible Paints
by Direct Injection into a Gas Chromatograph. ASTM Designation D3792-79.
3. Standard Practice for Sampling Liquid Paints and Related Pigment
Coatings. ASTM Designation D3925-81.
4. Standard Test Method for Determination of Dichloromethane and
1,1,1-Trichloroethane in Paints and Coatings by Direct Injection into a
Gas Chromatograph. ASTM Designation D4457-85.
5. Standard Test Method for Determining the Unreacted Monomer
Content of Latexes Using Capillary Column Gas Chromatography. ASTM
Designation D4827-93.
6. Standard Test Method for Determining Unreacted Monomer Content of
Latexes Using Gas-Liquid Chromatography. ASTM Designation D 4747-87.
7. Method 301--``Field Validation of Pollutant Measurement Methods
from Various Waste Media,'' 40 CFR 63, Appendix A.
8. ``Reagent Chemicals, American Chemical Society Specifications,''
American Chemical Society, Washington, DC. For suggestions on the
testing of reagents not listed by the American Chemical Society, see
``Reagent Chemicals and Standards'' by Joseph Rosin, D. Van Nostrand
Co., Inc., New York, NY and the ``United States Pharmacopeia.''
18. Tables, Diagrams, Flowcharts, and Validation Data
Agency:_________________________________________________________________
Inspector:______________________________________________________________
Date/Time:______________________________________________________________
Sample ID:_____________________________________________________
Source ID:______________________________________________________________
Coating Name/Type:______________________________________________________
Plant Witness:__________________________________________________________
Type Analysis Required:_________________________________________________
Special Handling:_______________________________________________________
Sample Container Label
Coating Data
Date:___________________________________________________________________
Source:_________________________________________________________________
------------------------------------------------------------------------
Data Sample ID No. Sample ID No.
------------------------------------------------------------------------
Coating:
Supplier Name....................... .............. ..............
Name and Color of Coating........... .............. ..............
Type of Coating (primer, clearcoat, .............. ..............
etc.)..............................
[[Page 248]]
Identification Number for Coating... .............. ..............
Coating Density (lbs/gal)........... .............. ..............
Total Volatiles Content (wt percent) .............. ..............
Water Content (wt percent).......... .............. ..............
Exempt Solvents Content (wt percent) .............. ..............
VOC Content (wt percent)............ .............. ..............
Solids Content (vol percent)........ .............. ..............
Diluent Properties:
Name................................
Identification Number............... .............. ..............
Diluent Solvent Density (lbs/gal)... .............. ..............
VOC Content (wt percent)............ .............. ..............
Water Content (wt percent).......... .............. ..............
Exempt Solvent Content (wt percent). .............. ..............
Diluent/Solvent Ratio (gal diluent .............. ..............
solvent/gal coating)...............
------------------------------------------------------------------------
Stock Reference Standard
Name of Reference Material:_____________________________________________
Supplier Name:__________________________________________________________
Lot Number:_____________________________________________________________
Purity:_________________________________________________________________
Name of Solvent Material: Dimethylformamide_____________________________
Supplier Name:__________________________________________________________
Lot Number:_____________________________________________________________
Purity:_________________________________________________________________
Date Prepared:__________________________________________________________
Prepared By:____________________________________________________________
Notebook/page no.:______________________________________________________
Preparation Information
1. Weight Empty Flask.................. --------,g
2. Weight Plus DMF..................... --------,g
3. Weight Plus Reference Material...... --------,g
4. Weight After Made to Volume......... --------,g
5. Weight DMF (lines 2-1+3-4).......... --------,g
6. Weight Ref. Material (lines 3-2).... --------,g
7. Corrected Weight of Reference --------,g
Material (line 6 times purity).
8. Fraction Reference Material in --------,g/g
Standard (Line 7 / Line 5) soln.
9. Total Volume of Standard Solution... --------, ml
10. Weight Reference Material per ml of --------,g/ml
Solution (Line 7 / Line 9).
Laboratory ID No. for this Standard.... --------
Expiration Date for this Standard...... --------
CALIBRATION STANDARD
Date Prepared:__________________________________________________________
Date Expires:___________________________________________________________
Prepared By:____________________________________________________________
Notebook/page:__________________________________________________________
Calibration Standard Identification No.:
[fxsp0]_________________________________________________________________
Preparation Information
Final Weight Flask Plus Reagents....... --------, g
Weight Empty Flask..................... --------, g
Total Weight Of Reagents............... --------, g
--------------------------------------------------------------------------------------------------------------------------------------------------------
Amount of stock reference standard added (by Weight
Stock volume or by weight) Calculated percent
reference ---------------------------------------------------- weight analyte in
Analyte name \a\ standard ID Amount in Amount in analyte calibration
No. Volume standard, g/ Weight standard, g/ added, g standard
added, ml ml added, g g soln \b\
--------------------------------------------------------------------------------------------------------------------------------------------------------
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
[[Page 249]]
........... ........... ........... ........... ........... ........... ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------
\a\ Include internal standard(s).
\b\ Weight percent = weight analyte added / total weight of reagents.
Quality Control Check Standard
Date Prepared:__________________________________________________________
Date Expires:___________________________________________________________
Prepared By:____________________________________________________________
Notebook/page:__________________________________________________________
Quality Control Check Standard Identification No.:
[fxsp0]_________________________________________________________________
Preparation Information
Final Weight Flask Plus Reagents....... --------,g
Weight Empty Flask..................... --------,g
Total Weight Of Reagents............... --------,g
--------------------------------------------------------------------------------------------------------------------------------------------------------
Amount of stock reference standard added (by Weight
Stock volume or by weight) Calculated percent
reference ---------------------------------------------------- weight analyte in
Analyte name \a\ standard ID Amount in Amount in analyte QCC
No. Volume standard, g/ Weight standard, g/ added, g standard
added, ml ml added, g g soln \b\
--------------------------------------------------------------------------------------------------------------------------------------------------------
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
........... ........... ........... ........... ........... ........... ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------
\a\ Include internal Standard(s).
\b\ Weight percent=weight analyte added / total weight of reagents.
Quality Control Check Standard Analysis
Date OCCS Analyzed:_____________________________________________________
OCCS Identification No._________________________________________________
Analyst:________________________________________________________________
QCC Expiration Date:____________________________________________________
Analysis Results
--------------------------------------------------------------------------------------------------------------------------------------------------------
Weight percent determined Meets criteria in
--------------------------------- Section 9.4.6
Analyte Mean Wt Percent Percent ---------------------
Run 1 Run 2 Run 3 percent accuracx RSD Percent Percent
accuracy RSD
--------------------------------------------------------------------------------------------------------------------------------------------------------
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
......... ......... ......... ......... ......... ......... ......... .........
--------------------------------------------------------------------------------------------------------------------------------------------------------
Calibration of Gas Chromatograph
Calibration Date:_______________________________________________________
Calibrated By:
[[Page 250]]
________________________________________________________________________
Part 1--Retention Times for Individual Analytes
--------------------------------------------------------------------------------------------------------------------------------------------------------
Recorder chart speed Distance from injection point
Stock -------------------------------- to peak maximum Retention
Analyte standard. ID -------------------------------- time, minutes
No. Inches/min. cm/min. Inches Centimeters \a\
--------------------------------------------------------------------------------------------------------------------------------------------------------
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
--------------------------------------------------------------------------------------------------------------------------------------------------------
\a\ Retention time=distance to peak maxima/chart speed.
CALIBRATION OF GAS CHROMATOGRAPH
Calibration Date:_______________________________________________________
Calibrated By:__________________________________________________________
Part 2--Analysis of Calibration Standards
----------------------------------------------------------------------------------------------------------------
Calib. STD ID Calib. STD ID Calib. STD ID
Analyte No. No. No.
----------------------------------------------------------------------------------------------------------------
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
Internal Standard Name:
Conc. in STD................................................ .............. .............. ..............
Area Response............................................... .............. .............. ..............
RT.......................................................... .............. .............. ..............
----------------------------------------------------------------------------------------------------------------
Calibration of Gas Chromatograph
Calibration Date:_______________________________________________________
Calibrated By:
[[Page 251]]
________________________________________________________________________
Part 3--Data Analysis for Calibration Standards
--------------------------------------------------------------------------------------------------------------------------------------------------------
Is RT within 0.05 Is percent
Analyte ID ID ID Mean of RF min of RT for stock? RSD <30% (Y/
(Y/N) N)
--------------------------------------------------------------------------------------------------------------------------------------------------------
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
Name:
RT.............................................. ........... ........... ........... ........... ........... .................... ...........
RF.............................................. ........... ........... ........... ........... ........... .................... ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------
Daily Calibration Check
Date:___________________________________________________________________
Analyst:________________________________________________________________
Calibration Check Standard ID No.:
Expiration Date:________________________________________________________
--------------------------------------------------------------------------------------------------------------------------------------------------------
Retention Time (RT) Response Factor (RF)
Analyte -----------------------------------------------------------------------------------------------
Last This Difference \a\ Last This Difference \b\
--------------------------------------------------------------------------------------------------------------------------------------------------------
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
.............. .............. .............. .............. .............. ..............
--------------------------------------------------------------------------------------------------------------------------------------------------------
\a\ Retention time (RT) change (difference) must be less than 0.10 minutes.
\b\ Response factor (RF) change (difference) must be less than 20 percent for each analyte and for the internal standard.
Sample Analysis
Vial A ID No.:__________________________________________________________
Vial B ID No.:__________________________________________________________
Analyzed By:____________________________________________________________
Date:___________________________________________________________________
----------------------------------------------------------------------------------------------------------------
Sample preparation information Vial A (g) Vial B (g)
----------------------------------------------------------------------------------------------------------------
Measured:
wt empty via..........................................................
wt plus DMF...........................................................
wt plus sample........................................................
wt plus internal......................................................
standard..............................................................
Calculated:
wt DMF................................................................
wt sample.............................................................
wt internal standard..................................................
----------------------------------------------------------------------------------------------------------------
[[Page 252]]
Analysis Results: Duplicate Samples
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Area response Wt percent in sample
Analyte -------------------------------- RF -----------------------------------------------
Vial A Vial B Vial A Vial B Average
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Internal Standard.......................................
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Method 312A--Determination of Styrene in Latex Styrene-Butadiene Rubber,
Through Gas Chromatography
1. Scope and Application
1.1 This method describes a procedure for determining parts per
million (ppm) styrene monomer (CAS No. 100-42-5) in aqueous samples,
including latex samples and styrene stripper water.
1.2 The sample is separated in a gas chromatograph equipped with a
packed column and a flame ionization detector.
2.0 Summary of Method
2.1 This method utilizes a packed column gas chromatograph with a
flame ionization detector to determine the concentration of residual
styrene in styrene butadiene rubber (SBR) latex samples.
3.0 Definitions
3.1 The definitions are included in the text as needed.
4.0 Interferences
4.1 In order to reduce matrix effects and emulsify the styrene,
similar styrene free latex is added to the internal standard. There are
no known interferences.
4.2 The operating parameters are selected to obtain resolution
necessary to determine styrene monomer concentrations in latex.
5.0 Safety
5.1 It is the responsibility of the user of this procedure to
establish appropriate safety and health practices.
6.0 Equipment and Supplies
6.1 Adjustable bottle-top dispenser, set to deliver 3 ml. (for
internal standard), Brinkmann Dispensette, or equivalent.
6.2 Pipettor, set to 10 ml., Oxford Macro-set, or equivalent.
6.3 Volumetric flask, 100-ml, with stopper.
6.4 Hewlett Packard Model 5710A dual channel gas chromatograph
equipped with flame ionization detector.
6.4.1 11 ft. x \1/8\ in. stainless steel column packed with 10% TCEP
on 100/120 mesh Chromosorb P, or equivalent.
6.4.2 Perkin Elmer Model 023 strip chart recorder, or equivalent.
6.5 Helium carrier gas, zero grade.
6.6 Liquid syringe, 25-[micro]l.
6.7 Digital MicroVAX 3100 computer with VG Multichrom software, or
equivalent data handling system.
6.6 Wire Screens, circular, 70-mm, 80-mesh diamond weave.
6.7 DEHA--(N,N-Diethyl hydroxylamine), 97+% purity, CAS No. 3710-84-
7
6.8 p-Dioxane, CAS No. 123-91-1
7.0 Reagents and Standards
7.1 Internal standard preparation.
7.1.1 Pipette 5 ml p-dioxane into a 1000-ml volumetric flask and
fill to the mark with distilled water and mix thoroughly.
7.2 Calibration solution preparation.
7.2.1 Pipette 10 ml styrene-free latex (eg: NBR latex) into a 100-ml
volumetric flask.
7.2.2 Add 3 ml internal standard (section 7.1.1 of this method).
7.2.3 Weigh exactly 10 [micro]l fresh styrene and record the weight.
7.2.4 Inject the styrene into the flask and mix well.
7.2.5 Add 2 drops of DEHA, fill to the mark with water and mix well
again.
7.2.6 Calculate concentration of the calibration solution as
follows:
mg/l styrene=(mg styrene added)/0.1 L
8.0 Sample Collection, Preservation, and Storage
8.1 A representative SBR emulsion sample should be caught in a
clean, dry 6-oz. teflon lined glass container. Close it properly to
assure no sample leakage.
[[Page 253]]
8.2 The container should be labeled with sample identification, date
and time.
9.0 Quality Control
9.1 The instrument is calibrated by injecting calibration solution
(Section 7.2 of this method) five times.
9.2 The retention time for components of interest and relative
response of monomer to the internal standard is determined.
9.3 Recovery efficiency must be determined once for each sample type
and whenever modifications are made to the method.
9.3.1 A set of six latex samples shall be collected. Two samples
shall be prepared for analysis from each sample. Each sample shall be
analyzed in duplicate.
9.3.2 The second set of six latex samples shall be analyzed in
duplicate before spiking each sample with approximately 1000 ppm
styrene. The spiked samples shall be analyzed in duplicate.
9.3.3 For each hydrocarbon, calculate the average recovery
efficiency (R) using the following equations:
where:
R=[Sigma](Rn)/6
where:
Rn=(cns-cv)/Sn
n=sample number
cns=concentration of compound measured in spiked sample
number n.
cnu= concentration of compound measured in unspiked sample
number n.
Sn=theoretical concentration of compound spiked into sample
n.
9.3.4 A value of R between 0.70 and 1.30 is acceptable.
9.3.5 R is used to correct all reported results for each compound by
dividing the measured results of each compound by the R for that
compound for the same sample type.
10.0 Calibration and Instrument Settings
10.1 Injection port temperature, 250 [deg]C.
10.2 Oven temperature, 110 [deg]C, isothermal.
10.3 Carrier gas flow, 25 cc/min.
10.4 Detector temperature, 250 [deg]C.
10.5 Range, 1X.
11.0 Procedure
11.1 Turn on recorder and adjust baseline to zero.
11.2 Prepare sample.
11.2.1 For latex samples, add 3 ml Internal Standard (section 7.1 of
this method) to a 100-ml volumetric flask. Pipet 10 ml sample into the
flask using the Oxford pipettor, dilute to the 100-ml mark with water,
and shake well.
11.2.2 For water samples, add 3 ml Internal Standard (section 7.1 of
this method) to a 100-ml volumetric flask and fill to the mark with
sample. Shake well.
11.3 Flush syringe with sample.
11.4 Carefully inject 2 [micro]l of sample into the gas
chromatograph column injection port and press the start button.
11.5 When the run is complete the computer will print a report of
the analysis.
12.0 Data Analysis and Calculation
12.1 For samples that are prepared as in section 11.2.1 of this
method:
ppm styrene = AxD
Where:
A = ``ppm'' readout from computer
D = dilution factor (10 for latex samples)
12.2 For samples that are prepared as in section 11.2.2 of this
method, ppm styrene is read directly from the computer.
13.0 Method Performance
13.1 This test has a standard deviation (1) of 3.3 ppm at 100 ppm
styrene. The average Spike Recovery from six samples at 1000 ppm Styrene
was 96.7 percent. The test method was validated using 926 ppm styrene
standard. Six analysis of the same standard provided average 97.7
percent recovery. Note: These are example recoveries and do not replace
quality assurance procedures in this method.
14.0 Pollution Prevention
14.1 Waste generation should be minimized where possible. Sample
size should be an amount necessary to adequately run the analysis.
15.0 Waste Management
15.1 All waste shall be handled in accordance with Federal and State
environmental regulations.
16.0 References and Publications
16.1 40 CFR 63 Appendix A--Method 301 Test Methods Field Validation
of Pollutant Measurement
16.2 DSM Copolymer Test Method T-3060, dated October 19, 1995,
entitled: Determination of Residual Styrene in Latex, Leonard, C.D.,
Vora, N.M.et al
Method 312B--Determination of Residual Styrene in Styrene-Butadiene
(SBR) Rubber Latex by Capillary Gas Chromatography
1.0 Scope
1.1 This method is applicable to SBR latex solutions.
1.2 This method quantitatively determines residual styrene
concentrations in SBR latex solutions at levels from 80 to 1200 ppm.
[[Page 254]]
2.0 Principle of Method
2.1 A weighed sample of a latex solution is coagulated with an ethyl
alcohol (EtOH) solution containing a specific amount of alpha-methyl
styrene (AMS) as the internal standard. The extract of this coagulation
is then injected into a gas chromatograph and separated into individual
components. Quantification is achieved by the method of internal
standardization.
3.0 Definitions
3.1 The definitions are included in the text as needed.
4.0 Interferences [Reserved]
5.0 Safety
5.1 This method may involve hazardous materials, operations, and
equipment. This method does not purport to address all of the safety
problems associated with its use. It is the responsibility of the user
of this method to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
6.0 Equipment and Supplies
6.1 Analytical balance, 160 g capacity, and 0.1 mg resolution
6.2 Bottles, 2-oz capacity, with poly-cap screw lids
6.3 Mechanical shaker
6.4 Syringe, 10-ul capacity
6.5 Gas chromatograph, Hewlett Packard model 5890A, or equivalent,
configured with FID with a megabore jet, splitless injector packed with
silanized glass wool.
6.5.1 Establish the following gas chromatographic conditions, and
allow the system to thoroughly equilibrate before use.
Injection technique = Splitless
Injector temperature = 225 deg C
Oven temperature = 70 deg C (isothermal)
Detector: temperature = 300 deg C
range = 5
attenuation = 0
Carrier gas: helium = 47 ml/min
Detector gases: hydrogen = 30 ml/min
air = 270 ml/min
make-up = 0 ml/min
Analysis time: = 3.2 min at the specified carrier gas flow rate and
column temperature.
6.6 Gas chromatographic column, DB-1, 30 M X 0.53 ID, or equivalent,
with a 1.5 micron film thickness.
6.7 Data collection system, Perkin-Elmer/Nelson Series Turbochrom 4
Series 900 Interface, or equivalent.
6.8 Pipet, automatic dispensing, 50-ml capacity, and 2-liter
reservoir.
6.9 Flasks, volumetric, class A, 100-ml and 1000-ml capacity.
6.10 Pipet, volumetric delivery, 10-ml capacity, class A.
7.0 Chemicals and Reagents
CHEMICALS:
7.1 Styrene, C8H8, 99+%, CAS 100-42-5
7.2 Alpha methyl styrene, C9H10, 99%, CAS 98-83-9
7.3 Ethyl alcohol, C2H5OH, denatured formula 2B, CAS 64-17-5
REAGENTS:
7.4 Internal Standard Stock Solution: 5.0 mg/ml AMS in ethyl
alcohol.
7.4.1 Into a 100-ml volumetric flask, weigh 0.50 g of AMS to the
nearest 0.1 mg.
7.4.2 Dilute to the mark with ethyl alcohol. This solution will
contain 5.0 mg/ml AMS in ethyl alcohol and will be labeled the AMS STOCK
SOLUTION.
7.5 Internal Standard Working Solution: 2500 ug/50 ml of AMS in
ethyl alcohol.
7.5.1 Using a 10 ml volumetric pipet, quantitatively transfer 10.0
ml of the AMS STOCK SOLUTION into a 1000-ml volumetric flask.
7.5.2 Dilute to the mark with ethyl alcohol. This solution will
contain 2500 ug/50ml of AMS in ethyl alcohol and will be labeled the AMS
WORKING SOLUTION.
7.5.3 Transfer the AMS WORKING SOLUTION to the automatic dispensing
pipet reservoir.
7.6 Styrene Stock Solution: 5.0 mg/ml styrene in ethyl alcohol.
7.6.1 Into a 100-ml volumetric flask, weigh 0.50 g of styrene to the
nearest 0.1 mg.
7.6.2 Dilute to the mark with ethyl alcohol. This solution will
contain 5.0 mg/ml styrene in ethyl alcohol and will be labeled the
STYRENE STOCK SOLUTION.
7.7 Styrene Working Solution: 5000 ug/10 ml of styrene in ethyl
alcohol.
7.7.1 Using a 10-ml volumetric pipet, quantitatively transfer 10.0
ml of the STYRENE STOCK SOLUTION into a 100-ml volumetric flask.
7.7.2 Dilute to the mark with ethyl alcohol. This solution will
contain 5000 ug/10 ml of styrene in ethyl alcohol and will be labeled
the STYRENE WORKING SOLUTION.
8.0 Sample Collection, Preservation and Storage
8.1 Label a 2-oz sample poly-cap lid with the identity, date and
time of the sample to be obtained.
8.2 At the sample location, open sample valve for at least 15
seconds to ensure that the sampling pipe has been properly flushed with
fresh sample.
8.3 Fill the sample jar to the top (no headspace) with sample, then
cap it tightly.
8.4 Deliver sample to the Laboratory for testing within one hour of
sampling.
8.5 Laboratory testing will be done within two hours of the sampling
time.
8.6 No special storage conditions are required unless the storage
time exceeds 2
[[Page 255]]
hours in which case refrigeration of the sample is recommended.
9.0 Quality Control
9.1 For each sample type, 12 samples of SBR latex shall be obtained
from the process for the recovery study. Half the vials and caps shall
be tared, labeled ``spiked'', and numbered 1 through 6. The other vials
are labeled ``unspiked'' and need not be tared, but are also numbered 1
through 6.
9.2 The six vials labeled ``spiked'' shall be spiked with an amount
of styrene to approximate 50% of the solution's expected residual
styrene level.
9.3 The spiked samples shall be shaken for several hours and allowed
to cool to room temperature before analysis.
9.4 The six samples of unspiked solution shall be coagulated and a
mean styrene value shall be determined, along with the standard
deviation, and the percent relative standard deviation.
9.5 The six samples of the spiked solution shall be coagulated and
the results of the analyses shall be determined using the following
equations:
Mr=Ms-Mu
R=Mr/S
where:
Mu=Mean value of styrene in the unspiked sample
Ms=Measured amount of styrene in the spiked sample
Mr=Measured amount of the spiked compound
S=Amount of styrene added to the spiked sample
R=Fraction of spiked styrene recovered
9.6 A value of R between 0.70 and 1.30 is acceptable.
9.7 R is used to correct all reported results for each compound by
dividing the measured results of each compound by the R for that
compound for the same sample type.
10.0 Calibration
10.1 Using a 10-ml volumetric pipet, quantitatively transfer 10.0 ml
of the STYRENE WORKING SOLUTION (section 7.7.2 of this method) into a 2-
oz bottle.
10.2 Using the AMS WORKING SOLUTION equipped with the automatic
dispensing pipet (section 7.5.3 of this method), transfer 50.0 ml of the
internal standard solution into the 2-oz bottle.
10.3 Cap the 2-oz bottle and swirl. This is the calibration
standard, which contains 5000 [micro]g of styrene and 2500 [micro]g of
AMS.
10.4 Using the conditions prescribed (section 6.5 of this method),
chromatograph 1 [micro]l of the calibration standard.
10.5 Obtain the peak areas and calculate the relative response
factor as described in the calculations section (section 12.1 of this
method).
11.0 Procedure
11.1 Into a tared 2-oz bottle, weigh 10.0 g of latex to the nearest
0.1 g.
11.2 Using the AMS WORKING SOLUTION equipped with the automatic
dispensing pipet (section 7.5.3 of this method), transfer 50.0 ml of the
internal standard solution into the 2-oz bottle.
11.3 Cap the bottle. Using a mechanical shaker, shake the bottle for
at least one minute or until coagulation of the latex is complete as
indicated by a clear solvent.
11.4 Using the conditions prescribed (section 6.5 of this method),
chromatograph 1 ul of the liquor.
11.5 Obtain the peak areas and calculate the concentration of
styrene in the latex as described in the calculations section (Section
12.2 of this method).
12.0 Calculations
12.1 Calibration:
RF=(WxxAis) / (WisxAx)
where:
RF=the relative response factor for styrene
Wx=the weight (ug) of styrene
Ais=the area of AMS
Wis=the weight (ug) of AMS
Ax=the area of styrene
12.2 Procedure:
ppmstyrene=(Ax RFxWis) /
(AisxWs)
where:
ppmstyrene=parts per million of styrene in the latex
Ax=the area of styrene
RF=the response factor for styrene
Wis=the weight (ug) of AMS
Ais=the area of AMS
Ws=the weight (g) of the latex sample
12.3 Correct for recovery (R) as determined by section 9.0 of this
method.
13.0 Precision
13.1 Precision for the method was determined at the 80, 144, 590,
and 1160 ppm levels. The standard deviations were 0.8, 1.5, 5 and 9 ppm
respectively. The percent relative standard deviations (%RSD) were 1% or
less at all levels. Five degrees of freedom were used for all precision
data except at the 80 ppm level, where nine degrees of freedom were
used. Note: These are example results and do not replace quality
assurance procedures in this method.
14.0 Pollution Prevention
14.1 Waste generation should be minimized where possible. Sample
size should be an amount necessary to adequately run the analysis.
15.0 Waste Management
15.1 Discard liquid chemical waste into the chemical waste drum.
[[Page 256]]
15.2 Discard latex sample waste into the latex waste drum.
15.3 Discard polymer waste into the polymer waste container.
16.0 References
16.1 This method is based on Goodyear Chemical Division Test Method
E-889.
Method 312C--Determination of Residual Styrene in SBR Latex Produced by
Emulsion Polymerization
1.0 Scope
1.1 This method is applicable for determining the amount of residual
styrene in SBR latex as produced in the emulsion polymerization process.
2.0 Principle of Method
2.1 A weighed sample of latex is coagulated in 2-propanol which
contains alpha-methyl styrene as an Internal Standard. The extract from
the coagulation will contain the alpha-methyl styrene as the Internal
Standard and the residual styrene from the latex. The extract is
analyzed by a Gas Chromatograph. Percent styrene is calculated by
relating the area of the styrene peak to the area of the Internal
Standard peak of known concentration.
3.0 Definitions
3.1 The definitions are included in the text as needed.
4.0 Interferences [Reserved]
5.0 Safety
5.1 When using solvents, avoid contact with skin and eyes. Wear hand
and eye protection. Wash thoroughly after use.
5.2 Avoid overexposure to solvent vapors. Handle only in well
ventilated areas.
6.0 Equipment and Supplies
6.1 Gas Chromatograph--Hewlett Packard 5890, Series II with flame
ionization detector, or equivalent.
Column--HP 19095F-123, 30m x 0.53mm, or equivalent. Substrate HP
FFAP (cross-linked) film thickness 1 micrometer. Glass injector port
liners with silanized glass wool plug.
Integrator--HP 3396, Series II, or equivalent.
6.2 Wrist action shaker
6.3 Automatic dispenser
6.4 Automatic pipet, calibrated to deliver 5.0 0.01 grams of latex
6.5 Four-ounce wide-mouth bottles with foil lined lids
6.6 Crimp cap vials, 2ml, teflon lined septa
6.7 Disposable pipets
6.8 Qualitative filter paper
6.9 Cap crimper
6.10 Analytical balance
6.11 10ml pipette
6.12 Two-inch funnel
7.0 Reagents and Standards
7.1 2-Propanol (HP2C grade)
7.2 Alpha methyl styrene (99+% purity)
7.3 Styrene (99+% purity)
7.4 Zero air
7.5 Hydrogen (chromatographic grade)
7.6 Helium
7.7 Internal Standard preparation
7.7.1 Weigh 5.000-5.005 grams of alpha-methyl styrene into a 100ml
volumetric flask and bring to mark with 2-propanol to make Stock ``A''
Solution.
Note: Shelf life--6 months.
7.7.2 Pipette 10ml of Stock ``A'' Solution into a 100ml volumetric
flask and bring to mark with 2-propanol to prepare Stock ``B'' Solution.
7.7.3 Pipette 10ml of the Stock ``B'' solution to a 1000ml
volumetric flask and bring to the mark with 2-propanol. This will be the
Internal Standard Solution (0.00005 grams/ml).
7.8 Certification of Internal Standard--Each batch of Stock ``B''
Solution will be certified to confirm concentration.
7.8.1 Prepare a Standard Styrene Control Solution in 2-propanol by
the following method:
7.8.1.1 Weigh 5.000 .005g of styrene to a
100ml volumetric flask and fill to mark with 2-propanol to make Styrene
Stock ``A'' Solution.
7.8.1.2 Pipette 10ml of Styrene Stock ``A'' Solution to a 100ml
volumetric flask and fill to mark with 2-propanol to make Styrene Stock
``B'' Solution.
7.8.1.3 Pipette 10ml of Styrene Stock ``B'' soluion to a 250ml
volumtric flask and fill to mark wtih 2-propanol to make the
Certification Solution.
7.8.2 Certify Alpha-Methyl Styrene Stock ``B'' Solution.
7.8.2.1 Pipette 5ml of the Certification Solution and 25ml of the
Alpha Methyl Styrene Internal Standard Solution to a 4-oz. bottle, cap
and shake well.
7.8.2.2 Analyze the resulting mixture by GC using the residual
styrene method. (11.4-11.6 of this method)
7.8.2.3 Calculate the weight of alpha methyl styrene present in the
25ml aliquat of the new Alpha Methyl Styrene Standard by the following
equation:
Wx = Fx xWis(Ax/
Ais)
Where
Ax = Peak area of alpha methyl styrene
Ais = Peak area of styrene
Wx = Weight of alpha methyl styrene
Wis = Weight of styrene (.00100)
Fx = Analyzed response factor = 1
[[Page 257]]
The Alpha Methyl Styrene Stock Solution used to prepare the Internal
Standard Solution may be considered certified if the weight of alpha
methyl styrene analyzed by this method is within the range of .00121g to
.00129g.
8.0 Sampling
8.1 Collect a latex sample in a capped container. Cap the bottle and
identify the sample as to location and time.
8.2 Deliver sample to Laboratory for testing within one hour.
8.3 Laboratory will test within two hours.
8.4 No special storage conditions are required.
9.0 Quality Control
9.1 The laboratory is required to operate a formal quality control
program. This consists of an initial demonstration of the capability of
the method as well as ongoing analysis of standards, blanks, and spiked
samples to demonstrate continued performance.
9.1.1 When the method is first set up, a calibration is run and the
recovery efficiency for each type of sample must be determined.
9.1.2 If new types of samples are being analyzed, then recovery
efficiency for each new type of sample must be determined. New type
includes any change, such as polymer type, physical form or a
significant change in the composition of the matrix.
9.2 Recovery efficiency must be determined once for each sample type
and whenever modifications are made to the method.
9.2.1 In determining the recovery efficiency, the quadruplet
sampling system shall be used. Six sets of samples (for a total of 24)
shall be taken. In each quadruplet set, half of the samples (two out of
the four) shall be spiked with styrene.
9.2.2 Prepare the samples as described in section 8 of this method.
To the vials labeled ``spiked'', add a known amount of styrene that is
expected to be present in the latex.
9.2.3 Run the spiked and unspiked samples in the normal manner.
Record the concentrations of styrene reported for each pair of spiked
and unspiked samples with the same vial number.
9.2.4 For each hydrocarbon, calculate the average recovery
efficiency (R) using the following equation:
R=[Sigma](Rn)/12
Where: n = sample number
Rn=(Ms-Mu)/S
Ms=total mass of compound (styrene) measured in spiked sample
([micro]g)
Mu=total mass of compound (styrene) measured in unspiked
sample ([micro]g)
S=theoretical mass of compound (styrene) spiked into sample ([micro]g)
R=fraction of spiked compound (styrene) recovered
9.2.5 A different R value should be obtained for each sample type. A
value of R between 0.70 and 1.30 is acceptable.
9.2.6 R is used to correct all reported results for each compound by
dividing the measured results of each compound by the R for that
compound for the same sample type.
10.0 Calibration
A styrene control sample will be tested weekly to confirm the FID
response and calibration.
10.1 Using the Styrene Certification Solution prepared in 7.8.1,
perform test analysis as described in 7.8.2 using the equation in
7.8.2.3 to calculate results.
10.2 Calculate the weight of styrene in the styrene control sample
using the following equation:
Wsty=(Fx xAsty
xWis)Ais
The instrument can be considered calibrated if the weight of the
styrene analyzed is within range of 0.00097-0.00103gms.
11.0 Procedure
11.1 Using an auto pipet, add 25ml of Internal Standard Solution to
a 4 oz. wide-mouth bottle.
11.2 Using a calibrated auto pipet, add 5.0 0.01g latex to the bottle containing the 25ml of
Internal Standard Solution.
11.3 Cap the bottle and place on the wrist action shaker. Shake the
sample for a minimum of five minutes using the timer on the shaker.
Remove from shaker.
11.4 Using a disposable pipet, fill the 2ml sample vial with the
clear alcohol extract. (If the extract is not clear, it should be
filtered using a funnel and filter paper.) Cap and seal the vial.
11.5 Place the sample in the autosampler tray and start the GC and
Integrator. The sample will be injected into the GC by the auto-
injector, and the Integrator will print the results.
11.6 Gas Chromatograph Conditions
Oven Temp--70 [deg]C
Injector Temp--225 [deg]C
Detector Temp--275 [deg]C
Helium Pressure--500 KPA
Column Head Pressure--70 KPA
Makeup Gas--30 ml/min.
Column--HP 19095F--123, 30mx0.53mm Substrate: HP--FFAP (cross-linked) 1
micrometer film thickness
12.0 Calculations
12.1 The integrator is programmed to do the following calculation at
the end of the analysis:
%ResidualStyrene=(Ax XWis)/(Ais
XWx)XFx X100
Where:
Ax=Peak area of styrene
Ais=Peak area of internal standard
[[Page 258]]
Wx=Weight of sample = 5g
Wis=Weight of internal std. = 0.00125g
Fx=Analyzed response factor = 1.0
12.2 The response factor is determined by analyzing a solution of
0.02g of styrene and 0.02g of alpha methyl styrene in 100ml of 2-
propanol. Calculate the factor by the following equation:
Fx=(Wx xAis)/(Wis
xAx)
Where:
Wx=Weight of styrene
Ax=Peak area of styrene
Wis=Weight of alpha methyl styrene
Ais=Peak area of alpha methyl styrene
13.0 Method Performance
13.1 Performance must be determined for each sample type by
following the procedures in section 9 of this method.
14.0 Waste Generation
14.1 Waste generation should be minimized where possible.
15.0 Waste Management
15.1 All waste shall be handled in accordance with Federal and State
environmental regulations.
16.0 References [Reserved]
Method 313A--Determination of Residual Hydrocarbons in Rubber Crumb
1.0 Scope and Application
1.1 This method determines residual toluene and styrene in stripper
crumb of the of the following types of rubber: polybutadiene (PBR) and
styrene/butadiene rubber (SBR), both derived from solution
polymerization processes that utilize toluene as the polymerization
solvent.
1.2 The method is applicable to a wide range of concentrations of
toluene and styrene provided that calibration standards cover the
desired range. It is applicable at least over the range of 0.01 to 10.0
% residual toluene and from 0.1 to 3.0 % residual styrene. It is
probably applicable over a wider range, but this must be verified prior
to use.
1.3 The method may also be applicable to other process samples as
long as they are of a similar composition to stripper crumb. See section
3.1 of this method for a description of stripper crumb.
2.0 Summary of Method
2.1 The wet crumb is placed in a sealed vial and run on a headspace
sampler which heats the vial to a specified temperature for a specific
time and then injects a known volume of vapor into a capillary GC. The
concentration of each component in the vapor is proportional to the
level of that component in the crumb sample and does not depend on water
content of the crumb.
2.2 Identification of each component is performed by comparing the
retention times to those of known standards.
2.3 Results are calculated by the external standard method since
injections are all performed in an identical manner. The response for
each component is compared with that obtained from dosed samples of
crumb.
2.4 Measured results of each compound are corrected by dividing each
by the average recovery efficiency determined for the same compound in
the same sample type.
3.0 Definitions
3.1 Stripper crumb refers to pieces of rubber resulting from the
steam stripping of a toluene solution of the same polymer in a water
slurry. The primary component of this will be polymer with lesser
amounts of entrained water and residual toluene and other hydrocarbons.
The amounts of hydrocarbons present must be such that the crumb is a
solid material, generally less that 10 % of the dry rubber weight.
4.0 Interferences
4.1 Contamination is not normally a problem since samples are sealed
into vials immediately on sampling.
4.2 Cross contamination in the headspace sampler should not be a
problem if the correct sampler settings are used. This should be
verified by running a blank sample immediately following a normal or
high sample. Settings may be modified if necessary if this proves to be
a problem, or a blank sample may be inserted between samples.
4.3 Interferences may occur if volatile hydrocarbons are present
which have retention times close to that of the components of interest.
Since the solvent makeup of the processes involved are normally fairly
well defined this should not be a problem. If it is found to be the
case, switching to a different chromatographic column will probably
resolve the situation.
5.0 Safety
5.1 The chemicals specified in this method should all be handled
according to standard laboratory practices as well as any special
precautions that may be listed in the MSDS for that compound.
5.2 Sampling of strippers or other process streams may involve high
pressures and temperatures or may have the potential for exposure to
chemical fumes. Only personnel who have been trained in the specific
sampling procedures required for that process should perform this
operation. An understanding of the process involved is necessary. Proper
personal protective equipment should be worn. Any sampling devices
should be inspected prior to use. A detailed sampling
[[Page 259]]
procedure which specifies exactly how to obtain the sample must be
written and followed.
6.0 Equipment and Supplies
6.1 Hewlett Packard (HP) 7694 Headspace sampler, or equivalent, with
the following conditions:
Times (min.): GC cycle time 6.0 , vial equilibration 30.0 ,
pressurization 0.25 , loop fill 0.25, loop equilibration 0.05 , inject
0.25
Temperatures (deg C): oven 70, loop 80, transfer line 90
Pressurization gas: He @ 16 psi
6.2 HP 5890 Series II capillary gas chromatograph, or equivalent,
with the following conditions:
Column: Supelco SPB-1, or equivalent, 15m x .25mm x .25 [micro] film
Carrier: He @ 6 psi
Run time: 4 minutes
Oven: 70 deg C isothermal
Injector: 200 deg C split ratio 50:1
Detector: FID @ 220 deg C
6.3 HP Chemstation consisting of computer, printer and Chemstation
software, or an equivalent chromatographic data system.
6.4 20 ml headspace vials with caps and septa.
6.5 Headspace vial crimper.
6.6 Microliter pipetting syringes.
6.7 Drying oven at 100 deg C vented into cold trap or other means of
trapping hydrocarbons released.
6.8 Laboratory shaker or tumbler suitable for the headspace vials.
6.9 Personal protective equipment required for sampling the process
such as rubber gloves and face and eye protection.
7.0 Reagents and Standards
7.1 Toluene, 99.9+% purity, HPLC grade.
7.2 Styrene, 99.9+% purity, HPLC grade.
7.3 Dry rubber of same type as the stripper crumb samples.
8.0 Sample Collection, Preservation and Storage
8.1 Collect a sample of crumb in a manner appropriate for the
process equipment being sampled.
8.1.1 If conditions permit, this may be done by passing a stream of
the crumb slurry through a strainer, thus separating the crumb from the
water. Allow the water to drain freely, do not attempt to squeeze any
water from the crumb. Results will not depend on the exact water content
of the samples. Immediately place several pieces of crumb directly into
a headspace vial. This should be done with rubber gloves to protect the
hands from both the heat and from contact with residual hydrocarbons.
The vial should be between \1/4\ and \1/3\ full. Results do not depend
on sample size as long as there is sufficient sample to reach an
equilibrium vapor pressure in the headspace of the vial. Cap and seal
the vial. Prepare each sample at least in duplicate. This is to minimize
the effect of the variation that naturally occurs in the composition of
non homogeneous crumb. The free water is not analyzed by this method and
should be disposed of appropriately along with any unused rubber crumb.
8.1.2 Alternatively the process can be sampled in a specially
constructed sealed bomb which can then be transported to the laboratory.
The bomb is then cooled to ambient temperature by applying a stream of
running water. The bomb can then be opened and the crumb separated from
the water and the vials filled as described in section 8.1.1 of this
method. The bomb may be stored up to 8 hours prior to transferring the
crumb into vials.
8.2 The sealed headspace vials may be run immediately or may be
stored up to 72 hours prior to running. It is possible that even longer
storage times may be acceptable, but this must be verified for the
particular type of sample being analyzed (see section 9.2.3 of this
method). The main concern here is that some types of rubber eventually
may flow, thus compacting the crumb so that the surface area is reduced.
This may have some effect on the headspace equilibration.
9.0 Quality Control
9.1 The laboratory is required to operate a formal quality control
program. This consists of an initial demonstration of the capability of
the method as well as ongoing analysis of standards, blanks and spiked
samples to demonstrate continued performance.
9.1.1 When the method is first set up a calibration is run
(described in section 10 of this method) and an initial demonstration of
method capability is performed (described in section 9.2 of this
method). Also recovery efficiency for each type of sample must be
determined (see section 9.4 of this method).
9.1.2 It is permissible to modify this method in order to improve
separations or make other improvements, provided that all performance
specifications are met. Each time a modification to the method is made
it is necessary to repeat the calibration (section 10 of this method),
the demonstration of method performance (section 9.2 of this method) and
the recovery efficiency for each type of sample (section 9.4 of this
method).
9.1.3 Ongoing performance should be monitored by running a spiked
rubber standard. If this test fails to demonstrate that the analysis is
in control, then corrective action must be taken. This method is
described in section 9.3 of this method.
9.1.4 If new types of samples are being analyzed then recovery
efficiency for each new type of sample must be determined. New type
includes any change, such as polymer
[[Page 260]]
type, physical form or a significant change in the composition of the
matrix.
9.2 Initial demonstration of method capability to establish the
accuracy and precision of the method. This is to be run following the
calibration described in section 10 of this method.
9.2.1 Prepare a series of identical spiked rubber standards as
described in section 9.3 of this method. A sufficient number to
determine statistical information on the test should be run. Ten may be
a suitable number, depending on the quality control methodology used at
the laboratory running the tests. These are run in the same manner as
unknown samples (see section 11 of this method).
9.2.2 Determine mean and standard deviation for the results. Use
these to determine the capability of the method and to calculate
suitable control limits for the ongoing performance check which will
utilize the same standards.
9.2.3 Prepare several additional spiked rubber standards and run 2
each day to determine the suitability of storage of the samples for 24,
48 and 72 hours or longer if longer storage times are desired.
9.3 A spiked rubber standard should be run on a regular basis to
verify system performance. This would probably be done daily if samples
are run daily. This is prepared in the same manner as the calibration
standards (section 10.1 of this method), except that only one
concentration of toluene and styrene is prepared. Choose concentrations
of toluene and styrene that fall in the middle of the range expected in
the stripper crumb and then do not change these unless there is a major
change in the composition of the unknowns. If it becomes necessary to
change the composition of this standard the initial performance
demonstration must be repeated with the new standard (section 9.2 of
this method).
9.3.1 Each day prepare one spiked rubber standard to be run the
following day. The dry rubber may be prepared in bulk and stored for any
length of time consistent with the shelf life of the product. The
addition of water and hydrocarbons must be performed daily and all the
steps described under section 10.1 of this method must be followed.
9.3.2 Run the spiked rubber standard prepared the previous day.
Record the results and plot on an appropriate control chart or other
means of determining statistical control.
9.3.3 If the results for the standard indicate that the test is out
of control then corrective action must be taken. This may include a
check on procedures, instrument settings, maintenance or recalibration.
Samples may be stored (see section 8.2 of this method) until compliance
is demonstrated.
9.4 Recovery efficiency must be determined once for each sample type
and whenever modifications are made to the method.
9.4.1 For each sample type collect 12 samples from the process
(section 8.1 of this method). This should be done when the process is
operating in a normal manner and residual hydrocarbon levels are in the
normal range. Half the vials and caps should be tared, labeled
``spiked'' and numbered 1 through 6. The other vials are labeled
``unspiked'' and need not be tared but are also numbered 1 through 6.
Immediately on sampling, the vials should be capped to prevent loss of
volatiles. Allow all the samples to cool completely to ambient
temperature. Reweigh each of the vials labeled ``spiked'' to determine
the weight of wet crumb inside.
9.4.2 The dry weight of rubber present in the wet crumb is estimated
by multiplying the weight of wet crumb by the fraction of nonvolatiles
typical for the sample. If this is not known, an additional quantity of
crumb may be sampled, weighed, dried in an oven and reweighed to
determine the fraction of volatiles and nonvolatiles prior to starting
this procedure.
9.4.3 To the vials labeled ``spiked'' add an amount of a mixture of
toluene and styrene that is between 40 and 60 % of the amount expected
in the crumb. This is done by removing the cap, adding the mixture by
syringe, touching the tip of the needle to the sample in order to remove
the drop and then immediately recapping the vials. The mixture is not
added through the septum, because a punctured septum may leak and vent
vapors as the vial is heated. The weights of toluene and styrene added
may be calculated from the volumes of the mixture added, its composition
and density, or may be determined by the weight of the vials and caps
prior to and after addition. The exact dry weight of rubber present and
the concentration of residual toluene and styrene are not known at this
time so an exact calculation of the concentration of hydrocarbons is not
possible until the test is completed.
9.4.4 Place all the vials onto a shaker or tumbler for 24 2 hours. This is essential in order for the hydrocarbons
to be evenly distributed and completely absorbed into the rubber. If
this is not followed the toluene and styrene will be mostly at the
surface of the rubber and high results will be obtained.
9.4.5 Remove the vials from the shaker and tap them so that all the
crumb settles to the bottom of the vials. Allow them to stand for 1 hour
prior to analysis to allow any liquid to drain fully to the bottom.
9.4.6 Run the spiked and unspiked samples in the normal manner.
Record the concentrations of toluene and styrene reported for each pair
of spiked and unspiked samples with the same vial number.
9.4.7 Open each of the vials labeled ``spiked'', remove all the
rubber crumb and
[[Page 261]]
place it into a tarred drying pan. Place in a 100 deg C oven for two
hours, cool and reweigh. Subtract the weight of the tare to give the dry
weight of rubber in each spiked vial. Calculate the concentration of
toluene and styrene spiked into each vial as percent of dry rubber
weight. This will be slightly different for each vial since the weights
of dry rubber will be different.
9.4.8 For each hydrocarbon calculate the average recovery efficiency
(R) using the following equations:
R=R--[Sigma](Pn)/6 (average of the 6 individual Rn
values)
Where:
Rn=(Cns--Cnu) / Sn
Where:
n=vial number
Cns=concentration of compound measured in spiked sample number n.
Cnu=concentration of compound measured in unspiked sample number n.
Sn=theoretical concentration of compound spiked into sample n calculated
in step 9.4.7
9.4.9 A different R value should be obtained for each compound
(styrene and toluene) and for each sample type.
9.4.10 A value of R between 0.70 and 1.30 is acceptable.
9.4.11 R is used to correct all reported results for each compound
by dividing the measured results of each compound by the R for that
compound for the same sample type (see section 12.2 of this method.)
10.0 Calibration
10.1 Calibration standards are prepared by dosing known amounts of
the hydrocarbons of interest into vials containing known amounts of
rubber and water.
10.1.1 Cut a sufficient quantity of dry rubber of the same type as
will be analyzed into pieces about the same size as that of the crumb.
Place these in a single layer on a piece of aluminum foil or other
suitable surface and place into a forced air oven at 100 [deg]C for four
hours. This is to remove any residual hydrocarbons that may be present.
This step may be performed in advance.
10.1.2 Into each of a series of vials add 3.0 g of the dry rubber.
10.1.3 Into each vial add 1.0 ml distilled water or an amount that
is close to the amount that will be present in the unknowns. The exact
amount of water present does not have much effect on the analysis, but
it is necessary to have a saturated environment. The water will also aid
in the uniform distribution of the spiked hydrocarbons over the surface
of the rubber after the vials are placed on the shaker (in step 10.1.5
of this method).
10.1.4 Into each vial add varying amounts of toluene and styrene by
microliter syringe and cap the vials immediately to prevent loss. The
tip of the needle should be carefully touched to the rubber in order to
transfer the last drop to the rubber. Toluene and styrene may first be
mixed together in suitable proportions and added together if desired.
The weights of toluene and styrene added may be calculated from the
volumes of the mixture added, its composition and density, or may be
determined by the weight of the vials and caps prior to and after
addition. Concentrations of added hydrocarbons are calculated as percent
of the dry rubber weight. At least 5 standards should be prepared with
the amounts of hydrocarbons added being calculated to cover the entire
range possible in the unknowns. Retain two samples with no added
hydrocarbons as blanks.
10.1.5 Place all the vials onto a shaker or tumbler for 24 2 hours. This is essential in order for the hydrocarbons
to be evenly distributed and completely absorbed into the rubber. If
this is not followed the toluene and styrene will be mostly at the
surface of the rubber and high results will be obtained.
10.1.6 Remove the vials from the shaker and tap them so that all the
crumb settles to the bottom of the vials. Allow them to stand for 1 hour
prior to analysis to allow any liquid to drain fully to the bottom.
10.2 Run the standards and blanks in the same manner as described
for unknowns (section 11 of this method), starting with a blank, then in
order of increasing hydrocarbon content and ending with the other blank.
10.3 Verify that the blanks are sufficiently free from toluene and
styrene or any interfering hydrocarbons.
10.3.1 It is possible that trace levels may be present even in dry
product. If levels are high enough that they will interfere with the
calibration then the drying procedure in section 10.1.1 of this method
should be reviewed and modified as needed to ensure that suitable
standards can be prepared.
10.3.2 It is possible that the final blank is contaminated by the
previous standard. If this is the case review and modify the sampler
parameters as needed to eliminate this problem. If necessary it is
possible to run blank samples between regular samples in order to reduce
this problem, though it should not be necessary if the sampler is
properly set up.
10.4 Enter the amounts of toluene and styrene added to each of the
samples (as calculated in section 10.1.4 of this method) into the
calibration table and perform a calibration utilizing the external
standard method of analysis.
10.5 At low concentrations the calibration should be close to
linear. If a wide range of levels are to be determined it may be
desirable to apply a nonlinear calibration to get the best fit.
[[Page 262]]
11.0 Procedure
11.1 Place the vials in the tray of the headspace sampler. Enter the
starting and ending positions through the console of the sampler. For
unknown samples each is run in duplicate to minimize the effect of
variations in crumb composition. If excessive variation is noted it may
be desirable to run more than two of each sample.
11.2 Make sure the correct method is loaded on the Chemstation. Turn
on the gas flows and light the FID flame.
11.3 Start the sequence on the Chemstation. Press the START button
on the headspace unit. The samples will be automatically injected after
equilibrating for 30 minutes in the oven. As each sample is completed
the Chemstation will calculate and print out the results as percent
toluene and styrene in the crumb based on the dry weight of rubber.
12.0 Data Analysis and Calculations
12.1 For each set of duplicate samples calculate the average of the
measured concentration of toluene and styrene. If more than two
replicates of each sample are run calculate the average over all
replicates.
12.2 For each sample correct the measured amounts of toluene and
styrene using the following equation:
Corrected Result = Cm/R
Where:
Cm = Average measured concentration for that compound.
R = Recovery efficiency for that compound in the same sample type (see
section 9.4 of this method)
12.3 Report the recovery efficiency (R) and the corrected results of
toluene and styrene for each sample.
13.0 Method Performance
13.1 This method can be very sensitive and reproducible. The actual
performance depends largely on the exact nature of the samples being
analyzed. Actual performance must be determined by each laboratory for
each sample type.
13.2 The main source of variation is the actual variation in the
composition of non homogeneous crumb in a stripping system and the small
sample sizes employed here. It therefore is the responsibility of each
laboratory to determine the optimum number of replicates of each sample
required to obtain accurate results.
14.0 Pollution Prevention
14.1 Samples should be kept sealed when possible in order to prevent
evaporation of hydrocarbons.
14.2 When drying of samples is required it should be done in an oven
which vents into a suitable device that can trap the hydrocarbons
released.
14.3 Dispose of samples as described in section 15.
15.0 Waste Management
15.1 Excess stripper crumb and water as well as the contents of the
used sample vials should be properly disposed of in accordance with
local and federal regulations.
15.2 Preferably this will be accomplished by having a system of
returning unused and spent samples to the process.
16.0 References
16.1 ``HP 7694 Headspace Sampler--Operating and Service Manual'',
Hewlett-Packard Company, publication number G1290-90310, June 1993.
Method 313B--The Determination of Residual Hydrocarbon in Solution
Polymers by Capillary Gas Chromatography
1.0 Scope
1.1 This method is applicable to solution polymerized polybutadiene
(PBD).
1.2 This method quantitatively determines n-hexane in wet crumb
polymer at levels from 0.08 to 0.15% by weight.
1.3 This method may be extended to the determination of other
hydrocarbons in solution produced polymers with proper experimentation
and documentation.
2.0 Principle of Method
2.1 A weighed sample of polymer is dissolved in chloroform and the
cement is coagulated with an isopropyl alcohol solution containing a
specific amount of alpha-methyl styrene (AMS) as the internal standard.
The extract of this coagulation is then injected into a gas
chromatograph and separated into individual components. Quantification
is achieved by the method of internal standardization.
3.0 Definitions
3.1 The definitions are included in the text as needed.
4.0 Interferences [Reserved]
5.0 Safety
5.1 This method may involve hazardous materials, operations, and
equipment. This method does not purport to address all of the safety
problems associated with its use. It is the responsibility of the user
of this method to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
6.0 Equipment and Supplies
6.1 Analytical balance, 160 g capacity, 0.1 mg resolution
[[Page 263]]
6.2 Bottles, 2-oz capacity with poly-cap screw lids
6.3 Mechanical shaker
6.4 Syringe, 10-ul capacity
6.5 Syringe, 2.5-ml capacity, with 22 gauge 1.25 inch needle, PP/PE
material, disposable
6.6 Gas chromatograph, Hewlett-Packard model 5890, or equivalent,
configured with FID, split injector packed with silanized glass wool.
6.6.1 Establish the following gas chromatographic conditions, and
allow the system to thoroughly equilibrate before use.
6.6.2 Injector parameters:
Injection technique=Split
Injector split flow=86 ml/min
Injector temperature=225 deg C
6.6.3 Oven temperature program:
Initial temperature=40 deg C
Initial time=6 min
Program rate=10 deg C/min
Upper limit temperature=175 deg C
Upper limit interval=10 min
6.6.4 Detector parameters:
Detector temperature=300 deg C
Hydrogen flow=30 ml/min
Air flow=350 ml/min
Nitrogen make up=26 ml/min
6.7 Gas chromatographic columns: SE-54 (5%-phenyl) (1%-vinyl)-
methylpolysiloxane, 15 Mx0.53 mm ID with a 1.2 micron film thickness,
and a Carbowax 20M (polyethylene glycol), 15 Mx0.53 mm ID with a 1.2
micron film thickness.
6.7.1 Column assembly: using a 0.53 mm ID butt connector union, join
the 15 Mx0.53 mm SE-54 column to the 15 Mx0.53 mm Carbowax 20M. The SE-
54 column will be inserted into the injector and the Carbowax 20M
inserted into the detector after they have been joined.
6.7.2 Column parameters:
Helium flow=2.8 ml/min
Helium headpressure=2 psig
6.8 Centrifuge
6.9 Data collection system, Hewlett-Packard Model 3396, or
equivalent
6.10 Pipet, 25-ml capacity, automatic dispensing, and 2 liter
reservoir
6.11 Pipet, 2-ml capacity, volumetric delivery, class A
6.12 Flasks, 100 and 1000-ml capacity, volumetric, class A
6.13 Vial, serum, 50-ml capacity, red rubber septa and crimp ring
seals
6.14 Sample collection basket fabricated out of wire mesh to allow
for drainage
7.0 Chemicals and Reagents
CHEMICALS:
7.1 alpha-Methyl Styrene, C9H10, 99+% purity, CAS 98-83-9
7.2 n-Hexane, C6H14, 99+% purity, CAS 110-54-3
7.3 Isopropyl alcohol, C3H8O 99.5+% purity, reagent grade, CAS 67-
63-0
7.4 Chloroform, CHCl3, 99% min., CAS 67-66-3
REAGENTS:
7.5 Internal Standard Stock Solution: 10 mg/25 ml AMS in isopropyl
alcohol.
7.5.1 Into a 25-ml beaker, weigh 0.4 g of AMS to the nearest 0.1 mg.
7.5.2 Quantitatively transfer this AMS into a 1-L volumetric flask.
Dilute to the mark with isopropyl alcohol.
7.5.3 Transfer this solution to the automatic dispensing pipet
reservoir. This will be labeled the AMS STOCK SOLUTION.
7.6 n-Hexane Stock Solution: 13mg/2ml hexane in isopropyl alcohol.
7.6.1 Into a 100-ml volumetric flask, weigh 0.65 g of n-hexane to
the nearest 0.1 mg.
7.6.2 Dilute to the mark with isopropyl alcohol. This solution will
be labeled the n-HEXANE STOCK SOLUTION.
8.0 Sample Collection, Preservation and Storage
8.1 A sampling device similar to Figure 1 is used to collect a non-
vented crumb rubber sample at a location that is after the stripping
operation but before the sample is exposed to the atmosphere.
8.2 The crumb rubber is allowed to cool before opening the sampling
device and removing the sample.
8.3 The sampling device is opened and the crumb rubber sample is
collected in the sampling basket.
8.4 One pound of crumb rubber sample is placed into a polyethylene
bag. The bag is labeled with the time, date and sample location.
8.5 The sample should be delivered to the laboratory for testing
within one hour of sampling.
8.6 Laboratory testing will be done within 3 hours of the sampling
time.
8.7 No special storage conditions are required unless the storage
time exceeds 3 hours in which case refrigeration of the samples is
recommended.
9.0 Quality Control
9.1 For each sample type, 12 samples shall be obtained from the
process for the recovery study. Half of the vials and caps shall be
tared, labeled ``spiked'', and numbered 1 through 6. The other vials
shall be labeled ``unspiked'' and need not be tared, but are also
numbered 1 through 6.
9.2 Determine the % moisture content of the crumb sample. After
determining the % moisture content, the correction factor for
calculating the dry crumb weight can be determined by using the equation
in section 12.2 of this method.
[[Page 264]]
9.3 Run the spiked and unspiked samples in the normal manner. Record
the concentrations of the n-hexane content of the mixed hexane reported
for each pair of spiked and unspiked samples.
9.4 For the recovery study, each sample of crumb shall be dissolved
in chloroform containing a known amount of mixed hexane solvent.
9.5 For each hydrocarbon, calculate the recovery efficiency (R)
using the following equations:
Mr=Ms-Mu
R=Mr/S
Where:
Mu=Measured amount of compound in the unspiked sample
Ms=Measured amount of compound in the spiked sample
Mr=Measured amount of the spiked compound
S=Amount of compound added to the spiked sample
R=Fraction of spiked compound recovered
9.6 Normally a value of R between 0.70 and 1.30 is acceptable.
9.7 R is used to correct all reported results for each compound by
dividing the measured results of each compound by the R for that
compound for the same sample type.
10.0 Calibration
10.1 Using the AMS STOCK SOLUTION equipped with the automatic
dispensing pipet (7.5.3 of this method), transfer 25.0 ml of the
internal standard solution into an uncapped 50-ml serum vial.
10.2 Using a 2.0 ml volumetric pipet, quantitatively transfer 2.0 ml
of the n-HEXANE STOCK SOLUTION (7.6.2 of this method) into the 50-ml
serum vial and cap. This solution will be labeled the CALIBRATION
SOLUTION.
10.3 Using the conditions prescribed (6.6 of this method), inject 1
[micro]l of the supernate.
10.4 Obtain the peak areas and calculate the response factor as
described in the calculations section (12.1 of this method).
11.0 Procedure
11.1 Determination of Dry Polymer Weight
11.1.1 Remove wet crumb from the polyethylene bag and place on paper
towels to absorb excess surface moisture.
11.1.2 Cut small slices or cubes from the center of the crumb sample
to improve sample uniformity and further eliminate surface moisture.
11.1.3 A suitable gravimetric measurement should be made on a sample
of this wet crumb to determine the correction factor needed to calculate
the dry polymer weight.
11.2 Determination of n-Hexane in Wet Crumb
11.2.1 Remove wet crumb from the polyethylene bag and place on paper
towels to absorb excess surface moisture.
11.2.2 Cut small slices or cubes from the center of the crumb sample
to improve sample uniformity and further eliminate surface moisture.
11.2.3 Into a tared 2 oz bottle, weigh 1.5 g of wet polymer to the
nearest 0.1 mg.
11.2.4 Add 25 ml of chloroform to the 2 oz bottle and cap.
11.2.5 Using a mechanical shaker, shake the bottle until the polymer
dissolves.
11.2.6 Using the autodispensing pipet, add 25.0 ml of the AMS STOCK
SOLUTION (7.5.3 of this method) to the dissolved polymer solution and
cap.
11.2.7 Using a mechanical shaker, shake the bottle for 10 minutes to
coagulate the dissolved polymer.
11.2.8 Centrifuge the sample for 3 minutes at 2000 rpm.
11.2.9 Using the conditions prescribed (6.6 of this method),
chromatograph 1 [micro]l of the supernate.
11.2.10 Obtain the peak areas and calculate the concentration of the
component of interest as described in the calculations (12.2 of this
method).
12.0 Calculations
12.1 Calibration:
RFx=(Wx x Ais) / (Wis x
Ax)
Where:
RFx=the relative response factor for n-hexane
Wx=the weight (g) of n-hexane in the CALIBRATION
SOLUTION
Ais=the area of AMS
Wis=the weight (g) of AMS in the CALIBRATION SOLUTION
Ax=the area of n-hexane
12.2 Procedure:
12.2.1 Correction Factor for calculating dry crumb weight.
F=1--(% moisture / 100)
Where:
F=Correction factor for calculating dry crumb weight
% moisture determined by appropriate method
12.2.2 Moisture adjustment for chromatographic determination.
Ws=F x Wc
Where:
Ws=the weight (g) of the dry polymer corrected for moisture
F=Correction factor for calculating dry crumb weight
Wc=the weight (g) of the wet crumb in section 9.6
12.2.3 Concentration (ppm) of hexane in the wet crumb.
[[Page 265]]
ppmx=(Ax * RFx * Wis *
10000) / (Ais * Ws)
Where:
ppmx=parts per million of n-hexane in the polymer
Ax=the area of n-hexane
RFx=the relative response factor for n-hexane
Wis=the weight (g) of AMS in the sample solution
Ais=the area of AMS
Ws=the weight (g) of the dry polymer corrected for moisture
13.0 Method Performance
13.1 Precision for the method was determined at the 0.08% level.
The standard deviation was 0.01 and the percent relative standard
deviation (RSD) was 16.3 % with five degrees of freedom.
14.0 Waste Generation
14.1 Waste generation should be minimized where possible.
15.0 Waste Management
15.1 Discard liquid chemical waste into the chemical waste drum.
15.2 Discard polymer waste into the polymer waste container.
16.0 References
16.1 This method is based on Goodyear Chemical Division Test Method
E-964.
Method 315--Determination of Particulate and Methylene Chloride
Extractable Matter (MCEM) From Selected Sources at Primary Aluminum
Production Facilities
Note: This method does not include all of the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical)
essential to its performance. Some material is incorporated by reference
from other methods in this part. Therefore, to obtain reliable results,
persons using this method should have a thorough knowledge of at least
the following additional test methods: Method 1, Method 2, Method 3, and
Method 5 of 40 CFR part 60, appendix A.
1.0 Scope and Application
1.1 Analytes. Particulate matter (PM). No CAS number assigned.
Methylene chloride extractable matter (MCEM). No CAS number assigned.
1.2 Applicability. This method is applicable for the simultaneous
determination of PM and MCEM when specified in an applicable regulation.
This method was developed by consensus with the Aluminum Association and
the U.S. Environmental Protection Agency (EPA) and has limited precision
estimates for MCEM; it should have similar precision to Method 5 for PM
in 40 CFR part 60, appendix A since the procedures are similar for PM.
1.3 Data quality objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.
2.0 Summary of Method
Particulate matter and MCEM are withdrawn isokinetically from the
source. PM is collected on a glass fiber filter maintained at a
temperature in the range of 120 14 [deg]C (248
25 [deg]F) or such other temperature as specified
by an applicable subpart of the standards or approved by the
Administrator for a particular application. The PM mass, which includes
any material that condenses on the probe and is subsequently removed in
an acetone rinse or on the filter at or above the filtration
temperature, is determined gravimetrically after removal of uncombined
water. MCEM is then determined by adding a methylene chloride rinse of
the probe and filter holder, extracting the condensable hydrocarbons
collected in the impinger water, adding an acetone rinse followed by a
methylene chloride rinse of the sampling train components after the
filter and before the silica gel impinger, and determining residue
gravimetrically after evaporating the solvents.
3.0 Definitions [Reserved]
4.0 Interferences [Reserved]
5.0 Safety
This method may involve hazardous materials, operations, and
equipment. This method does not purport to address all of the safety
problems associated with its use. It is the responsibility of the user
of this method to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to
performing this test method.
6.0 Equipment and Supplies
Note: Mention of trade names or specific products does not
constitute endorsement by the EPA.
6.1 Sample collection. The following items are required for sample
collection:
6.1.1 Sampling train. A schematic of the sampling train used in this
method is shown in Figure 5-1, Method 5, 40 CFR part 60, appendix A.
Complete construction details are given in APTD-0581 (Reference 2 in
section 17.0 of this method); commercial models of this train are also
available. For changes from APTD-0581 and for allowable modifications of
the train shown in Figure 5-1, Method 5, 40 CFR part 60, appendix A, see
the following subsections.
Note: The operating and maintenance procedures for the sampling
train are described in APTD-0576 (Reference 3 in section 17.0 of
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this method). Since correct usage is important in obtaining valid
results, all users should read APTD-0576 and adopt the operating and
maintenance procedures outlined in it, unless otherwise specified
herein. The use of grease for sealing sampling train components is not
recommended because many greases are soluble in methylene chloride. The
sampling train consists of the following components:
6.1.1.1 Probe nozzle. Glass or glass lined with sharp, tapered
leading edge. The angle of taper shall be <=30 [deg], and the taper
shall be on the outside to preserve a constant internal diameter. The
probe nozzle shall be of the button-hook or elbow design, unless
otherwise specified by the Administrator. Other materials of
construction may be used, subject to the approval of the Administrator.
A range of nozzle sizes suitable for isokinetic sampling should be
available. Typical nozzle sizes range from 0.32 to 1.27 cm (\1/8\ to \1/
2\ in.) inside diameter (ID) in increments of 0.16 cm (\1/16\ in.).
Larger nozzle sizes are also available if higher volume sampling trains
are used. Each nozzle shall be calibrated according to the procedures
outlined in section 10.0 of this method.
6.1.1.2 Probe liner. Borosilicate or quartz glass tubing with a
heating system capable of maintaining a probe gas temperature at the
exit end during sampling of 120 14 [deg]C
(248