[Title 40 CFR ]
[Code of Federal Regulations (annual edition) - July 1, 2001 Edition]
[From the U.S. Government Printing Office]
[[Page i]]
40
Parts 53 to 59
Revised as of July 1, 2001
Protection of Environment
Containing a codification of documents of general
applicability and future effect
As of July 1, 2001
With Ancillaries
Published by
Office of the Federal Register
National Archives and Records
Administration
A Special Edition of the Federal Register
[[Page ii]]
U.S. GOVERNMENT PRINTING OFFICE
WASHINGTON : 2001
For sale by the Superintendent of Documents, U.S. Government Printing
Office
Internet: bookstore.gpo.gov Phone: (202) 512-1800 Fax: (202) 512-
2250
Mail: Stop SSOP, Washington, DC 20402-0001
[[Page iii]]
Table of Contents
Page
Explanation................................................. v
Title 40:
Chapter I--Environmental Protection Agency 3
Finding Aids:
Material Approved for Incorporation by Reference........ 343
Table of CFR Titles and Chapters........................ 345
Alphabetical List of Agencies Appearing in the CFR...... 363
List of CFR Sections Affected........................... 373
[[Page iv]]
----------------------------
Cite this Code: CFR
To cite the regulations in
this volume use title,
part and section number.
Thus, 40 CFR 53.1 refers
to title 40, part 53,
section 1.
----------------------------
[[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
into 50 titles which represent broad areas subject to Federal
regulation. Each title is divided into chapters which usually bear the
name of the issuing agency. Each chapter is further subdivided into
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
volume.
LEGAL STATUS
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evidence of the text of the original documents (44 U.S.C. 1510).
HOW TO USE THE CODE OF FEDERAL REGULATIONS
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To determine whether a Code volume has been amended since its
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EFFECTIVE AND EXPIRATION DATES
Each volume of the Code contains amendments published in the Federal
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OMB CONTROL NUMBERS
The Paperwork Reduction Act of 1980 (Pub. L. 96-511) requires
Federal agencies to display an OMB control number with their information
collection request.
[[Page vi]]
Many agencies have begun publishing numerous OMB control numbers as
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OBSOLETE PROVISIONS
Provisions that become obsolete before the revision date stated on
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of provisions in effect on a given date in the past by using the
appropriate numerical list of sections affected. For the period before
January 1, 1986, consult either the List of CFR Sections Affected, 1949-
1963, 1964-1972, or 1973-1985, published in seven separate volumes. For
the period beginning January 1, 1986, a ``List of CFR Sections
Affected'' is published at the end of each CFR volume.
INCORPORATION BY REFERENCE
What is incorporation by reference? Incorporation by reference was
established by statute and allows Federal agencies to meet the
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This material, like any other properly issued regulation, has the force
of law.
What is a proper incorporation by reference? The Director of the
Federal Register will approve an incorporation by reference only when
the requirements of 1 CFR part 51 are met. Some of the elements on which
approval is based are:
(a) The incorporation will substantially reduce the volume of
material published in the Federal Register.
(b) The matter incorporated is in fact available to the extent
necessary to afford fairness and uniformity in the administrative
process.
(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
the material is not available, please notify the Director of the Federal
Register, National Archives and Records Administration, Washington DC
20408, or call (202) 523-4534.
CFR INDEXES AND TABULAR GUIDES
A subject index to the Code of Federal Regulations is contained in a
separate volume, revised annually as of January 1, entitled CFR Index
and Finding Aids. This volume contains the Parallel Table of Statutory
Authorities and Agency Rules (Table I). A list of CFR titles, chapters,
and parts and an alphabetical list of agencies publishing in the CFR are
also included in this volume.
An index to the text of ``Title 3--The President'' is carried within
that volume.
The Federal Register Index is issued monthly in cumulative form.
This index is based on a consolidation of the ``Contents'' entries in
the daily Federal Register.
A List of CFR Sections Affected (LSA) is published monthly, keyed to
the revision dates of the 50 CFR titles.
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REPUBLICATION OF MATERIAL
There are no restrictions on the republication of material appearing
in the Code of Federal Regulations.
INQUIRIES
For a legal interpretation or explanation of any regulation in this
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Raymond A. Mosley,
Director,
Office of the Federal Register.
July 1, 2001.
[[Page ix]]
THIS TITLE
Title 40--Protection of Environment is composed of twenty-eight
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 (63.600-1-63.1199), part 63 (63.1200-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, 2001.
Chapter I--Environmental Protection Agency appears in all twenty-
four volumes. A Pesticide Tolerance Commodity/Chemical Index and Crop
Grouping Commodities Index appear in parts 150-189. A Toxic Substances
Chemical--CAS Number Index appears in parts 700-789 and part 790 to End.
Redesignation Tables appear in the volumes containing parts 50-51, parts
150-189, and parts 700-789. 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.
[[Page x]]
[[Page 1]]
TITLE 40--PROTECTION OF ENVIRONMENT
(This book contains parts 53-59)
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Part
chapter i--Environmental Protection Agency (Continued)...... 53
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CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY
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Editorial Notes: 1. Subchapter C--Air Programs is contained in volumes
40 CFR parts 50-51, part 52.01-52.1018, part 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 (63.1200-End), parts 64-71,
parts 72-80, parts 81-85, part 86 (86.1-86.599-99), part 86 (86.600 to
end) and parts 87-99.
2. Nomenclature changes to chapter I appear at 65 FR 47324, 47325,
Aug. 2, 2000; 66 FR 34375, 34376, June 28, 2001.
SUBCHAPTER C--AIR PROGRAMS (CONTINUED)
Part Page
53 Ambient air monitoring reference and
equivalent methods...................... 5
54 Prior notice of citizen suits............... 104
55 Outer continental shelf air regulations..... 105
56 Regional consistency........................ 129
57 Primary nonferrous smelter orders........... 131
58 Ambient air quality surveillance............ 205
59 National volatile organic compound emission
standards for consumer and commercial
products................................ 291
[[Page 5]]
SUBCHAPTER C--AIR PROGRAMS--(Continued)
PART 53--AMBIENT AIR MONITORING REFERENCE AND EQUIVALENT METHODS--Table of Contents
Subpart A--General Provisions
Sec.
53.1 Definitions.
53.2 General requirements for a reference method determination.
53.3 General requirements for an equivalent method determination.
53.4 Applications for reference or equivalent method determinations.
53.5 Processing of applications.
53.6 Right to witness conduct of tests.
53.7 Testing of methods at the initiative of the Administrator.
53.8 Designation of reference and equivalent methods.
53.9 Conditions of designation.
53.10 Appeal from rejection of application.
53.11 Cancellation of reference or equivalent method designation.
53.12 Request for hearing on cancellation.
53.13 Hearings.
53.14 Modification of a reference or equivalent method.
53.15 Trade secrets and confidential or privileged information.
53.16 Supersession of reference methods.
Table A-1 to Subpart A--Summary of Applicable Requirements for Reference
Equivalent Methods for Air Monitoring of Criteria Pollutants
Appendix A to Subpart A--References
Subpart B--Procedures for Testing Performance Characteristics of
Automated Methods for SO2, CO, O3, and NO2
53.20 General provisions.
53.21 Test conditions.
53.22 Generation of test atmospheres.
53.23 Test procedures.
Appendix A to Subpart B--Optional Forms for Reporting Test Results
Subpart C--Procedures for Determining Comparability Between Candidate
Methods and Reference Methods
53.30 General provisions.
53.31 Test conditions.
53.32 Test procedures for methods for SO2, CO,
O3, and NO2.
53.33 Test procedure for methods for lead.
53.34 Test procedure for methods for PM10 and
PM2.5.
Table C-1 to Subpart C--Test Concentration Ranges, Number of
Measurements Required, and Maximum Discrepancy Specification
Table C-2 to Subpart C--Sequence of Test Measurements
Table C-3 to Subpart C--Test Specifications for Lead Methods
Table C-4 to Subpart C--Test Specifications for PM10 and
PM2.5 Methods
Figure C-1 to Subpart C--Suggested Format for Reporting Test Results
Appendix A to Subpart C--References
Subpart D--Procedures for Testing Performance Characteristics of Methods
for PM10
53.40 General provisions.
53.41 Test conditions.
53.42 Generation of test atmospheres for wind tunnel tests.
53.43 Test procedures.
Subpart E--Procedures for Testing Physical (Design) and Performance
Characteristics of Reference Methods and Class I Equivalent Methods for
PM2.5
53.50 General provisions.
53.51 Demonstration of compliance with design specifications and
manufacturing and test requirements.
53.52 Leak check test.
53.53 Test for flow rate accuracy, regulation, measurement accuracy,
and cut-off.
53.54 Test for proper sampler operation following power interruptions.
53.55 Test for effect of variations in power line voltage and ambient
temperature.
53.56 Test for effect of variations in ambient pressure.
53.57 Test for filter temperature control during sampling and post-
sampling periods.
53.58 Operational field precision and blank test.
53.59 Aerosol transport test for Class I equivalent method samplers.
Table E-1 to Subpart E--Summary of Test Requirements for Reference and
Class I Equivalent Methods for PM2.5
Table E-2 to Subpart E--Spectral Energy Distribution and Permitted
Tolerance for Conducting Radiative Tests
Figure E-1 to Subpart E--Designation Testing Checklist
Figure E-2 to Subpart E--Product Manufacturing Checklist
Appendix A to Subpart E--References
Subpart F--Procedures for Testing Performance Characteristics of Class
II Equivalent Methods for PM2.5
53.60 General provisions.
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53.61 Test conditions for PM2.5 reference method
equivalency.
53.62 Test procedure: Full wind tunnel test.
53.63 Test procedure: Wind tunnel inlet aspiration test.
53.64 Test procedure: Static fractionator test.
53.65 Test procedure: Loading test.
53.66 Test procedure: Volatility test.
Table F-1 to Subpart F--Performance Specifications for PM2.5
Class II Equivalent Samplers
Table F-2 to Subpart F--Particle Sizes and Wind Speeds for Full Wind
Tunnel Test, Wind Tunnel Inlet Aspiration Test, and Static
Chamber Test
Table F-3 to Subpart F--Critical Parameters of Idealized Ambient
Particle Size Distributions
Table F-4 to Subpart F--Estimated Mass Concentration Measurement of
PM2.5 for Idealized Coarse Aerosol Size
Distribution
Table F-5 to Subpart F--Estimated Mass Concentration Measurement of
PM2.5 for Idealized ``Typical'' Coarse Aerosol Size
Distribution
Table F-6 to Subpart F--Estimated Mass Concentration Measurement of
PM2.5 for Idealized Fine Aerosol Size Distribution
Figure E-1 to Subpart F--Designation Testing Checklist
Appendix A to Subpart F--References
Authority: Sec. 301(a) of the Clean Air Act (42 U.S.C. sec.
1857g(a)), as amended by sec. 15(c)(2) of Pub. L. 91-604, 84 Stat. 1713,
unless otherwise noted.
Source: 40 FR 7049, Feb. 18, 1975, unless otherwise noted.
Subpart A--General Provisions
Source: 62 FR 38784, July 18, 1997, unless otherwise noted.
Sec. 53.1 Definitions.
Terms used but not defined in this part shall have the meaning given
them by the Act.
Act means the Clean Air Act (42 U.S.C. 1857-1857l), as amended.
Administrator means the Administrator of the Environmental
Protection Agency or the Administrator's authorized representative.
Agency means the Environmental Protection Agency.
Applicant means a person or entity who submits an application for a
reference or equivalent method determination under Sec. 53.4, or a
person or entity who assumes the rights and obligations of an applicant
under Sec. 53.7. Applicant may include a manufacturer, distributor,
supplier, or vendor.
Automated method or analyzer means a method for measuring
concentrations of an ambient air pollutant in which sample collection
(if necessary), analysis, and measurement are performed automatically by
an instrument.
Candidate method means a method for measuring the concentration of
an air pollutant in the ambient air for which an application for a
reference method determination or an equivalent method determination is
submitted in accordance with Sec. 53.4, or a method tested at the
initiative of the Administrator in accordance with Sec. 53.7.
Class I equivalent method means an equivalent method for
PM2.5 which is based on a sampler that is very similar to the
sampler specified for reference methods in appendix L of this part, with
only minor deviations or modifications, as determined by EPA.
Class II equivalent method means an equivalent method for
PM2.5 that utilizes a PM2.5 sampler in which an
integrated PM2.5 sample is obtained from the atmosphere by
filtration and is subjected to a subsequent filter conditioning process
followed by a gravimetric mass determination, but which is not a Class I
equivalent method because of substantial deviations from the design
specifications of the sampler specified for reference methods in
appendix L of part 50 of this chapter, as determined by EPA.
Class III equivalent method means an equivalent method for
PM2.5 that has been determined by EPA not to be a Class I or
Class II equivalent method. This fourth type of PM2.5 method
includes alternative equivalent method samplers and continuous
analyzers, based on designs and measurement principles different from
those specified for reference methods (e.g., a means for estimating
aerosol mass concentration other than by conventional integrated
filtration followed by equilibration and gravimetric analysis. These
samplers (or monitors) are those deemed to be substantially different
from reference method samplers and
[[Page 7]]
are likely to use components and methods other than those specified for
reference method samplers.
Collocated describes two or more air samplers, analyzers, or other
instruments which sampler the ambient air that are operated
silmultaneously while located side by side, separated by a distance that
is large enough to preclude the air sampled by any of the devices from
being affected by any of the other devices, but small enough so that all
devices obtain identical or uniform ambient air samples that are equally
representative of the general area in which the group of devices is
located.
Equivalent method means a method for measuring the concentration of
an air pollutant in the ambient air that has been designated as an
equivalent method in accordance with this part; it does not include a
method for which an equivalent method designation has been canceled in
accordance with Sec. 53.11 or Sec. 53.16.
ISO 9001-registered facility means a manufacturing facility that is
either:
(1) An International Organization for Standardization (ISO) 9001-
registered manufacturing facility, registered to the ISO 9001 standard
(by the Registrar Accreditation Board (RAB) of the American Society for
Quality Control (ASQC) in the United States), with registration
maintained continuously.
(2) A facility that can be demonstrated, on the basis of information
submitted to the EPA, to be operated according to an EPA-approved and
periodically audited quality system which meets, to the extent
appropriate, the same general requirements as an ISO 9001-registered
facility for the design and manufacture of designated reference and
equivalent method samplers and monitors.
ISO-certified auditor means an auditor who is either certified by
the Registrar Accreditation Board (in the United States) as being
qualified to audit quality systems using the requirements of recognized
standards such as ISO 9001, or who, based on information submitted to
the EPA, meets the same general requirements as provided for ISO-
certified auditors.
Manual method means a method for measuring concentrations of an
ambient air pollutant in which sample collection, analysis, or
measurement, or some combination therof, is performed manually. A method
for PM10 or PM2.5 which utilizes a sampler that
requires manual preparation, loading, and weighing of filter samples is
considered a manual method even though the sampler may be capable of
automatically collecting a series of sequential samples.
PM2.5 sampler means a device, associated with a manual
method for measuring PM2.5, designed to collect
PM2.5 from an ambient air sample, but lacking the ability to
automatically analyze or measure the collected sample to determine the
mass concentrations of PM2.5 in the sampled air.
PM10 sampler means a device, associated with a manual
method for measuring PM10, designed to collect
PM10 from an ambient air sample, but lacking the ability to
automatically analyze or measure the collected sample to determine the
mass concentrations of PM10 in the sampled air.
Reference method means a method of sampling and analyzing the
ambient air for an air pollutant that is specified as a reference method
in an appendix to part 50 of this chapter, or a method that has been
designated as a reference method in accordance with this part; it does
not include a method for which a reference method designation has been
canceled in accordance with Sec. 53.11 or Sec. 53.16.
Sequential samples for PM samplers means two or more PM samples for
sequential (but not necessarily contiguous) time periods that are
collected automatically by the same sampler without the need for
intervening operator service.
Test analyzer means an analyzer subjected to testing as part of a
candidate method in accordance with subparts B, C, D, E, or F of this
part, as applicable. Test sampler means a PM10 sampler or a
PM2.5 sampler subjected to testing as part of a candidate
method in accordance with subparts C, D, E, or F of this part.
Ultimate purchaser means the first person or entity who purchases a
reference method or an equivalent method for purposes other than resale.
[[Page 8]]
Sec. 53.2 General requirements for a reference method determination.
The following general requirements for a reference method
determination are summarized in table A-1 of this subpart.
(a) Manual methods. (1) For measuring sulfur dioxide
(SO2) and lead, Appendices A and G of part 50 of this chapter
specify unique manual reference methods for those pollutants. Except as
provided in Sec. 53.16, other manual methods for SO2 and lead
will not be considered for reference method determinations under this
part.
(2) A reference method for measuring PM10 must be a
manual method that meets all requirements specified in appendix J of
part 50 of this chapter and must include a PM10 sampler that
has been shown in accordance with this part to meet all requirements
specified in subparts A and D of this part.
(3) A reference method for measuring PM2.5 must be a
manual method that meets all requirements specified in appendix L of
part 50 of this chapter and must include a PM2.5 sampler that
has been shown in accordance with this part to meet the applicable
requirements specified in subparts A and E of this part. Further,
reference method samplers must be manufactured in an ISO 9001-registered
facility, as defined in Sec. 53.1 and as set forth in Sec. 53.51, and
the Product Manufacturing Checklist set forth in subpart E of this part
must be completed by an ISO-certified auditor, as defined in Sec. 53.1,
and submitted to EPA annually to retain a PM2.5 reference
method designation.
(b) Automated methods. An automated reference method for measuring
carbon monoxide (CO), ozone (O3), and nitrogen dioxide
(NO2) must utilize the measurement principle and calibration
procedure specified in the appropriate appendix to part 50 of this
chapter and must have been shown in accordance with this part to meet
the requirements specified in subpart B of this part.
Sec. 53.3 General requirements for an equivalent method determination.
(a) Manual methods. A manual equivalent method must have been shown
in accordance with this part to satisfy the applicable requirements
specified in subpart C of this part. In addition, PM10 or
PM2.5 samplers associated with manual equivalent methods for
PM10 or PM2.5 must have been shown in accordance
with this part to satisfy the following additional requirements:
(1) A PM10 sampler associated with a manual method for
PM10 must satisfy the requirements of subpart D of this part.
(2) A PM2.5 Class I equivalent method sampler must
satisfy all requirements of subparts C and E of this part, which include
appropriate demonstration that each and every deviation or modification
from the reference method sampler specifications does not significantly
alter the performance of the sampler.
(3) A PM2.5 Class II equivalent method sampler must
satisfy the applicable requirements of subparts C, E, and F of this
part.
(4) Requirements for PM2.5 Class III equivalent method
samplers are not provided in this part because of the wide range of non-
filter-based measurement technologies that could be applied and the
likelihood that these requirements will have to be specifically adapted
for each such type of technology. Specific requirements will be
developed as needed and may include selected requirements from subparts
C, E, or F of this part or other requirements not contained in this
part.
(5) All designated equivalent methods for PM2.5 must be
manufactured in an ISO 9001-registered facility, as defined in Sec. 53.1
and as set forth in Sec. 53.51, and the Product Manufacturing Checklist
set forth in subpart E of this part must be completed by an ISO-
certified auditor, as defined in Sec. 53.1, and submitted to EPA
annually to retain a PM2.5 equivalent method designation.
(b) Automated methods. (1) Automated equivalent methods for
pollutants other than PM2.5 or PM10 must have been
shown in accordance with this part to satisfy the requirements specified
in subparts B and C of this part.
(2) Automated equivalent methods for PM10 must have been
shown in accordance with this part to satisfy the requirements of
subparts C and D of this part.
(3) Requirements for PM2.5 Class III automated equivalent
methods for
[[Page 9]]
PM2.5 are not provided in this part because of the wide range
of non-filter-based measurement technologies that could be applied and
the likelihood that these requirements will have to be specifically
adapted for each such type of technology. Specific requirements will be
developed as needed and may include selected requirements from subparts
C, E, or F of this part or other requirements not contained in this
part.
(4) All designated equivalent methods for PM2.5 must be
manufactured in an ISO 9001-registered facility, as set forth in subpart
E of this part, and the Product Manufacturing Checklist set forth in
subpart E of this part must be completed by an ISO-certified auditor and
submitted to EPA annually to retain a PM2.5 equivalent method
designation.
[62 FR 38784, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Sec. 53.4 Applications for reference or equivalent method determinations.
(a) Applications for reference or equivalent method determinations
shall be submitted in duplicate to: Director, National Exposure Research
Laboratory, Department E (MD-77B), U.S. Environmental Protection Agency,
Research Triangle Park, North Carolina 27711.
(b) Each application shall be signed by an authorized representative
of the applicant, shall be marked in accordance with Sec. 53.15 (if
applicable), and shall contain the following:
(1) A clear identification of the candidate method, which will
distinguish it from all other methods such that the method may be
referred to unambiguously. This identification must consist of a unique
series of descriptors such as title, identification number, analyte,
measurement principle, manufacturer, brand, model, etc., as necessary to
distinguish the method from all other methods or method variations, both
within and outside the applicant's organization.
(2) A detailed description of the candidate method, including but
not limited to the following: The measurement principle, manufacturer,
name, model number and other forms of identification, a list of the
significant components, schematic diagrams, design drawings, and a
detailed description of the apparatus and measurement procedures.
Drawings and descriptions pertaining to candidate methods or samplers
for PM2.5 must meet all applicable requirements in reference
1 of appendix A of this subpart, using appropriate graphical,
nomenclature, and mathematical conventions such as those specified in
references 3 and 4 of appendix A of this subpart.
(3) A copy of a comprehensive operation or instruction manual
providing a complete and detailed description of the operational,
maintenance, and calibration procedures prescribed for field use of the
candidate method and all instruments utilized as part of that method
(under Sec. 53.9(a)).
(i) As a minimum this manual shall include:
(A) Description of the method and associated instruments.
(B) Explanation of all indicators, information displays, and
controls.
(C) Complete setup and installation instructions, including any
additional materials or supplies required.
(D) Details of all initial or startup checks or acceptance tests and
any auxiliary equipment required.
(E) Complete operational instructions.
(F) Calibration procedures and required calibration equipment and
standards.
(G) Instructions for verification of correct or proper operation.
(H) Trouble-shooting guidance and suggested corrective actions for
abnormal operation.
(I) Required or recommended routine, periodic, and preventative
maintenance and maintenance schedules.
(J) Any calculations required to derive final concentration
measurements.
(K) Appropriate references to appendix L of part 50 of this chapter;
reference 6 of appendix A of this subpart; and any other pertinent
guidelines.
(ii) The manual shall also include adequate warning of potential
safety hazards that may result from normal use and/or malfunction of the
method and a description of necessary safety precautions. (See
Sec. 53.9(b).) However, the previous requirement shall not be
interpreted to constitute or imply any warranty of safety of the method
by
[[Page 10]]
EPA. For samplers and automated methods, the manual shall include a
clear description of all procedures pertaining to installation,
operation, preventive maintenance, and troubleshooting and shall also
include parts identification diagrams. The manual may be used to satisfy
the requirements of paragraphs (b)(1) and (b)(2) of this section to the
extent that it includes information necessary to meet those
requirements.
(4) A statement that the candidate method has been tested in
accordance with the procedures described in subparts B, C, D, E, and/or
F of this part, as applicable.
(5) Descriptions of test facilities and test configurations, test
data, records, calculations, and test results as specified in subparts
B, C, D, E, and/or F of this part, as applicable. Data must be
sufficiently detailed to meet appropriate principles described in
paragraphs 4 through 6 of reference 2 of appendix A of this subpart,
part b, sections 3.3.1 (paragraph 1) and 3.5.1 (paragraphs 2 and 3) and
in paragraphs 1 through 3 of reference 5 (section 4.8, Records) of
appendix A of this subpart. Salient requirements from these references
include the following:
(i) The applicant shall maintain and include records of all relevant
measuring equipment, including the make, type, and serial number or
other identification, and most recent calibration with identification of
the measurement standard or standards used and their National Institute
of Standards and Technology (NIST) traceability. These records shall
demonstrate the measurement capability of each item of measuring
equipment used for the application and include a description and
justification (if needed) of the measurement setup or configuration in
which it was used for the tests. The calibration results shall be
recorded and identified in sufficient detail so that the traceability of
all measurements can be determined and any measurement could be
reproduced under conditions close to the original conditions, if
necessary, to resolve any anomalies.
(ii) Test data shall be collected according to the standards of good
practice and by qualified personnel. Test anomalies or irregularities
shall be documented and explained or justified. The impact and
significance of the deviation on test results and conclusions shall be
determined. Data collected shall correspond directly to the specified
test requirement and be labeled and identified clearly so that results
can be verified and evaluated against the test requirement. Calculations
or data manipulations must be explained in detail so that they can be
verified.
(6) A statement that the method, analyzer, or sampler tested in
accordance with this part is representative of the candidate method
described in the application.
(c) For candidate automated methods and candidate manual methods for
PM10 and PM2.5, the application shall also contain
the following:
(1) A detailed description of the quality system that will be
utilized, if the candidate method is designated as a reference or
equivalent method, to ensure that all analyzers or samplers offered for
sale under that designation will have essentially the same performance
characteristics as the analyzer(s) or samplers tested in accordance with
this part. In addition, the quality system requirements for candidate
methods for PM2.5 must be described in sufficient detail,
based on the elements described in section 4 of reference 1 (Quality
System Requirements) of appendix A of this subpart. Further
clarification is provided in the following sections of reference 2 of
appendix A of this subpart: part A (Management Systems), sections 2.2
(Quality System and Description), 2.3 (Personnel Qualification and
Training), 2.4 (Procurement of Items and Services), 2.5 (Documents and
Records), and 2.7 (Planning); part B (Collection and Evaluation of
Environmental Data), sections 3.1 (Planning and Scoping), 3.2 (Design of
Data Collection Operations), and 3.5 (Assessment and Verification of
Data Usability); and part C (Operation of Environmental Technology),
sections 4.1 (Planning), 4.2 (Design of Systems), and 4.4 (Operation of
Systems).
(2) A description of the durability characteristics of such
analyzers or samplers (see Sec. 53.9(c)). For methods for
PM2.5, the warranty program must ensure that the required
specifications (see table A-1 of this subpart) will be
[[Page 11]]
met throughout the warranty period and that the applicant accepts
responsibility and liability for ensuring this conformance or for
resolving any nonconformities, including all necessary components of the
system, regardless of the original manufacturer. The warranty program
must be described in sufficient detail to meet appropriate provisions of
the ANSI/ASQC and ISO 9001 standards (references 1 and 2 in appendix A
of this subpart) for controlling conformance and resolving
nonconformance, particularly sections 4.12, 4.13, and 4.14 of reference
1 in appendix A of this subpart.
(i) Section 4.12 in appendix A of this subpart requires the
manufacturer to establish and maintain a system of procedures for
identifying and maintaining the identification of inspection and test
status throughout all phases of manufacturing to ensure that only
instruments that have passed the required inspections and tests are
released for sale.
(ii) Section 4.13 in appendix A of this subpart requires documented
procedures for control of nonconforming product, including review and
acceptable alternatives for disposition; section 4.14 in appendix A of
this subpart requires documented procedures for implementing corrective
(4.14.2) and preventive (4.14.3) action to eliminate the causes of
actual or potential nonconformities. In particular, section 4.14.3
requires that potential causes of nonconformities be eliminated by using
information such as service reports and customer complaints to eliminate
potential causes of nonconformities.
(d) For candidate reference or equivalent methods for
PM2.5, the applicant shall provide to EPA for test purposes
one sampler or analyzer that is representative of the sampler or
analyzer associated with the candidate method. The sampler or analyzer
shall be shipped FOB destination to Department E, (MD-77B), U.S. EPA, 79
T.W. Alexander Drive, Research Triangle Park, NC 27711, scheduled to
arrive concurrent with or within 30 days of the arrival of the other
application materials. This analyzer or sampler may be subjected to
various tests that EPA determines to be necessary or appropriate under
Sec. 53.5(f), and such tests may include special tests not described in
this part. If the instrument submitted under this paragraph
malfunctions, becomes inoperative, or fails to perform as represented in
the application before the necessary EPA testing is completed, the
applicant shall be afforded an opportunity to repair or replace the
device at no cost to EPA. Upon completion of EPA testing, the analyzer
or sampler submitted under this paragraph shall be repacked by EPA for
return shipment to the applicant, using the same packing materials used
for shipping the instrument to EPA unless alternative packing is
provided by the applicant. Arrangements for, and the cost of, return
shipment shall be the responsibility of the applicant. EPA does not
warrant or assume any liability for the condition of the analyzer or
sampler upon return to the applicant.
Sec. 53.5 Processing of applications.
After receiving an application for a reference or equivalent method
determination, the Administrator will publish notice of the application
in the Federal Register and, within 120 calendar days after receipt of
the application, take one or more of the following actions:
(a) Send notice to the applicant, in accordance with Sec. 53.8, that
the candidate method has been determined to be a reference or equivalent
method.
(b) Send notice to the applicant that the application has been
rejected, including a statement of reasons for rejection.
(c) Send notice to the applicant that additional information must be
submitted before a determination can be made and specify the additional
information that is needed (in such cases, the 120-day period shall
commence upon receipt of the additional information).
(d) Send notice to the applicant that additional test data must be
submitted and specify what tests are necessary and how the tests shall
be interpreted (in such cases, the 120-day period shall commence upon
receipt of the additional test data).
(e) Send notice to the applicant that the application has been found
to be
[[Page 12]]
substantially deficient or incomplete and cannot be processed until
additional information is submitted to complete the application and
specify the general areas of substantial deficiency.
(f) Send notice to the applicant that additional tests will be
conducted by the Administrator, specifying the nature of and reasons for
the additional tests and the estimated time required (in such cases, the
120-day period shall commence 1 calendar day after the additional tests
have been completed).
Sec. 53.6 Right to witness conduct of tests.
(a) Submission of an application for a reference or equivalent
method determination shall constitute consent for the Administrator or
the Administrator's authorized representative, upon presentation of
appropriate credentials, to witness or observe any tests required by
this part in connection with the application or in connection with any
modification or intended modification of the method by the applicant.
(b) The applicant shall have the right to witness or observe any
test conducted by the Administrator in connection with the application
or in connection with any modification or intended modification of the
method by the applicant.
(c) Any tests by either party that are to be witnessed or observed
by the other party shall be conducted at a time and place mutually
agreeable to both parties.
Sec. 53.7 Testing of methods at the initiative of the Administrator.
(a) In the absence of an application for a reference or equivalent
method determination, the Administrator may conduct the tests required
by this part for such a determination, may compile such other
information as may be necessary in the judgment of the Administrator to
make such a determination, and on the basis of the tests and information
may determine that a method satisfies applicable requirements of this
part.
(b) In the absence of an application requesting the Administrator to
consider revising an appendix to part 50 of this chapter in accordance
with Sec. 53.16, the Administrator may conduct such tests and compile
such information as may be necessary in the Administrator's judgment to
make a determination under Sec. 53.16(d) and on the basis of the tests
and information make such a determination.
(c) If a method tested in accordance with this section is designated
as a reference or equivalent method in accordance with Sec. 53.8 or is
specified or designated as a reference method in accordance with
Sec. 53.16, any person or entity who offers the method for sale as a
reference or equivalent method thereafter shall assume the rights and
obligations of an applicant for purposes of this part, with the
exception of those pertaining to submission and processing of
applications.
Sec. 53.8 Designation of reference and equivalent methods.
(a) A candidate method determined by the Administrator to satisfy
the applicable requirements of this part shall be designated as a
reference method or equivalent method (as applicable), and a notice of
the designation shall be submitted for publication in the Federal
Register not later than 15 days after the determination is made.
(b) A notice indicating that the method has been determined to be a
reference method or an equivalent method shall be sent to the applicant.
This notice shall constitute proof of the determination until a notice
of designation is published in accordance with paragraph (a) of this
section.
(c) The Administrator will maintain a current list of methods
designated as reference or equivalent methods in accordance with this
part and will send a copy of the list to any person or group upon
request. A copy of the list will be available for inspection or copying
at EPA Regional Offices.
Sec. 53.9 Conditions of designation.
Designation of a candidate method as a reference method or
equivalent method shall be conditioned to the applicant's compliance
with the following requirements. Failure to comply with any of the
requirements shall constitute a ground for cancellation of the
designation in accordance with Sec. 53.11.
[[Page 13]]
(a) Any method offered for sale as a reference or equivalent method
shall be accompanied by a copy of the manual referred to in
Sec. 53.4(b)(3) when delivered to any ultimate purchaser.
(b) Any method offered for sale as a reference or equivalent method
shall generate no unreasonable hazard to operators or to the environment
during normal use or when malfunctioning.
(c) Any analyzer, PM10 sampler, or PM2.5
sampler offered for sale as part of a reference or equivalent method
shall function within the limits of the performance specifications
referred to in Sec. 53.20(a), Sec. 53.30(a), Sec. 53.50, or Sec. 53.60,
as applicable, for at least 1 year after delivery and acceptance when
maintained and operated in accordance with the manual referred to in
Sec. 53.4(b)(3).
(d) Any analyzer, PM10 sampler, or PM2.5
sampler offered for sale as a reference or equivalent method shall bear
a prominent, permanently affixed label or sticker indicating that the
analyzer or sampler has been designated by EPA as a reference method or
as an equivalent method (as applicable) in accordance with this part and
displaying any designated method identification number that may be
assigned by EPA.
(e) If an analyzer is offered for sale as a reference or equivalent
method and has one or more selectable ranges, the label or sticker
required by paragraph (d) of this section shall be placed in close
proximity to the range selector and shall indicate clearly which range
or ranges have been designated as parts of the reference or equivalent
method.
(f) An applicant who offers analyzers, PM10 samplers, or
PM2.5 samplers for sale as reference or equivalent methods
shall maintain an accurate and current list of the names and mailing
addresses of all ultimate purchasers of such analyzers or samplers. For
a period of 7 years after publication of the reference or equivalent
method designation applicable to such an analyzer or sampler, the
applicant shall notify all ultimate purchasers of the analyzer or
PM2.5 or PM10 sampler within 30 days if the
designation has been canceled in accordance with Sec. 53.11 or
Sec. 53.16 or if adjustment of the analyzer or sampler is necessary
under Sec. 53.11(b).
(g) If an applicant modifies an analyzer, PM10 sampler,
or PM2.5 sampler that has been designated as a reference or
equivalent method, the applicant shall not sell the modified analyzer or
sampler as a reference or equivalent method nor attach a label or
sticker to the modified analyzer or sampler under paragraph (d) or (e)
of this section until the applicant has received notice under
Sec. 53.14(c) that the existing designation or a new designation will
apply to the modified analyzer, PM10 sampler, or
PM2.5 sampler or has applied for and received notice under
Sec. 53.8(b) of a new reference or equivalent method determination for
the modified analyzer or sampler.
(h) An applicant who has offered PM2.5 samplers or
analyzers for sale as part of a reference or equivalent method may
continue to do so only so long as the facility in which the samplers or
analyzers are manufactured continues to be an ISO 9001-registered
facility, as set forth in subpart E of this part. In the event that the
ISO 9001 registration for the facility is withdrawn, suspended, or
otherwise becomes inapplicable, either permanently or for some specified
time interval, such that the facility is no longer an ISO 9001-
registered facility, the applicant shall notify EPA within 30 days of
the date the facility becomes other than an ISO 9001-registered
facility, and upon such notification, EPA shall issue a preliminary
finding and notification of possible cancellation of the reference or
equivalent method designation under Sec. 53.11.
(i) An applicant who has offered PM2.5 samplers or
analyzers for sale as part of a reference or equivalent method may
continue to do so only so long as updates of the Product Manufacturing
Checklist set forth in subpart E of this part are submitted annually. In
the event that an annual Checklist update is not received by EPA within
12 months of the date of the last such submitted Checklist or Checklist
update, EPA shall notify the applicant within 30 days that the Checklist
update has not been received and shall, within 30 days from the issuance
of such notification, issue a preliminary finding and notification of
possible cancellation of the reference or equivalent method designation
under Sec. 53.11.
[[Page 14]]
Sec. 53.10 Appeal from rejection of application.
Any applicant whose application for a reference or equivalent method
determination has been rejected may appeal the Administrator's decision
by taking one or more of the following actions:
(a) The applicant may submit new or additional information in
support of the application.
(b) The applicant may request that the Administrator reconsider the
data and information already submitted.
(c) The applicant may request that any test conducted by the
Administrator that was a material factor in the decision to reject the
application be repeated.
Sec. 53.11 Cancellation of reference or equivalent method designation.
(a) Preliminary finding. If the Administrator makes a preliminary
finding on the basis of any available information that a representative
sample of a method designated as a reference or equivalent method and
offered for sale as such does not fully satisfy the requirements of this
part or that there is any violation of the requirements set forth in
Sec. 53.9, the Administrator may initiate proceedings to cancel the
designation in accordance with the following procedures.
(b) Notification and opportunity to demonstrate or achieve
compliance. (1) After making a preliminary finding in accordance with
paragraph (a) of this section, the Administrator will send notice of the
preliminary finding to the applicant, together with a statement of the
facts and reasons on which the preliminary finding is based, and will
publish notice of the preliminary finding in the Federal Register.
(2) The applicant will be afforded an opportunity to demonstrate or
to achieve compliance with the requirements of this part within 60 days
after publication of notice in accordance with paragraph (b)(1) of this
section or within such further period as the Administrator may allow, by
demonstrating to the satisfaction of the Administrator that the method
in question satisfies the requirements of this part, by commencing a
program to make any adjustments that are necessary to bring the method
into compliance, or by taking such action as may be necessary to cure
any violation of the requirements of Sec. 53.9. If adjustments are
necessary to bring the method into compliance, all such adjustments
shall be made within a reasonable time as determined by the
Administrator. If the applicant demonstrates or achieves compliance in
accordance with this paragraph (b)(2), the Administrator will publish
notice of such demonstration or achievement in the Federal Register.
(c) Request for hearing. Within 60 days after publication of a
notice in accordance with paragraph (b)(1) of this section, the
applicant or any interested person may request a hearing as provided in
Sec. 53.12.
(d) Notice of cancellation. If, at the end of the period referred to
in paragraph (b)(2) of this section, the Administrator determines that
the reference or equivalent method designation should be canceled, a
notice of cancellation will be published in the Federal Register and the
designation will be deleted from the list maintained under Sec. 53.8(c).
If a hearing has been requested and granted in accordance with
Sec. 53.12, action under this paragraph (d) will be taken only after
completion of proceedings (including any administrative review)
conducted in accordance with Sec. 53.13 and only if the decision of the
Administrator reached in such proceedings is that the designation in
question should be canceled.
Sec. 53.12 Request for hearing on cancellation.
Within 60 days after publication of a notice in accordance with
Sec. 53.11(b)(1), the applicant or any interested person may request a
hearing on the Administrator's action. If, after reviewing the request
and supporting data, the Administrator finds that the request raises a
substantial issue of fact, a hearing will be granted in accordance with
Sec. 53.13 with respect to such issue. The request shall be in writing,
signed by an authorized representative of the applicant or interested
person, and shall include a statement specifying:
(a) Any objections to the Administrator's action.
(b) Data or other information in support of such objections.
[[Page 15]]
Sec. 53.13 Hearings.
(a)(1) After granting a request for a hearing under Sec. 53.12, the
Administrator will designate a presiding officer for the hearing.
(2) If a time and place for the hearing have not been fixed by the
Administrator, the hearing will be held as soon as practicable at a time
and place fixed by the presiding officer, except that the hearing shall
in no case be held sooner than 30 days after publication of a notice of
hearing in the Federal Register.
(3) For purposes of the hearing, the parties shall include EPA, the
applicant or interested person(s) who requested the hearing, and any
person permitted to intervene in accordance with paragraph (c) of this
section.
(4) The Deputy General Counsel or the Deputy General Counsel's
representative will represent EPA in any hearing under this section.
(5) Each party other than EPA may be represented by counsel or by
any other duly authorized representative.
(b)(1) Upon appointment, the presiding officer will establish a
hearing file. The file shall contain copies of the notices issued by the
Administrator pursuant to Sec. 53.11(b)(1), together with any
accompanying material, the request for a hearing and supporting data
submitted therewith, the notice of hearing published in accordance with
paragraph (a)(2) of this section, and correspondence and other material
data relevant to the hearing.
(2) The hearing file shall be available for inspection by the
parties or their representatives at the office of the presiding officer,
except to the extent that it contains information identified in
accordance with Sec. 53.15.
(c) The presiding officer may permit any interested person to
intervene in the hearing upon such a showing of interest as the
presiding officer may require; provided that permission to intervene may
be denied in the interest of expediting the hearing where it appears
that the interests of the person seeking to intervene will be adequately
represented by another party (or by other parties), including EPA.
(d)(1) The presiding officer, upon the request of any party or at
the officer's discretion, may arrange for a prehearing conference at a
time and place specified by the officer to consider the following:
(i) Simplification of the issues.
(ii) Stipulations, admissions of fact, and the introduction of
documents.
(iii) Limitation of the number of expert witnesses.
(iv) Possibility of agreement on disposing of all or any of the
issues in dispute.
(v) Such other matters as may aid in the disposition of the hearing,
including such additional tests as may be agreed upon by the parties.
(2) The results of the conference shall be reduced to writing by the
presiding officer and made part of the record.
(e)(1) Hearings shall be conducted by the presiding officer in an
informal but orderly and expeditious manner. The parties may offer oral
or written evidence, subject to exclusion by the presiding officer of
irrelevant, immaterial, or repetitious evidence.
(2) Witnesses shall be placed under oath.
(3) Any witness may be examined or cross-examined by the presiding
officer, the parties, or their representatives. The presiding officer
may, at his/her discretion, limit cross-examination to relevant and
material issues.
(4) Hearings shall be reported verbatim. Copies of transcripts of
proceedings may be purchased from the reporter.
(5) All written statements, charts, tabulations, and data offered in
evidence at the hearing shall, upon a showing satisfactory to the
presiding officer of their authenticity, relevancy, and materiality, be
received in evidence and shall constitute part of the record.
(6) Oral argument shall be permitted. The presiding officer may
limit oral presentations to relevant and material issues and designate
the amount of time allowed for oral argument.
(f)(1) The presiding officer shall make an initial decision which
shall include written findings and conclusions and the reasons therefore
on all the material issues of fact, law, or discretion presented on the
record. The findings, conclusions, and written decision shall be
provided to the parties and made part of the record. The initial
decision
[[Page 16]]
shall become the decision of the Administrator without further
proceedings unless there is an appeal to, or review on motion of, the
Administrator within 30 calendar days after the initial decision is
filed.
(2) On appeal from or review of the initial decision, the
Administrator will have all the powers consistent with making the
initial decision, including the discretion to require or allow briefs,
oral argument, the taking of additional evidence or the remanding to the
presiding officer for additional proceedings. The decision by the
Administrator will include written findings and conclusions and the
reasons or basis therefore on all the material issues of fact, law, or
discretion presented on the appeal or considered in the review.
Sec. 53.14 Modification of a reference or equivalent method.
(a) An applicant who offers a method for sale as a reference or
equivalent method shall report to the EPA Administrator prior to
implementation any intended modification of the method, including but
not limited to modifications of design or construction or of operational
and maintenance procedures specified in the operation manual (see
Sec. 53.9(g)). The report shall be signed by an authorized
representative of the applicant, marked in accordance with Sec. 53.15
(if applicable), and addressed as specified in Sec. 53.4(a).
(b) A report submitted under paragraph (a) of this section shall
include:
(1) A description, in such detail as may be appropriate, of the
intended modification.
(2) A brief statement of the applicant's belief that the
modification will, will not, or may affect the performance
characteristics of the method.
(3) A brief statement of the probable effect if the applicant
believes the modification will or may affect the performance
characteristics of the method.
(4) Such further information, including test data, as may be
necessary to explain and support any statement required by paragraphs
(b)(2) and (b)(3) of this section.
(c) Within 30 calendar days after receiving a report under paragraph
(a) of this section, the Administrator will take one or more of the
following actions:
(1) Notify the applicant that the designation will continue to apply
to the method if the modification is implemented.
(2) Send notice to the applicant that a new designation will apply
to the method (as modified) if the modification is implemented, submit
notice of the determination for publication in the Federal Register, and
revise or supplement the list referred to in Sec. 53.8(c) to reflect the
determination.
(3) Send notice to the applicant that the designation will not apply
to the method (as modified) if the modification is implemented and
submit notice of the determination for publication in the Federal
Register.
(4) Send notice to the applicant that additional information must be
submitted before a determination can be made and specify the additional
information that is needed (in such cases, the 30-day period shall
commence upon receipt of the additional information).
(5) Send notice to the applicant that additional tests are necessary
and specify what tests are necessary and how they shall be interpreted
(in such cases, the 30-day period shall commence upon receipt of the
additional test data).
(6) Send notice to the applicant that additional tests will be
conducted by the Administrator and specify the reasons for and the
nature of the additional tests (in such cases, the 30-day period shall
commence 1 calendar day after the additional tests are completed).
(d) An applicant who has received a notice under paragraph (c)(3) of
this section may appeal the Administrator's action as follows:
(1) The applicant may submit new or additional information pertinent
to the intended modification.
(2) The applicant may request the Administrator to reconsider data
and information already submitted.
(3) The applicant may request that the Administrator repeat any test
conducted that was a material factor in the Administrator's
determination. A representative of the applicant may be present during
the performance of any such retest.
[[Page 17]]
Sec. 53.15 Trade secrets and confidential or privileged information.
Any information submitted under this part that is claimed to be a
trade secret or confidential or privileged information shall be marked
or otherwise clearly identified as such in the submittal. Information so
identified will be treated in accordance with part 2 of this chapter
(concerning public information).
Sec. 53.16 Supersession of reference methods.
(a) This section prescribes procedures and criteria applicable to
requests that the Administrator specify a new reference method, or a new
measurement principle and calibration procedure on which reference
methods shall be based, by revision of the appropriate appendix to part
50 of this chapter. Such action will ordinarily be taken only if the
Administrator determines that a candidate method or a variation thereof
is substantially superior to the existing reference method(s).
(b) In exercising discretion under this section, the Administrator
will consider:
(1) The benefits, in terms of the requirements and purposes of the
Act, that would result from specifying a new reference method or a new
measurement principle and calibration procedure.
(2) The potential economic consequences of such action for State and
local control agencies.
(3) Any disruption of State and local air quality monitoring
programs that might result from such action.
(c) An applicant who wishes the Administrator to consider revising
an appendix to part 50 of this chapter on the ground that the
applicant's candidate method is substantially superior to the existing
reference method(s) shall submit an application for a reference or
equivalent method determination in accordance with Sec. 53.4 and shall
indicate therein that such consideration is desired. The application
shall include, in addition to the information required by Sec. 53.4,
data and any other information supporting the applicant's claim that the
candidate method is substantially superior to the existing reference
method(s).
(d) After receiving an application under paragraph (c) of this
section, the Administrator will publish notice of its receipt in the
Federal Register and, within 120 calendar days after receipt of the
application, take one of the following actions:
(1) Determine that it is appropriate to propose a revision of the
appendix to part 50 of this chapter in question and send notice of the
determination to the applicant.
(2) Determine that it is inappropriate to propose a revision of the
appendix to part 50 of this chapter in question, determine whether the
candidate method is a reference or equivalent method, and send notice of
the determinations, including a statement of reasons for the
determination not to propose a revision, to the applicant.
(3) Send notice to the applicant that additional information must be
submitted before a determination can be made and specify the additional
information that is needed (in such cases, the 120-day period shall
commence upon receipt of the additional information).
(4) Send notice to the applicant that additional tests are
necessary, specifying what tests are necessary and how the test shall be
interpreted (in such cases, the 120-day period shall commence upon
receipt of the additional test data).
(5) Send notice to the applicant that additional tests will be
conducted by the Administrator, specifying the nature of and reasons for
the additional tests and the estimated time required (in such cases, the
120-day period shall commence 1 calendar day after the additional tests
have been completed).
(e)(1)(i) After making a determination under paragraph (d)(1) of
this section, the Administrator will publish a notice of proposed
rulemaking in the Federal Register. The notice of proposed rulemaking
will indicate that the Administrator proposes:
(A) To revise the appendix to part 50 of this chapter in question.
(B) Where the appendix specifies a measurement principle and
calibration procedure, to cancel reference method designations based on
the appendix.
[[Page 18]]
(C) To cancel equivalent method designations based on the existing
reference method(s).
(ii) The notice of proposed rulemaking will include the terms or
substance of the proposed revision, will indicate what period(s) of time
the Administrator proposes to allow for replacement of existing methods
under section 2.3 of appendix C to part 58 of this chapter, and will
solicit public comments on the proposal with particular reference to the
considerations set forth in paragraphs (a) and (b) of this section.
(2)(i) If, after consideration of comments received, the
Administrator determines that the appendix to part 50 in question should
be revised, the Administrator will, by publication in the Federal
Register:
(A) Promulgate the proposed revision, with such modifications as may
be appropriate in view of comments received.
(B) Where the appendix to part 50 (prior to revision) specifies a
measurement principle and calibration procedure, cancel reference method
designations based on the appendix.
(C) Cancel equivalent method designations based on the existing
reference method(s).
(D) Specify the period(s) that will be allowed for replacement of
existing methods under section 2.3 of appendix C to part 58 of this
chapter, with such modifications from the proposed period(s) as may be
appropriate in view of comments received.
(3) Canceled designations will be deleted from the list maintained
under Sec. 53.8(c). The requirements and procedures for cancellation set
forth in Sec. 53.11 shall be inapplicable to cancellation of reference
or equivalent method designations under this section.
(4) If the appendix to part 50 of this chapter in question is
revised to specify a new measurement principle and calibration procedure
on which the applicant's candidate method is based, the Administrator
will take appropriate action under Sec. 53.5 to determine whether the
candidate method is a reference method.
(5) Upon taking action under paragraph (e)(2) of this section, the
Administrator will send notice of the action to all applicants for whose
methods reference and equivalent method designations are canceled by
such action.
(f) An applicant who has received notice of a determination under
paragraph (d)(2) of this section may appeal the determination by taking
one or more of the following actions:
(1) The applicant may submit new or additional information in
support of the application.
(2) The applicant may request that the Administrator reconsider the
data and information already submitted.
(3) The applicant may request that any test conducted by the
Administrator that was a material factor in making the determination be
repeated.
Table A-1 to Subpart A--Summary of Applicable Requirements
for Reference and Equivalent Methods for Air Monitoring of
Criteria Pollutants
--------------------------------------------------------------------------------------------------------------------------------------------------------
Applicable Subparts of Part 53
Pollutant Ref. or Equivalent Manual or Automated Applicable Part -----------------------------------------------
50 Appendix A B C D E F
--------------------------------------------------------------------------------------------------------------------------------------------------------
SO2.................................. Reference.............. Manual................. A
Manual................. ....................... ......
Equivalent............. Automated.............. ............... > >
CO................................... Reference.............. Automated.............. C >
Manual................. ....................... ......
Equivalent............. Automated.............. ............... > >
O3................................... Reference.............. Automated.............. D >
Manual................. ....................... ......
Equivalent............. Automated.............. ............... > >
NO2.................................. Reference.............. Automated.............. F >
Manual................. ....................... ......
Equivalent............. Automated.............. ............... > >
Pb................................... Reference.............. Manual................. G
Equivalent............. Manual................. ............... >
PM10................................. Reference.............. Manual................. J >
Manual................. ....................... ...... >
Equivalent............. Automated.............. ............... > >
[[Page 19]]
PM2.5................................ Reference.............. Manual................. L >
Equivalent Class I..... Manual................. L > >
Equivalent Class II.... Manual................. L > > >
Equivalent Class III... Manual or Automated.... ............... > \1\ > \1\ > \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Note: Because of the wide variety of potential devices possible, the specific requirements applicable to a Class III candidate equivalent method for
PM2.5 are not specified explicitly in this part but, instead, shall be determined on a case-by-case basis for each such candidiate method.
Appendix A to Subpart A--References
(1) American National Standard Quality Systems-Model for Quality
Assurance in Design, Development, Production, Installation, and
Servicing, ANSI/ISO/ASQC Q9001-1994. Available from American Society for
Quality Control, 611 East Wisconsin Avenue, Milwaukee, WI 53202.
(2) American National Standard--Specifications and Guidelines for
Quality Systems for Environmental Data Collection and Environmental
Technology Programs, ANSI/ASQC E41994. Available from American Society
for Quality Control, 611 East Wisconsin Avenue, Milwaukee, WI 53202.
(3) Dimensioning and Tolerancing, ASME Y14.5M-1994. Available from
the American Society of Mechanical Engineers, 345 East 47th Street, New
York, NY 10017.
(4) Mathematical Definition of Dimensioning and Tolerancing
Principles, ASME Y14.5.1M-1994. Available from the American Society of
Mechanical Engineers, 345 East 47th Street, New York, NY 10017.
(5) ISO 10012, Quality Assurance Requirements for Measuring
Equipment-Part 1: Meteorological confirmation system for measuring
equipment):1992(E). Available from American Society for Quality Control,
611 East Wisconsin Avenue, Milwaukee, WI 53202.
(6) Copies of section 2.12 of the Quality Assurance Handbook for Air
Pollution Measurement Systems, Volume II, Ambient Air Specific Methods,
EPA/600/R-94/038b, are available from Department E (MD-77B), U.S. EPA,
Research Triangle Park, NC 27711.
Subpart B--Procedures for Testing Performance Characteristics of
Automated Methods SO2, CO, O3, and NO2
Sec. 53.20 General provisions.
(a) The test procedures given in this subpart shall be used to test
the performance of candidate automated methods against the performance
specifications given in table B-1. A test analyzer representative of the
candidate automated method must exhibit performance better than, or
equal to, the specified value for each such specification (except Range)
to satisfy the requirements of this subpart. Except as provided in
paragraph (b) of this section, the range of the candidate method must be
the range specified in table B-1 to satisfy the requirements of this
subpart.
(b) For a candidate method having more than one selectable range,
one range must be that specified in table B-1 and a test analyzer
representative of the method must pass the tests required by this
subpart while operated in that range. The tests may be repeated for a
broader range (i.e., one extending to higher concentrations) than that
specified in table B-1 provided that the range does not extend to
concentrations more than two times the upper range limit specified in
table B-1. If the application is for a reference method determination,
the tests may be repeated for a narrower range (one extending to lower
concentrations) than that specified in table B-1.
If the tests are conducted or passed only for the specified range, any
reference or equivalent method determination with respect to the method
will be limited to that range. If the tests are passed for both the
specified range and a broader range (or ranges), any such determination
will include the broader range(s) as well as the specified range,
provided that the tests required by subpart C of this part (if
applicable) are met for the broader range(s). If the tests are passed
for both the specified range and a narrower range, a reference method
determination for the method will include the narrower range as well as
the specified range. Appropriate test data shall be submitted for each
range sought to be included in a reference or equivalent
[[Page 20]]
method determination under this paragraph (b).
(c) For each performance specification (except Range), the test
procedure shall be initially repeated seven (7) times to yield 7 test
results. Each result shall be compared with the corresponding
specification in table B-1; a value higher than or outside that
specified constitutes a failure. These 7 results for each parameter
shall be interpreted as follows:
(1) Zero (0) failures: Candidate method passes the performance
parameter.
(2) Three (3) or more failures: Candidate method fails the
performance parameter.
(3) One (1) or two (2) failures: Repeat the test procedures for the
parameter eight (8) additional times yielding a total of fifteen (15)
test results. The combined total of 15 test results shall then be
interpreted as follows:
(i) One (1) or two (2) failures: Candidate method passes the
performance parameter.
(ii) Three (3) or more failures: Candidate method fails the
performance parameter.
Table B-1--Performance Specifications for Automated Methods
----------------------------------------------------------------------------------------------------------------
Sulfur Photochemical Carbon Nitrogen Definitions and
Performance parameter Units \1\ dioxide oxidants monoxide dioxide test procedures
----------------------------------------------------------------------------------------------------------------
1. Range..................... Parts per 0-0.5 0-0.5 0-50 0-0.5 Sec. 53.23(a).
million.
2. Noise..................... ......do........ .005 .005 .50 .005 Sec. 53.23(b).
3. Lower detectable limit.... Parts per .01 .01 1.0 .01 Sec. 53.23(c).
million.
4. Interference equivalent... ................ ......... ............. ......... ......... Sec. 53.23(d).
Each interferant........... Parts per plus-minu plus-minus.02 plus-minu plus-minu
million. s.02 s1.0 s0.02
Total interferant.......... ......do........ .06 .06 1.5 .04
5. Zero drift, 12 and 24 hour ......do........ plus-minu plus-minus.02 plus-minu plus-minu Sec. 52.23(e).
s.02 s1.0 s.02
6. Span drift, 24 hour....... ................ ......... ............. ......... ......... Do.
20 percent of upper range Percent......... plus-minu plus-minus20. plus-minu plus-minu
limit. s20.0 0 s10.0 s20.0
80 percent of upper range ......do........ plus-minu plus-minus5.0 plus-minu plus-minu
limit. s5.0 s2.5 s5.0
7. Lag time.................. Minutes......... 20 20 10 20 Do.
8. Rise time................. ......do........ 15 15 5 15 Do.
9. Fall time................. ......do........ 15 15 5 15 Do.
10. Precision................ ................ ......... ............. ......... ......... Do.
20 percent of upper range Parts per .01 .01 .5 .02
limit. million.
80 percent of upper range ......do........ .015 .01 .5 .03
limit.
----------------------------------------------------------------------------------------------------------------
\1\ To convert from parts per million to g/m \3\ at 25 deg.C and 760 mm Hg, multiply by M/0.02447,
where M is the molecular weight of the gas.
(d) The tests for zero drift, span drift, lag time, rise time, fall
time, and precision shall be combined into a single sequential procedure
to be conducted at various line voltages and ambient temperatures
specified in Sec. 53.23(e). The tests for noise, lower detectable limit,
and interference equivalents shall be made at any temperature between 20
deg.C. and 30 deg.C. and at any normal line voltage between 105 and
125 volts, and shall be conducted such that not more than three (3) test
results for each parameter are obtained per 24 hours.
(e) All response readings to be recorded shall first be converted to
concentration units according to the calibration curve constructed in
accordance with Sec. 53.21(b).
(f) All recorder chart tracings, records, test data and other
documentation obtained from or pertinent to these tests shall be
identified, dated, signed by the analyst performing the test, and
submitted.
Note: Suggested formats for reporting the test results and
calculations are provided in Figures B-2, B-3, B-4, B-5, and B-6 in
appendix A. Symbols and abbreviations used in this subpart are listed in
table B-5, appendix A.
[40 FR 7049, Feb. 18, 1975, as amended at 40 FR 18168, Apr. 25, 1975; 41
FR 52694, Dec. 1, 1976]
Sec. 53.21 Test conditions.
(a) Set-up and start-up of the test analyzer shall be in strict
accordance with the operating instructions specified in the manual
referred to in Sec. 53.4(b)(3). Allow adequate warm-up or stabilization
time as indicated in the operating instructions before beginning the
tests. If the candidate method does not include an integral strip chart
recorder,
[[Page 21]]
connect the output signal of the test analyzer to a suitable strip chart
recorder of the servo, null-balance type. This recorder shall have a
chart width of at least 25 centimeters, chart speeds up to 10 cm per
hour, a response time of 1 second or less, a deadband of not more than
0.25 percent of full scale, and capability either of reading
measurements at least 5 percent below zero or of offsetting the zero by
at least 5 percent.
Note: Other data acquisition components may be used along with the
chart recorder during conduct of these tests. Use of the chart recorder
is intended only to facilitate evaluation of data submitted.
(b) Calibration of the test analyzer shall be as indicated in the
manual referred to in Sec. 53.4(b)(3) and as follows: If the chart
recorder does not have below zero capability, adjust either the controls
of the test analyzer or the chart recorder to obtain a +5% offset zero
reading on the recorder chart to facilitate observing negative response
or drift. If the candidate method is not capable of negative response,
the test analyzer (not recorder) shall be operated with an offset zero.
Construct and submit a calibration curve showing a plot of recorder
scale readings (ordinate) against pollutant concentrations (abscissa). A
plot of output units (volts, millivolts, milliamps, etc.) against
pollutant concentrations shall also be shown for methods not including
an integral chart recorder. All such plots shall consist of at least
seven (7) approximately equally spaced, identifiable points, including 0
and 90plus-minus5 percent of full scale.
(c) Once the test analyzer has been set up and calibrated and the
tests started, manual adjustment or normal periodic maintenance is
permitted only every 3 days. Automatic adjustments which the test
analyzer performs by itself are permitted at any time. The submitted
records shall show clearly when any manual adjustment or periodic
maintenance was made and describe the operations performed.
(d) If the test analyzer should malfunction during any of the
performance tests, the tests for that parameter shall be repeated. A
detailed explanation of the malfunction, remedial action taken, and
whether recalibration was necessary (along with all pertinent records
and charts) shall be submitted. If more than one malfunction occurs, all
performance test procedures for all parameters shall be repeated.
(e) Tests for all performance parameters shall be completed on the
same test analyzer, except that use of multiple test analyzers to
accelerate testing will be permitted when alternate ranges of a multi-
range candidate method are being tested.
Sec. 53.22 Generation of test atmospheres.
(a) Table B-2 specifies preferred methods for generating test
atmospheres and suggested methods of verifying the concentrations. Only
one means of establishing the concentration of a test atmosphere is
normally required. If the method of generation can produce reproducible
concentrations, verification is optional. If the method of generation is
not reproducible, then establishment of the concentration by some
verification method is required. However, when a method of generation
other than that given in table B-2 is used, the test concentration shall
be verified.
(b) The test atmosphere delivery system shall be designed and
constructed so as not to significantly alter the test atmosphere
composition or concentration during the period of the test. The delivery
system shall be fabricated from borosilicate glass or FEP Teflon.
(c) The output of the test atmosphere generation system shall be
sufficiently stable to obtain stable response during the required tests.
If a permeation device is used for generation of a test atmosphere, the
device, as well as the air passing over it, shall be controlled to
plus-minus0.1 deg.C.
(d) All diluent air shall be zero air free of contaminants likely to
cause a detectable response on the test analyzer.
[[Page 22]]
Table B-2--Test Atmospheres
----------------------------------------------------------------------------------------------------------------
Test gas Generation Verification
----------------------------------------------------------------------------------------------------------------
Ammonia............................... Permeation device. Similar to Indophenol method, reference 3.
system described in references 1
and 2.
Carbon dioxide........................ Cylinder of zero air or nitrogen Use NBS-certified standards whenever
containing CO2 as required to possible. If NBS standards are not
obtain the concentration available, obtain 2 standards from
specified in table B-3. independent sources which agree
within 2 percent; or obtain one
standard and submit it to an
independent laboratory for analysis
which must agree within 2 percent of
the supplier's nominal analysis.
Carbon monoxide....................... Cylinder of zero air or nitrogen Do.
containing CO as required to
obtain the concentration
specified in table B-3.
Ethane................................ Cylinder of zero air or nitrogen Do.
containing ethane as required to
obtain the concentration
specified in table B-3.
Ethylene.............................. Cylinder of prepurified nitrogen Do.
containing ethylene as required
to obtain the concentration
specified in table B-3.
Hydrogen chloride..................... Cylinder \1\ of prepurified Collect samples in bubbler containing
nitrogen containing distilled water and analyze by the
approximately 100 p/m of gaseous mercuric thiocyanate method, ASTM
HCl. Dilute with zero air to (D512), p. 29, reference 4.
concentration specified in table
B-3.
Hydrogen sulfide...................... Permeation device system Tentative method of analysis for H 2
described in references 1 and 2. S content of the atmosphere, p. 426,
reference 5.
Methane............................... Cylinder of zero air containing Use NBS-certified standards whenever
methane as required to obtain possible. If NBS standards are not
the concentration specified in available, obtain 2 standards from
table B-3. independent sources which agree
within 2 percent; or obtain one
standard and submit it to an
independent laboratory for an
analysis which must agree within 2
percent of the supplier's nominal
analysis.
Nitric oxide.......................... Cylinder \1\ of prepurified Gas-phase titration as described in
nitrogen containing reference 6, section 7.1.
approximately 100 p/m NO. Dilute
with zero air to required
concentration.
Nitrogen dioxide...................... 1. Gas phase titration as 1. Use an NO 2 analyzer calibrated
described in reference 6. with a gravimetrically calibrated
2. Permeation device, similar to permeation device.
system described in references 1 2. Use an NO 2 analyzer calibrated by
and 2. gas-phase titration as described in
reference 6.
Ozone................................. Calibrated ozone generator as Use an ozone analyzer calibrated by
described in reference 7, gas-phase titration as described in
appendix D. reference 6.
Sulfur dioxide........................ Permeation device Similar to P-rosaniline method. Reference 7,
system described in reference appendix A.
method for SO2, reference 7,
appendix A.
Water................................. Pass zero air through distilled Measure relative humidity by means of
water at a fixed known a dew-point indicator, calibrated
temperature between 20 deg. and electrolytic or piezo electric
30 deg.C. such that the air hygrometer, or wet/dry bulb
stream becomes saturated. Dilute thermometer.
with zero air to concentration
specified in table B-3.
Xylene................................ Cylinder of prepurified nitrogen Use NBS-certified standards whenever
containing 100 p/m xylene. possible. If NBS standards are not
Dilute with zero air to available, obtain 2 standards from
concentration specified in table independent sources which agree
B-3. within 2 percent; or obtain one
standard and submit it to an
independent laboratory for an
analysis which must agree within 2
percent of the supplier's nominal
analysis.
Zero air.............................. 1. Ambient air purified by
appropriate scrubbers or other
devices such that it is free of
contaminants likely to cause a
detectable response on the
analyzer.
2. Cylinder of compressed zero
air certified by the supplier or
an independent laboratory to be
free of contaminants likely to
cause a detectable response on
the analyzer.
----------------------------------------------------------------------------------------------------------------
\1\ Use stainless steel pressure regulator dedicated to the pollutant measured.
Reference 1. O'Keeffe, A. E., and Ortaman, G. C. ``Primary Standards for Trace Gas Analysis,'' Anal. Chem. 38,
760 (1966).
Reference 2. Scaringelli, F. P., A. E., Rosenberg, E., and Bell, J. P., ``Primary Standards for Trace Gas
Analysis.'' Anal. Chem. 42, 871 (1970).
Reference 3. ``Tentative Method of Analysis for Ammonia in the Atmosphere (Indophenol Method)'', Health Lab
Sciences, vol. 10, No. 2, 115-118, April 1973.
Reference 4. 1973 Annual Book of ASTM Standards, American Society for Testing and Materials, 1916 Race St.,
Philadelphia, PA.
Reference 5. Methods for Air Sampling and Analysis, Intersociety Committee, 1972, American Public Health
Association, 1015.
Reference 6. Federal Register, vol. 38, No. 110, Tentative Method for the Continuous Measurement of Nitrogen
Dioxide (Chemiluminescent) addenda C. (June 8, 1973).
Reference 7. Federal Register, vol. 36, No. 228, National Primary and Secondary Ambient Air Quality Standards,
Nov. 25, 1971.
[[Page 23]]
(e) The concentration of each test atmosphere shall be established
and/or verified before or during each series of tests. Samples for
verifying test concentrations shall be collected from the test
atmosphere delivery system as close as possible to the sample intake
port of the test analyzer.
(f) The accuracy of all flow measurements used to calculate test
atmosphere concentrations shall be documented and referenced to a
primary standard (such as a spirometer, bubble meter, etc.). Any
corrections shall be clearly shown. All flow measurements given in
volume units shall be standardized to 25 deg.C. and 760 mm Hg.
(g) Schematic drawings and other information showing complete
procedural details of the test atmosphere generation, verification, and
delivery system shall be provided. All pertinent calculations shall be
clearly indicated.
[40 FR 7049, Feb. 18, 1975, as amended at 40 FR 18168, Apr. 25, 1975]
Sec. 53.23 Test procedures.
(a) Range--(1) Technical definition. Nominal minimum and maximum
concentrations which a method is capable of measuring.
Note: The nominal range is specified at the lower and upper range
limits in concentration units, for example, 0-0.5 p/m.
(2) Test procedure. Submit a suitable calibration curve, as
specified in Sec. 53.21(b), showing the test analyzer's response over at
least 95 percent of the required range.
Note: A single calibration curve will normally suffice.
(b) Noise--(1) Technical definition. Spontaneous, short duration
deviations in output, about the mean output, which are not caused by
input concentration changes. Noise is determined as the standard
deviation about the mean and is expressed in concentration units.
(2) Test procedure. (i) Allow sufficient time for the test analyzer
to warm up and stabilize. Determine at two concentrations, first using
zero air and then a pollutant test gas concentration as indicated below.
The noise specification in table B-1 shall apply to both of these tests.
(ii) Connect an integrating-type digital meter (DM) suitable for the
test analyzer's output and accurate to three significant digits, to
measure the analyzer's output signal.
Note: Use of a chart recorder in addition to the DM is optional.
(iii) Measure zero air for 60 minutes. During this 60-minute
interval, record twenty-five (25) readings at 2-minute intervals. (See
Figure B-2 in appendix A.)
(iv) Convert each DM reading to concentration units (p/m) by
reference to the test analyzer's calibration curve as determined in
Sec. 53.21(b). Label the converted DM readings r1,
r2, r3 . . . ri . . . r25.
(v) Calculate the standard deviation, S, as follows:
where i indicates the i-th DM reading in ppm.
(vi) Let S at 0 ppm be identified as So; compare So
to the noise specification given in table B-1.
(vii) Repeat steps (iii) through (vi) of this section using a
pollutant test atmosphere concentration of 80plus-minus5
percent of the upper range limit (URL) instead of zero gas, and let S at
80 percent of the URL be identified as S80. Compare S80
to the noise specification given in table B-1.
(viii) Both S0 and S80 must be less than or
equal to the specification for noise to pass the test for the noise
parameter.
(c) Lower detectable limit--(1) Technical definition. The minimum
pollutant concentration which produces a signal of twice the noise
level.
(2) Test procedure. (i) Allow sufficient time for the test analyzer
to warm up and stabilize. Measure zero air and record the stable reading
in ppm as BZ. (See Figure B-3 in appendix A.)
(ii) Generate and measure a pollutant test atmosphere concentration
equal to the value for the lower detectable limit specified in table B-
1.
Note: If necessary, the test atmosphere concentration may be
generated or verified at a higher concentration, then accurately diluted
with zero air to the final required concentration.
[[Page 24]]
(iii) Record the test analyzer's stable indicated reading, in ppm,
as BL.
(iv) Determine the Lower Detectable Limit (LDL) as LDL =
BL-BZ. Compare this LDL value with the noise
level, S0, determined in Sec. 53.23(b), for 0 concentration
test atmosphere. LDL must be equal to or higher than 2S0 to
pass this test.
(d) Interference equivalent--(1) Technical definition. Positive or
negative response caused by a substance other than the one being
measured.
(2) Test procedure. The test analyzer shall be tested for all
substances likely to cause a detectable response. The test analyzer
shall be challenged, in turn, with each interfering agent specified in
table B-3. In the event that there are substances likely to cause a
significant interference which have not been specified in table B-3,
these substances shall be tested at a concentration substantially higher
than that normally found in the ambient air. The interference may be
either positive or negative, depending on whether the test analyzer's
response is increased or decreased by the presence of the interferent.
Interference equivalents shall be determined by mixing each interferent,
one at a time, with the pollutant at the concentrations specified in
table B-3, and comparing the test analyzer's response to the response
caused by the pollutant alone. Known gas-phase reactions that might
occur between an interferent and the pollutant are designated by
footnote 3 in table B-3. In these cases, the interference equivalent
shall be determined in the absence of the pollutant.
(i) Allow sufficient time for warm-up and stabilization of the test
analyzer.
(ii) For a candidate method using a prefilter or scrubber based upon
a chemical reaction to derive part of its specificity, and which
requires periodic service or maintenance, the test analyzer shall be
``conditioned'' prior to each interference test as follows:
[[Page 25]]
Table B-3--Interferant Test Concentration,\1\ Parts Per Million
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Hydrochloric Hydrogen Sulfur Nitrogen Nitric Carbon M- Water Carbon
Pollutant Analyzer type \2\ acid Ammonia sulfide dioxide dioxide oxide dioxide Ethylene Ozone xylene vapor monoxide Methane Ethane
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
SO2..................... Flame photometric (FPD)..... ............ ....... 0.1 \1\ 0.14 ........ ....... 750 ........ ....... ....... \3\ 20,0 50 ....... .......
00
SO2..................... Gas chromatography (FPD).... ............ ....... .1 \4\.14 ........ ....... 750 ........ ....... ....... \3\ 20,0 50 ....... .......
00
SO2..................... Spectrophotometric-wet 0.2 \3\ 0.1 .1 \4\.14 0.5 ....... 750 ........ 0.5 ....... ........ ........ ....... .......
chemical (pararosaniline
reaction).
SO2..................... Electrochemical............. .2 \3\.1 .1 \4\.14 .5 0.5 ........ 0.2 .5 ....... \3\ 20,0 ........ ....... .......
00
SO2..................... Conductivity................ .2 \3\.1 ........ \4\.14 .5 ....... 750 ........ ....... ....... ........ ........ ....... .......
SO2..................... Spectrophotometric-gas phase ............ ....... ........ \4\.14 .5 .5 ........ ........ .5 0.2 ........ ........ ....... .......
O3...................... Chemiluminescent............ ............ ....... \3\.1 ........ ........ ....... 750 ........ \4\.08 ....... \3\ 20,0 ........ ....... .......
00
O3...................... Electrochemical............. ............ \3\.1 ........ .5 .5 ....... ........ ........ \4\.08 ....... \3\ 20,0 ........ ....... .......
00
O3...................... Spectrophotometric-wet ............ \3\.1 ........ .5 .5 \3\.5 ........ ........ \4\.08 ....... ........ ........ ....... .......
chemical (potassium iodide
reaction).
O3...................... Spectrophotometric-gas phase ............ ....... ........ .5 .5 \3\.5 ........ ........ \4\.08 ....... ........ ........ ....... .......
CO...................... Infrared.................... ............ ....... ........ ........ ........ ....... 750 ........ ....... ....... 20,000 \4\ 10 ....... .......
CO...................... Gas chromatography with ............ ....... ........ ........ ........ ....... ........ ........ ....... ....... 20,000 \4\ 10 ....... 0.5
flame ionization detector.
CO...................... Electrochemical............. ............ ....... ........ ........ ........ .5 ........ .2 ....... ....... 20,000 \4\ 10 ....... .......
CO...................... Catalytic combustion-thermal ............ .1 ........ ........ ........ ....... 750 .2 ....... ....... 20,000 \4\ 10 5.0 .5
detection.
CO...................... IR fluorescence............. ............ ....... ........ ........ ........ ....... 750 ........ ....... ....... 20,000 \4\ 10 ....... .5
CO...................... Mercury replacement UV ............ ....... ........ ........ ........ ....... ........ .2 ....... ....... ........ \4\ 10 ....... .5
photometric.
NO2..................... Chemiluminescent............ ............ \3\.1 ........ .5 \4\.1 .5 ........ ........ ....... ....... 20,000 ........ ....... .......
NO2..................... Spectrophotometric-wet ............ ....... ........ .5 \4\.1 .5 750 ........ .5 ....... ........ ........ ....... .......
chemical (azo-dye reaction).
NO2..................... Electrochemical............. 0.2 \3\.1 ........ .5 \4\.1 .5 750 ........ .5 ....... 20,000 50 ....... .......
NO2..................... Spectrophotometric-gas phase ............ \3\.1 ........ .5 \4\.1 .5 ........ ........ .5 ....... 20,000 50 ....... .......
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Concentrations of interferant listed must be prepared and controlled to plus-minus 10 percent of the state value.
\2\ Analyzer types not listed will be considered by the administrator as special cases.
\3\ Do not mix with pollutant.
\4\ Concentration of pollutant used for test. These pollutant concentrations must be prepared to plus-minus 10 percent of the stated value.
[[Page 26]]
(A) Service or perform the indicated maintenance on the scrubber or
prefilter as directed in the manual referred to in Sec. 53.4(b)(3).
(B) Before testing for each interferent, allow the test analyzer to
sample through the scrubber a test atmosphere containing the interferent
at a concentration equal to the value specified in table B-3. Sampling
shall be at the normal flow rate and shall be continued for 6 continuous
hours prior to testing.
(iii) Generate three test atmosphere streams as follows:
(A) Test atmosphere P: Pollutant concentration.
(B) Test atmosphere I: Interference concentration.
(C) Test atmosphere Z: Zero air.
(iv) Adjust the individual flow rates and the pollutant or
interferent generators for the three test atmospheres as follows:
(A) The flow rates of test atmospheres I and Z shall be identical.
(B) The concentration of pollutant in test atmosphere P shall be
adjusted such that when P is mixed (diluted) with either test atmosphere
I or Z, the resulting concentration of pollutant shall be as specified
in table B-3.
(C) The concentration of interferent in test atmosphere I shall be
adjusted such that when I is mixed (diluted) with test atmosphere P, the
resulting concentration of interferent shall be equal to the value
specified in table B-3.
(D) To minimize concentration errors due to flow rate differences
between I and Z, it is recommended that, when possible, the flow rate of
P be from 10 to 20 times larger than the flow rates of I and Z.
(v) Mix test atmospheres P and Z by passing the total flow of both
atmospheres through a mixing flask.
(vi) Sample and measure the mixture of test atmospheres P and Z with
the test analyzer. Allow for a stable reading, and record the reading,
in concentration units, as R (see Figure B-3).
(vii) Mix test atmospheres P and I by passing the total flow of both
atmospheres through a mixing flask.
(viii) Sample and measure this mixture. Record the stable reading,
in concentration units, as RI.
(ix) Calculate the interference equivalent (IE) as:
IE = RI - R
IE must be equal to or less than the specification given in table B-1
for each interferent to pass the test.
(x) Follow steps (iii) through (ix) of this section, in turn, to
determine the interference equivalent for each interferent.
(xi) For those interferents which cannot be mixed with the
pollutant, as indicated by footnote (3) in table B-3, adjust the
concentration of test atmosphere I to the specified value without being
mixed or diluted by the pollutant test atmosphere. Determine IE as
follows:
(A) Sample and measure test atmosphere Z (zero air). Allow for a
stable reading and record the reading, in concentration units, as R.
(B) Sample and measure the interferent test atmosphere I. If the
test analyzer is not capable of negative readings, adjust the analyzer
(not the recorder) to give an offset zero. Record the stable reading in
concentration units as RI, extrapolating the calibration
curve, if necessary, to represent negative readings.
(C) Calculate IE=RI-R. IE must be equal to or less than
the specification in table B-1 to pass the test.
(xii) Sum the absolute value of all the individual interference
equivalents. This sum must be equal to or less than the total
interferent specification given in table B-1 to pass the test.
(e) Zero drift, span drift, lag time, rise time, fall time, and
precision--(1) Technical definitions--(i) Zero drift: The change in
response to zero pollutant concentration, over 12- and 24-hour periods
of continuous unadjusted operation.
(ii) Span drift: The percent change in response to an up-scale
pollutant concentration over a 24-hour period of continuous unadjusted
operation.
(iii) Lag time: The time interval between a step change in input
concentration and the first observable corresponding change in response.
(iv) Rise time: The time interval between initial response and 95
percent of final response after a step increase in input concentration.
[[Page 27]]
(v) Fall time: The time interval between initial response and 95
percent of final response after a step decrease in input concentration.
(vi) Precision: Variation about the mean of repeated measurements of
the same pollutant concentration, expressed as one standard deviation
about the mean.
(2) Tests for these performance parameters shall be accomplished
over a period of seven (7) or more days. During this time, the line
voltage supplied to the test analyzer and the ambient temperature
surrounding the analyzer shall be varied from day to day. One test
result for each performance parameter shall be obtained each test day,
for seven (7) or fifteen (15) test days as necessary. The tests are
performed sequentially in a single procedure.
(3) The 24-hour test day may begin at any clock hour. The first 12
hours out of each test day are required for testing 12-hour zero drift.
Tests for the other parameters shall be conducted during the remaining
12 hours.
(4) Table B-4 specifies the line voltage and room temperature to be
used for each test day. The line voltage and temperature shall be
changed to the specified values at the start of each test day (i.e., at
the start of the 12-hour zero test). Initial adjustments (day zero)
shall be made at a line voltage of 115 volts (rms) and a room
temperature of 25 deg.C.
(5) The tests shall be conducted in blocks consisting of 3 test days
each until 7 or 15 test results have been obtained. (The final block may
contain fewer than three test days.) If a test is interrupted by an
occurrence other than a malfunction of the test analyzer, only the block
during which the interruption occurred shall be repeated.
(6) During each block, manual adjustments to the electronics, gas,
or reagent flows or periodic maintenance shall not be permitted.
Automatic adjustments which the test analyzer performs by itself are
permitted at any time.
(7) At least 4 hours prior to the start of the first test day of
each block, the test analyzer may be adjusted and/or serviced according
to the periodic maintenance procedures specified in the manual referred
to in Sec. 53.4(b)(3). If a new block is to immediately follow a
previous block, such adjustments or servicing may be done immediately
after completion of the day's tests for the last day of the previous
block and at the voltage and temperature specified for that day, but
only on test days 3, 6, 9, and 12.
Note: If necessary, the beginning of the test days succeeding such
maintenance or adjustment may be delayed as necessary to complete the
service or adjustment operation.
(8) All response readings to be recorded shall first be converted to
concentration units according to the calibration curve. Whenever a test
atmosphere is to be measured but a stable reading is not required, the
test atmosphere shall be measured long enough to cause a change in
response of at least 10% of full scale. Identify all readings and other
pertinent data on the strip chart. (See Figure B-1 illustrating the
pattern of the required readings.)
Table B-4--Line Voltage and Room Temperature Test Conditions
------------------------------------------------------------------------
Line Room
Test day voltage,\1\ temperature,\2\ Comments
rms deg.C
------------------------------------------------------------------------
0................... 115 25 Initial set-up and
adjustments.
1................... 125 20
2................... 105 20
3................... 125 30 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
4................... 105 30
5................... 125 20
6................... 105 20 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
7................... 125 30 Examine test results
to ascertain if
further testing is
required.
8................... 105 30
9................... 125 20 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
10.................. 105 20
11.................. 125 30
12.................. 105 30 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
13.................. 125 20
[[Page 28]]
14.................. 105 20
15.................. 125 30
------------------------------------------------------------------------
\1\ Voltage specified shall be controlled to plus-minus 1 volt.
\2\ Temperature specified shall be controlled to plus-minus 1 deg.C.
[[Page 29]]
[GRAPHIC] [TIFF OMITTED] TC01JY92.000
(9) Test procedure. (i) Arrange to generate pollutant test
atmospheres as follows:
------------------------------------------------------------------------
Pollutant concentration
Test atmosphere (percent)
------------------------------------------------------------------------
A0........................................ Zero air.
A20....................................... 20plus-minus5 of the upper
range limit.
A30....................................... 30plus-minus5 of the upper
range limit.
[[Page 30]]
A80....................................... 80plus-minus5 of the upper
range limit.
A90....................................... 90plus-minus5 of the upper
range limit.
------------------------------------------------------------------------
Test atmospheres A0, A20, and A80 shall
be consistent during the tests and from day to day.
(ii) For steps (xxv) through (xxxi) of this section, a chart speed
of at least 10 centimeters per hour shall be used. The actual chart
speed, chart speed changes, and time checks shall be clearly marked on
the chart.
(iii) Allow sufficient time for test analyzer to warm up and
stabilize at a line voltage of 115 volts and a room temperature of 25
deg.C. Recalibrate, if necessary, and adjust the zero baseline to 5
percent of chart. No further adjustments shall be made to the analyzer
until the end of the tests on the third day.
(iv) Measure test atmosphere A0 until a stable reading is
obtained, and record this reading (in ppm) as Z'n, where n =
0 (see Figure B-4 in appendix A).
(v) Measure test atmosphere A20. Allow for a stable
reading and record it as M'n, where n = 0.
(vi) Measure test atmosphere A80. Allow for a stable
reading and record it as S'n, where n = 0.
(vii) The above readings for Z'0, M'0, and
S'0 should be taken at least four (4) hours prior to the
beginning of test day 1.
(viii) At the beginning of each test day, adjust the line voltage
and room temperature to the values given in table B-4.
(ix) Measure test atmosphere A0 continuously for at least
twelve (12) continuous hours during each test day.
(x) After the 12-hour zero drift test (step ix), sample test
atmosphere A0. A stable reading is not required.
(xi) Measure test atmosphere A20 and record the stable
reading (in ppm) as P1. (See Figure B-4 in appendix A.)
(xii) Sample test atmosphere A30; a stable reading is not
required.
(xiii) Measure test atmosphere A20 and record the stable
reading as P2.
(xiv) Sample test atmosphere A0; a stable reading is not
required.
(xv) Measure test atmosphere A20 and record the stable
reading as P3.
(xvi) Sample test atmosphere A30; a stable reading is not
required.
(xvii) Measure test atmosphere A20 and record the stable
reading as P4.
(xviii) Sample test atmosphere A0; a stable reading is
not required.
(xix) Measure test atmosphere A20 and record the stable
reading as P5.
(xx) Sample test atmosphere A30; a stable reading is not
required.
(xxi) Measure test atmosphere A20 and record the stable
reading as P6.
(xxii) Measure test atmosphere A30 and record the stable
reading as P7.
(xxiii) Sample test atmosphere A90; a stable reading is
not required.
(xxiv) Measure test atmosphere A80 and record the stable
reading as P8. Increase chart speed to at least 10
centimeters per hour.
(xxv) Measure test atmosphere A0. Record the stable
reading as L1.
(xxvi) Quickly switch the test analyzer to measure test atmosphere
A80 and mark the recorder chart to show the exact time when
the switch occurred.
(xxvii) Measure test atmosphere A90 and record the stable
reading as P80.
(xxviii) Sample test atmosphere A90; a stable reading is
not required.
(xxix) Measure test atmosphere A80 and record the stable
reading as P10.
(xxx) Measure test atmosphere A0 and record the stable
reading as L2.
(xxxi) Measure test atmosphere A80 and record the stable
reading as P11.
(xxxii) Sample test atmosphere A90; a stable reading is
not required.
(xxxiii) Measure test atmosphere A80 and record the
stable reading as P12.
(xxxiv) Repeat steps (viii) through (xxxiii) of this section, each
test day.
(xxxv) If zero and span adjustments are made after the readings are
taken on test days 3, 6, 9, or 12, complete all adjustments; then
measure test atmospheres A0, A80, and A20.
Allow for a stable reading on each, and record the readings as
Z'nS'n, and Mn respectively, where n =
the test day number.
(10) Determine the results of each day's tests as follows. Mark the
recorder chart to show readings and determinations.
(i) Zero drift. (A) 12-hour. Examine the strip chart pertaining to
the 12-
[[Page 31]]
hour continuous zero air test. Determine the minimum (Cmin.) and maximum
(Cmax.) readings (in p/m) during this period of 12 consecutive hours,
extrapolating the calibration curve to negative concentration units if
necessary. Determine the 12-hour zero drift (12ZD) as 12ZD =
Cmax.-Cmin.. (See Figure B-5 in appendix A.)
(B) Calculate the 24-hour zero drift (24ZD) for the n-th test day as
24ZDn = Zn-Zn-1, or 24ZDn =
Zn-Z'n-1 if zero adjustment was made on the
previous day, where Zn = \1/2\(L1+L2)
for L1 and L2 taken on the n-th test day.
(C) Compare 12ZD and 24ZD to the zero drift specification in table
B-1. Both 12ZD and 24ZD must be equal to or less than the specified
value to pass the test for zero drift.
(ii) Span drift. (A) Span drift at 20 percent of URL (MSD)
[GRAPHIC] [TIFF OMITTED] TC09NO91.000
[GRAPHIC] [TIFF OMITTED] TC09NO91.001
If span adjustment was made on the previous day, where
[GRAPHIC] [TIFF OMITTED] TC09NO91.002
n indicates the n-th test day, and i indicates the i-th reading on the n
th day.
(B) Span drift at 80 percent of URL (USD):
[GRAPHIC] [TIFF OMITTED] TC09NO91.003
or
[GRAPHIC] [TIFF OMITTED] TC09NO91.004
If span adjustment was made on the previous day, where
[GRAPHIC] [TIFF OMITTED] TC09NO91.005
n indicates the n-th test day, and i indicates the i-th reading on the
n-th test day.
(C) Both USD and MSD must be equal to or less than the respective
specifications given in table B-1 to pass the test for span draft.
(iii) Lag time. Determine, from the strip chart, the elapsed time in
minutes between the mark made in step (xxvi) and the first observable
(two times the noise level) response. This time must be equal to or less
than the time specified in table B-1 to pass the test for lag time.
(iv) Rise time. Calculate 95 percent of reading P9 and
determine from the recorder chart, the elapsed time between the first
observable (two times noise level) response and a response equal to 95
percent of the P9 reading. This time must be equal to or less
than the rise time specified in table B-1 to pass the test for rise
time.
(v) Fall time. Calculate five percent of
(P10-L2) and determine, from the strip chart, the
elapsed time in minutes between the first observable decrease in
response following reading P10 and a response equal to five
percent of (P10-L2). This time must be equal to or
less than the fall time specification in table B-1 to pass the test for
fall time.
(vi) Precision. Calculate precision (P20 and
P80) for each day's test as follows:
(A)
[GRAPHIC] [TIFF OMITTED] TC09NO91.006
(B)
[GRAPHIC] [TIFF OMITTED] TC09NO91.007
[[Page 32]]
(C) Both P20 and P80 must be equal to or less
than the specification given in table B-1 to pass the test for
precision.
[40 FR 7049, Feb. 18, 1975, as amended at 41 FR 52694, Dec. 1, 1976]
Appendix A to Subpart B--Optional Forms for Reporting Test Results
Table B-5--Symbols and Abbreviations
BL............................ Analyzer reading at specified LDL
concentration.
Bz............................ Analyzer reading at 0 concentration for
LDL test.
DM............................ Digital meter.
Cmax.......................... Maximum analyzer reading during 12ZD
test.
Cmin.......................... Minimum analyzer reading during 12ZD
test.
i............................. Subscript indicating the i-th quantity
in a series.
IE............................ Interference equivalent.
L1............................ First analyzer zero reading for 24ZD
test.
L2............................ Second analyzer zero reading for 24ZD
test.
Mn............................ Average of P1 . . . P6 for the n-th test
day.
M'n........................... Adjusted span reading at 20 percent of
URL on the n-th test day.
MSD........................... Span drift at 20 percent of URL.
n............................. Subscript indicating the test day
number.
P............................. Analyzer reading for precision test.
Pi............................ The i-th analyzer reading for precision
test.
P20........................... Precision at 20 percent of URL.
P80........................... Precision at 80 percent of URL.
R............................. Analyzer reading of pollutant alone for
IE test.
RI............................ Analyzer reading with interferent added
for IE test.
ri............................ The i-th DM reading for noise test.
S............................. Standard deviation of noise readings.
S0............................ Noise value (S) measured at 0
concentration.
S80........................... Noise value (S) measured at 80 percent
of URL.
Sn............................ Average of P7 . . . P12 for the n-th
test day.
S'n........................... Adjusted span reading at 80 percent of
URL on the n-th test day.
URL........................... Upper range limit.
USD........................... Span drift at 80 percent o
Z............................. Average of L1 and L2.
Zn............................ Average of L1 and L2 on the n-th test
day.
Z'n........................... Adjusted zero reading on the n-th test
day.
ZD............................ Zero drift.
12ZD.......................... 12-hour zero drift.
24ZD.......................... 24-hour zero drift.
[[Page 33]]
[[Page 34]]
[[Page 35]]
[[Page 36]]
[[Page 37]]
[GRAPHIC] [TIFF OMITTED] TC09NO91.031
[40 FR 7049, Feb. 18, 1975, as amended at 40 FR 18169, Apr. 25, 1975]
Subpart C--Procedures for Determining Comparability Between Candidate
Methods and Reference Methods
Source: 62 FR 38792, July 18, 1997, unless otherwise noted.
Sec. 53.30 General provisions.
(a) Determination of comparability. The test procedures prescribed
in this subpart shall be used to determine if a candidate method is
comparable to a reference method when both methods measure pollutant
concentrations in ambient air.
[[Page 38]]
(1) Comparability is shown for SO2, CO, O3,
and NO2 methods when the differences between:
(i) Measurements made by a candidate manual method or by a test
analyzer representative of a candidate automated method.
(ii) Measurements made simultaneously by a reference method, are
less than or equal to the values specified in the last column of table
C-1 of this subpart.
(2) Comparability is shown for lead methods when the differences
between:
(i) Measurements made by a candidate method.
(ii) Measurements made by the reference method on simultaneously
collected lead samples (or the same sample, if applicable), are less
than or equal to the value specified in table C-3 of this subpart.
(3) Comparability is shown for PM10 and PM2.5
methods when the relationship between:
(i) Measurements made by a candidate method.
(ii) Measurements made by a reference method on simultaneously
collected samples (or the same sample, if applicable) at each of two
test sites, is such that the linear regression parameters (slope,
intercept, and correlation coefficient) describing the relationship meet
the values specified in table C-4 of this subpart.
(b) Selection of test sites--(1) All methods. Each test site shall
be in a predominately urban area which can be shown to have at least
moderate concentrations of various pollutants. The site shall be clearly
identified and shall be justified as an appropriate test site with
suitable supporting evidence such as maps, population density data,
vehicular traffic data, emission inventories, pollutant measurements
from previous years, concurrent pollutant measurements, and
meteorological data. If approval of a proposed test site is desired
prior to conducting the tests, a written request for approval of the
test site or sites must be submitted prior to conducting the tests and
must include the supporting and justification information required. The
Administrator may exercise discretion in selecting a different site (or
sites) for any additional tests the Administrator decides to conduct.
(2) Methods for SO2, CO, O3, and
NO2. All test measurements are to be made at the same test
site. If necessary, the concentration of pollutant in the sampled
ambient air may be augmented with artificially generated pollutant to
facilitate measurements in the specified ranges described under
paragraph (d)(2) of this section.
(3) Methods for Pb. Test measurements may be made at any number of
test sites. Augmentation of pollutant concentrations is not permitted,
hence an appropriate test site or sites must be selected to provide lead
concentrations in the specified range.
(4) Methods for PM10. Test measurements must be made, or
derived from particulate samples collected, at not less than two test
sites, each of which must be located in a geographical area
characterized by ambient particulate matter that is significantly
different in nature and composition from that at the other test site(s).
Augmentation of pollutant concentrations is not permitted, hence
appropriate test sites must be selected to provide PM10
concentrations in the specified range. The tests at the two sites may be
conducted in different calendar seasons, if appropriate, to provide
PM10 concentrations in the specified ranges.
(5) Methods for PM2.5. Augmentation of pollutant
concentrations is not permitted, hence appropriate test sites must be
selected to provide PM2.5 concentrations and
PM2.5/PM10 ratios (if applicable) in the specified
ranges.
(i) Where only one test site is required, as specified in table C-4
of this subpart, the site need only meet the PM2.5 ambient
concentration levels required by Sec. 53.34(c)(3).
(ii) Where two sites are required, as specified in table C-4 of this
subpart, each site must be selected to provide the ambient concentration
levels required by Sec. 53.34(c)(3). In addition, one site must be
selected such that all acceptable test sample sets, as defined in
Sec. 53.34(c)(3), have a PM2.5/PM10 ratio of more
than 0.75; the other site must be selected such that all acceptable test
sample sets, as defined in Sec. 53.34(c)(3), have a PM2.5/
PM10 ratio of less than 0.40. At least two reference method
[[Page 39]]
PM10 samplers shall be collocated with the candidate and
reference method PM2.5 samplers and operated simultaneously
with the other samplers at each test site to measure concurrent ambient
concentrations of PM10 to determine the PM2.5/
PM10 ratio for each sample set. The PM2.5/
PM10 ratio for each sample set shall be the average of the
PM2.5 concentration, as determined in Sec. 53.34(c)(1),
divided by the average PM10 concentration, as measured by the
PM10 samplers. The tests at the two sites may be conducted in
different calendar seasons, if appropriate, to provide PM2.5
concentrations and PM2.5/PM10 ratios in the
specified ranges.
(c) Test atmosphere. Ambient air sampled at an appropriate test site
or sites shall be used for these tests. Simultaneous concentration
measurements shall be made in each of the concentration ranges specified
in tables C-1, C-3, or C-4 of this subpart, as appropriate.
(d) Sample collection--(1) All methods. All test concentration
measurements or samples shall be taken in such a way that both the
candidate method and the reference method receive air samples that are
homogenous or as nearly identical as practical.
(2) Methods for SO2, CO, O3, and
NO2. Ambient air shall be sampled from a common intake and
distribution manifold designed to deliver homogenous air samples to both
methods. Precautions shall be taken in the design and construction of
this manifold to minimize the removal of particulates and trace gases,
and to ensure that identical samples reach the two methods. If
necessary, the concentration of pollutant in the sampled ambient air may
be augmented with artificially-generated pollutant. However, at all
times the air sample measured by the candidate and reference methods
under test shall consist of not less than 80 percent ambient air by
volume. Schematic drawings, physical illustrations, descriptions, and
complete details of the manifold system and the augmentation system (if
used) shall be submitted.
(3) Methods for Pb, PM10 and PM2.5. The
ambient air intake points of all the candidate and reference method
collocated samplers for lead, PM10 or PM2.5 shall
be positioned at the same height above the ground level, and between 2
and 4 meters apart. The samplers shall be oriented in a manner that will
minimize spatial and wind directional effects on sample collection.
(4) PM10 methods employing the same sampling procedure as
the reference method but a different analytical method. Candidate
methods for PM10 which employ a sampler and sample collection
procedure that are identical to the sampler and sample collection
procedure specified in the reference method, but use a different
analytical procedure, may be tested by analyzing common samples. The
common samples shall be collected according to the sample collection
procedure specified by the reference method and shall be analyzed in
accordance with the analytical procedures of both the candidate method
and the reference method.
(e) Submission of test data and other information. All recorder
charts, calibration data, records, test results, procedural descriptions
and details, and other documentation obtained from (or pertinent to)
these tests shall be identified, dated, signed by the analyst performing
the test, and submitted. For candidate methods for PM2.5, all
submitted information must meet the requirements of the ANSI/ASQC E4
Standard, sections 3.3.1, paragraphs 1 and 2 (reference 1 of appendix A
of this subpart).
Sec. 53.31 Test conditions.
(a) All methods. All test measurements made or test samples
collected by means of a sample manifold as specified in Sec. 53.30(d)(2)
shall be at a room temperature between 20 deg.C and 30 deg.C, and at a
line voltage between 105 and 125 volts. All methods shall be calibrated
as specified in paragraph (c) of this section prior to initiation of the
tests.
(b) Samplers and automated methods. (1) Setup and start-up of the
test analyzer, test sampler(s), and reference method (if applicable)
shall be in strict accordance with the applicable operation manual(s).
If the test analyzer does not have an integral strip chart or digital
data recorder, connect the analyzer output to a suitable strip chart or
digital data recorder. This recorder shall have a chart width of at
least 25
[[Page 40]]
centimeters, a response time of 1 second or less, a deadband of not more
than 0.25 percent of full scale, and capability of either reading
measurements at least 5 percent below zero or offsetting the zero by at
least 5 percent. Digital data shall be recorded at appropriate time
intervals such that trend plots similar to a strip chart recording may
be constructed with a similar or suitable level of detail.
(2) Other data acquisition components may be used along with the
chart recorder during the conduct of these tests. Use of the chart
recorder is intended only to facilitate visual evaluation of data
submitted.
(3) Allow adequate warmup or stabilization time as indicated in the
applicable operation manual(s) before beginning the tests.
(c) Calibration. The reference method shall be calibrated according
to the appropriate appendix to part 50 of this chapter (if it is a
manual method) or according to the applicable operation manual(s) (if it
is an automated method). A candidate manual method (or portion thereof)
shall be calibrated, according to the applicable operation manual(s), if
such calibration is a part of the method.
(d) Range. (1) Except as provided in paragraph (d)(2) of this
section, each method shall be operated in the range specified for the
reference method in the appropriate appendix to part 50 of this chapter
(for manual reference methods), or specified in table B-1 of subpart B
of this part (for automated reference methods).
(2) For a candidate method having more than one selectable range,
one range must be that specified in table B-1 of subpart B of this part
and a test analyzer representative of the method must pass the tests
required by this subpart while operated on that range. The tests may be
repeated for a broader range (i.e., one extending to higher
concentrations) than the one specified in table B-1 of subpart B of this
part, provided that the range does not extend to concentrations more
than two times the upper range limit specified in table B-1 of subpart B
of this part and that the test analyzer has passed the tests required by
subpart B of this part (if applicable) for the broader range. If the
tests required by this subpart are conducted or passed only for the
range specified in table B-1 of subpart B of this part, any equivalent
method determination with respect to the method will be limited to that
range. If the tests are passed for both the specified range and a
broader range (or ranges), any such determination will include the
broader range(s) as well as the specified range. Appropriate test data
shall be submitted for each range sought to be included in such a
determination.
(e) Operation of automated methods. (1) Once the test analyzer has
been set up and calibrated and tests started, manual adjustment or
normal periodic maintenance as specified in the manual referred to in
Sec. 53.4(b)(3) is permitted only every 3 days. Automatic adjustments
which the test analyzer performs by itself are permitted at any time.
The submitted records shall show clearly when manual adjustments were
made and describe the operations performed.
(2) All test measurements shall be made with the same test analyzer;
use of multiple test analyzers is not permitted. The test analyzer shall
be operated continuously during the entire series of test measurements.
(3) If a test analyzer should malfunction during any of these tests,
the entire set of measurements shall be repeated, and a detailed
explanation of the malfunction, remedial action taken, and whether
recalibration was necessary (along with all pertinent records and
charts) shall be submitted.
Sec. 53.32 Test procedures for methods for SO2, CO, O3, and NO2.
(a) Conduct the first set of simultaneous measurements with the
candidate and reference methods:
(1) Table C-1 of this subpart specifies the type (1- or 24-hour) and
number of measurements to be made in each of the three test
concentration ranges.
(2) The pollutant concentration must fall within the specified range
as measured by the reference method.
(3) The measurements shall be made in the sequence specified in
table C-2 of this subpart, except for the 1-hour SO2
measurements, which are all in the high range.
[[Page 41]]
(b) For each pair of measurements, determine the difference
(discrepancy) between the candidate method measurement and reference
method measurement. A discrepancy which exceeds the discrepancy
specified in table C-1 of this subpart constitutes a failure. Figure C-1
of this subpart contains a suggested format for reporting the test
results.
(c) The results of the first set of measurements shall be
interpreted as follows:
(1) Zero failures. The candidate method passes the test for
comparability.
(2) Three or more failures. The candidate method fails the test for
comparability.
(3) One or two failures. Conduct a second set of simultaneous
measurements as specified in table C-1 of this subpart. The results of
the combined total of first-set and second-set measurements shall be
interpreted as follows:
(i) One or two failures. The candidate method passes the test for
comparability.
(ii) Three or more failures. The candidate method fails the test for
comparability.
(4) For SO2, the 1-hour and 24-hour measurements shall be
interpreted separately, and the candidate method must pass the tests for
both 1- and 24-hour measurements to pass the test for comparability.
(d) A 1-hour measurement consists of the integral of the
instantaneous concentration over a 60-minute continuous period divided
by the time period. Integration of the instantaneous concentration may
be performed by any appropriate means such as chemical, electronic,
mechanical, visual judgment, or by calculating the mean of not less than
12 equally spaced instantaneous readings. Appropriate allowances or
corrections shall be made in cases where significant errors could occur
due to characteristic lag time or rise/fall time differences between the
candidate and reference methods. Details of the means of integration and
any corrections shall be submitted.
(e) A 24-hour measurement consists of the integral of the
instantaneous concentration over a 24-hour continuous period divided by
the time period. This integration may be performed by any appropriate
means such as chemical, electronic, mechanical, or by calculating the
mean of 24 sequential 1-hour measurements.
(f) For ozone and carbon monoxide, no more than six 1-hour
measurements shall be made per day. For sulfur dioxide, no more than
four 1-hour measurements or one 24-hour measurement shall be made per
day. One-hour measurements may be made concurrently with 24-hour
measurements if appropriate.
(g) For applicable methods, control or calibration checks may be
performed once per day without adjusting the test analyzer or method.
These checks may be used as a basis for a linear interpolation-type
correction to be applied to the measurements to correct for drift. If
such a correction is used, it shall be applied to all measurements made
with the method, and the correction procedure shall become a part of the
method.
Sec. 53.33 Test procedure for methods for lead.
(a) Sample collection. Collect simultaneous 24-hour samples
(filters) of lead at the test site or sites with both the reference and
candidate methods until at least 10 filter pairs have been obtained. If
the conditions of Sec. 53.30(d)(4) apply, collect at least 10 common
samples (filters) in accordance with Sec. 53.30(d)(4) and divide each to
form the filter pairs.
(b) Audit samples. Three audit samples must be obtained from the
address given in Sec. 53.4(a). The audit samples are 3/4 x 8-inch glass
fiber strips containing known amounts of lead at the following nominal
levels: 100 g/strip; 300 g/strip; 750 g/
strip. The true amount of lead, in total g/strip, will be
provided with each audit sample.
(c) Filter analysis. (1) For both the reference method samples and
the audit samples, analyze each filter extract three times in accordance
with the reference method analytical procedure. The analysis of
replicates should not be performed sequentially, i.e., a single sample
should not be analyzed three
[[Page 42]]
times in sequence. Calculate the indicated lead concentrations for the
reference method samples in g/m3 for each analysis
of each filter. Calculate the indicated total lead amount for the audit
samples in g/strip for each analysis of each strip. Label these
test results as R1A, R1B, R1C,
R2A, R2B, ..., Q1A, Q1B,
Q1C, ..., where R denotes results from the reference method
samples; Q denotes results from the audit samples; 1, 2, 3 indicate the
filter number, and A, B, C indicate the first, second, and third
analysis of each filter, respectively.
(2) For the candidate method samples, analyze each sample filter or
filter extract three times and calculate, in accordance with the
candidate method, the indicated lead concentrates in g/
m3 for each analysis of each filter. Label these test results
as C1A, C1B, C2C, ..., where C denotes
results from the candidate method. For candidate methods which provide a
direct measurement of lead concentrations without a separable procedure,
C1A = C1B = C1C, C2A =
C2B = C2C, etc.
(d) Average lead concentration. For the reference method, calculate
the average lead concentration for each filter by averaging the
concentrations calculated from the three analyses:
Equation 1
[GRAPHIC] [TIFF OMITTED] TR18JY97.052
where:
i is the filter number.
(e) Acceptable filter pairs. Disregard all filter pairs for which
the lead concentration as determined in the previous paragraph (d) of
this section by the average of the three reference method
determinations, falls outside the range of 0.5 to 4.0 g/
m3. All remaining filter pairs must be subjected to both of
the following tests for precision and comparability. At least five
filter pairs must be within the 0.5 to 4.0 g/m3
range for the tests to be valid.
(f) Test for precision. (1) Calculate the precision (P) of the
analysis (in percent) for each filter and for each method, as the
maximum minus the minimum divided by the average of the three
concentration values, as follows:
Equation 2
[GRAPHIC] [TIFF OMITTED] TR18JY97.053
or
Equation 3
[GRAPHIC] [TIFF OMITTED] TR18JY97.054
where:
i indicates the filter number.
(2) If any reference method precision value (PRi) exceeds
15 percent, the precision of the reference method analytical procedure
is out of control. Corrective action must be taken to determine the
source(s) of imprecision and the reference method determinations must be
repeated according to paragraph (c) of this section, or the entire test
procedure (starting with paragraph (a) of this section) must be
repeated.
(3) If any candidate method precision value (PCi) exceeds
15 percent, the candidate method fails the precision test.
(4) The candidate method passes this test if all precision values
(i.e., all PRi's and all PCi's) are less than 15
percent.
(g) Test for accuracy. (1)(i) For the audit samples calculate the
average lead concentration for each strip by averaging the
concentrations calculated from the three analyses:
Equation 4
[GRAPHIC] [TIFF OMITTED] TR18JY97.055
where:
i is audit sample number.
(ii) Calculate the percent difference (Dq) between the
indicated lead concentration for each audit sample and the true lead
concentration (Tq) as follows:
Equation 5
[GRAPHIC] [TIFF OMITTED] TR18JY97.056
(2) If any difference value (Dqi) exceeds 5
percent, the accuracy of the
[[Page 43]]
reference method analytical procedure is out of control. Corrective
action must be taken to determine the source of the error(s) (e.g.,
calibration standard discrepancies, extraction problems, etc.) and the
reference method and audit sample determinations must be repeated
according to paragraph (c) of this section, or the entire test procedure
(starting with paragraph (a) of this section) must be repeated.
(h) Test for comparability. (1) For each filter pair, calculate all
nine possible percent differences (D) between the reference and
candidate methods, using all nine possible combinations of the three
determinations (A, B, and C) for each method, as:
Equation 6
[GRAPHIC] [TIFF OMITTED] TR18JY97.057
where:
i is the filter number, and n numbers from 1 to 9 for the nine possible
difference combinations for the three determinations for each method (j
= A, B, C, candidate; k = A, B, C, reference).
(2) If none of the percent differences (D) exceeds 20
percent, the candidate method passes the test for comparability.
(3) If one or more of the percent differences (D) exceeds
20 percent, the candidate method fails the test for
comparability.
(i) The candidate method must pass both the precision test
(paragraph (f) of this section) and the comparability test (paragraph
(h) of this section) to qualify for designation as an equivalent method.
Sec. 53.34 Test procedure for methods for PM10 and PM2.5.
(a) Collocated measurements. Set up three reference method samplers
collocated with three candidate method samplers or analyzers at each of
the number of test sites specified in table C-4 of this subpart. At each
site, obtain as many sets of simultaneous PM10 or
PM2.5 measurements as necessary (see paragraph (c)(3) of this
section), each set consisting of three reference method and three
candidate method measurements, all obtained simultaneously. For
PM2.5 candidate Class II equivalent methods, at least two
collocated PM10 reference method samplers are also required
to obtain PM2.5/PM10 ratios for each sample set.
Candidate PM10 method measurements shall be 24-hour
integrated measurements; PM2.5 measurements may be either 24-
or 48-hour integrated measurements. All collocated measurements in a
sample set must cover the same 24- or 48-hour time period. For samplers,
retrieve the samples promptly after sample collection and analyze each
sample according to the reference method or candidate method, as
appropriate, and determine the PM10 or PM2.5
concentration in g/m3. If the conditions of
Sec. 53.30(d)(4) apply, collect sample sets only with the three
reference method samplers. Guidance for quality assurance procedures for
PM2.5 methods is found in section 2.12 of the Quality
Assurance Handbook (reference 6 of appendix A to subpart A of this
part).
(b) Sequential samplers. For sequential samplers, the sampler shall
be configured for the maximum number of sequential samples and shall be
set for automatic collection of all samples sequentially such that the
test samples are collected equally, to the extent possible, among all
available sequential channels or utilizing the full available sequential
capability.
(c) Test for comparability and precision. (1) For each of the
measurement sets, calculate the average PM10 or
PM2.5 concentration obtained with the reference method
samplers:
Equation 7
[GRAPHIC] [TIFF OMITTED] TR18JY97.058
where:
R denotes results from the reference method;
i is the sampler number; and
j is the set.
(2)(i) For each of the measurement sets, calculate the precision of
the reference method PM10 or PM2.5 measurements
as:
[[Page 44]]
Equation 8
[GRAPHIC] [TIFF OMITTED] TR18JY97.059
If the corresponding Rj is below:
80 g/m3 for PM10 methods.
40 g/m3 for 24-hour PM2.5 at single test
sites for Class I candidate methods.
40 g/m3 for 24-hour PM2.5 at sites having
PM2.5/PM10 ratios >0.75.
30 g/m3 for 48-hour PM2.5 at single test
sites for Class I candidate methods.
30 g/m3 for 48-hour PM2.5 at sites having
PM2.5/PM10 ratios >0.75.
30 g/m3 for 24-hour PM2.5 at sites having
PM2.5/PM10 ratios 0.40.
20 g/m3 for 48-hour PM2.5 at sites having
PM2.5/PM10 ratios >0.75.
(ii) Otherwise, calculate the precision of the reference method
PM10 or PM2.5 measurements as:
Equation 9
[GRAPHIC] [TIFF OMITTED] TR18JY97.060
(3) If Rj falls outside the acceptable concentration
range specified in table C-4 of this subpart for any set, or if
Pj RPj as applicable, exceeds the value specified
in table C-4 of this subpart for any set, that set of measurements shall
be discarded. For each site, table C-4 of this subpart specifies the
minimum number of sample sets required for various conditions, and
Sec. 53.30(b)(5) specifies the PM2.5/PM10 ratio
requirements applicable to Class II candidate equivalent methods.
Additional measurement sets shall be collected and analyzed, as
necessary, to provide a minimum of 10 acceptable measurement sets for
each test site. If more than 10 measurement sets are collected that meet
the above criteria, all such measurement sets shall be used to
demonstrate comparability.
(4) For each of the acceptable measurement sets, calculate the
average PM10 or PM2.5 concentration obtained with
the candidate method samplers:
Equation 10
[GRAPHIC] [TIFF OMITTED] TR18JY97.061
where:
C denotes results from the candidate method;
i is the sampler number; and
j is the set.
(5) For each site, plot the average PM10 or
PM2.5 measurements obtained with the candidate method
(Rj) against the corresponding average PM10 or
PM2.5 measurements obtained with the reference method
(Rj). For each site, calculate and record the linear
regression slope and intercept, and the correlation coefficient.
(6) If the linear regression parameters calculated under paragraph
(c)(5) of this section meet the values specified in table C-4 of this
subpart for all test sites, the candidate method passes the test for
comparability.
[62 FR 38792, July 19, 1997; 63 FR 7714, Feb. 17, 1998]
Table C-1 to Subpart C--Test Concentration Ranges, Number of
Measurements Required, and Maximum Discrepancy Specification
--------------------------------------------------------------------------------------------------------------------------------------------------------
Simultaneous Measurements Required Maximum
------------------------------------------------ Discrepancy
Pollutant Concentration Range Parts per Million 1-hr 24-hr Specification,
------------------------------------------------ Parts per
First Set Second Set First Set Second Set Million
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ozone...................................... Low 0.06 to 0.10......................... 5 6 .......... .......... 0.02
Med 0.15 to 0.25......................... 5 6 .......... .......... .03
High 0.35 to 0.45........................ 4 6 .......... .......... .04
-----------------------------------------------------------------
Total.................................. 14 18
=================================================================
Carbon Monoxide............................ Low 7 to 11.............................. 5 6 .......... .......... 1.5
Med 20 to 30............................. 5 6 .......... .......... 2.0
[[Page 45]]
High 35 to 45............................ 4 6 .......... .......... 3.0
-----------------------------------------------------------------
Total.................................. 14 18
=================================================================
Sulfur Dioxide............................. Low 0.02 to 0.05......................... .......... .......... 3 3 0.02
Med 0.10 to 0.15......................... .......... .......... 2 3 .03
High 0.30 to 0.50........................ 7 8 2 2 .04
-----------------------------------------------------------------
Total................................. 7 8 7 8
=================================================================
Nitrogen Dioxide........................... Low 0.02 to 0.08......................... .......... .......... 3 3 0.02
Med 0.10 to 0.20......................... .......... .......... 2 3 .03
High 0.25 to 0.35........................ .......... .......... 2 2 .03
-----------------------------------------------------------------
Total.................................. .......... .......... 7 8
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table C-2 to Subpart C--Sequence of Test Measurements
------------------------------------------------------------------------
Concentration Range
Measurement ---------------------------------
First Set Second Set
------------------------------------------------------------------------
1..................................... Low Medium
2..................................... High High
3..................................... Medium Low
4..................................... High High
5..................................... Low Medium
6..................................... Medium Low
7..................................... Low Medium
8..................................... Medium Low
9..................................... High High
10.................................... Medium Low
11.................................... High Medium
12.................................... Low High
13.................................... Medium Medium
14.................................... Low High
15.................................... ............... Low
16.................................... ............... Medium
17.................................... ............... Low
18.................................... ............... High
------------------------------------------------------------------------
Table C-3 to Subpart C--Test Specifications for Lead Methods
------------------------------------------------------------------------
------------------------------------------------------------------------
Concentration range, g/m\3\.......................... 0.5-4.0
Minimum number of 24-hr measurements.......................... 5
Maximum analytical precision, percent......................... 5
Maximum analytical accuracy, percent.......................... 10 and PM2.5 Methods
------------------------------------------------------------------------
PM2.5
Specification PM10 -------------------------
Class I Class II
------------------------------------------------------------------------
Acceptable concentration range 30-300 10-200 10-200
(Rj), g/m3.............
Minimum number of test sites..... 2 1 2
Number of candidate method 3 3 3
samplers per site...............
Number of reference method 3 3 3
samplers per site...............
Minimum number of acceptable
sample sets per site for PM10:
Rj 80 g/m3......... 3
Rj > 80 g/m3........ 3
Total.................... 10
[[Page 46]]
Minimum number of acceptable
sample sets per site for PM2.5:
Single test site for Class I
candidate equivalent
methods:
Rj 40 g/m3 for 3
24-hr or Rj 30 g/m3 for 48-hr samples
Rj > 40 g/m3 for 3
24-hr or Rj > 30 g/m3 for 48-hr samples
Sites at which the PM2.5/PM10
ratio must be > 0.75:
Rj 40 g/m3 for 3
24-hr or Rj 30 g/m3 for 48-hr samples
Rj > 40 g/m3 for 3
24-hr or Rj > 30 g/m3 for 48-hr samples
Sites at which the PM2.5/PM10
ratio must be 0.40:
Rj 30 g/m3 for 3
24-hr or Rj 20 g/m3 for 48-hr samples
Rj > 30 g/m3 for 3
24-hr or Rj > 20 g/m3 for 48-hr samples
Total, each site................. 10 10
Precision of replicate reference 5 j or RPj m>g/m3 or m>g/m3 or m>g/m3 or
respectively, maximum........... 7% 5% 5%
Slope of regression relationship. 1g/m3..... s5 s1 s1
Correlation of reference method
and candidate method 0.97 0.97 0.97
measurements....................
------------------------------------------------------------------------
[62 FR 38792, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
[[Page 47]]
Figure C-1 to Subpart C--Suggested Format for Reporting Test
Results
Candidate Method____________________________________________________________
Reference Method____________________________________________________________
Applicant____________________________________________________________________
{time} First Set {time} Second Set {time} Type {time} 1 Hour {time} 24 Hour
----------------------------------------------------------------------------------------------------------------
Concentration, ppm
Concentration Range Date Time -------------------------- Difference Table C-1 Pass or
Candidate Reference Spec. Fail
----------------------------------------------------------------------------------------------------------------
Low 1
__________ ppm
to ________ ppm1
--------------------------------------------------------------------------------------------
2
--------------------------------------------------------------------------------------------
3
--------------------------------------------------------------------------------------------
4
--------------------------------------------------------------------------------------------
5
--------------------------------------------------------------------------------------------
6
----------------------------------------------------------------------------------------------------------------
Medium 1
__________ ppm
to ________ ppm1
--------------------------------------------------------------------------------------------
2
--------------------------------------------------------------------------------------------
3
--------------------------------------------------------------------------------------------
4
--------------------------------------------------------------------------------------------
5
--------------------------------------------------------------------------------------------
6
----------------------------------------------------------------------------------------------------------------
High 1
__________ ppm
to ________ ppm1
--------------------------------------------------------------------------------------------
2
--------------------------------------------------------------------------------------------
3
--------------------------------------------------------------------------------------------
4
--------------------------------------------------------------------------------------------
5
--------------------------------------------------------------------------------------------
6
--------------------------------------------------------------------------------------------
7
--------------------------------------------------------------------------------------------
8
--------------------------------------------------------------------------------------------
... .......... .......... ........... ........... ............ Total
Failures:
----------------------------------------------------------------------------------------------------------------
Appendix A to Subpart C--References
(1) American National Standard--Specifications and Guidelines for
Quality Systems for Environmental Data Collection and Environmental
Technology Programs, ANSI/ASQC E4-1994. Available from American Society
for Quality Control, 611 East Wisconsin Avenue, Milwaukee, WI 53202.
Subpart D--Procedures for Testing Performance Characteristics of Methods
for PM10
Source: 52 FR 24729, July 1, 1987, unless otherwise noted.
[[Page 48]]
Sec. 53.40 General provisions.
(a) The test procedures prescribed in this subpart shall be used to
test the performance of candidate methods for PM10 against
the performance specifications given in table D-1. Except as provided in
paragraph (b) of this section, a test sampler or samplers representative
of the sampler described in the candidate method must exhibit
performance better than, or equal to, the specified value for each
performance parameter, to satisfy the requirements of this subpart.
(b) For a candidate method using a PM10 sampler
previously approved as part of a designated PM10 method, only
the test for precision need be conducted and passed to satisfy the
requirements of this subpart. For a candidate method using a
PM10 sampler inlet previously approved as part of a
designated PM10 method, the tests for precision and flow rate
stability must be conducted and passed to satisfy the requirements of
this subpart; the tests for sampling effectiveness and 50 percent
cutpoint need not be conducted if suitable rationale is provided to
demonstrate that test results submitted for the previously approved
method are applicable to the candidate method.
(c) The liquid particle sampling effectiveness and 50 percent
cutpoint of a test sampler shall be determined in a wind tunnel using 10
particle sizes and three wind speeds as specified in table D-2. A
minimum of 3 replicate measurements of sampling effectiveness shall be
required for each of the 30 test conditions for a minimum of 90 test
measurements.
(d) For the liquid particle sampling effectiveness parameter, a
smooth curve plot shall be constructed of sampling effectiveness
(percent) versus aerodynamic particle diameter (m) for each of
the three wind speeds. These plots shall be used to calculate the
expected mass concentration for the test sampler, using the procedure in
Sec. 53.43(a). The candidate method passes the liquid particle sampling
effectiveness test if the expected mass concentration calculated for the
test sampler at each wind speed differs by no more than 10
percent from that predicted for the ``ideal'' sampler.*
---------------------------------------------------------------------------
* The sampling effectiveness curve for this ``ideal'' sampler is
described by column 5 of table D-3 and is based on a model that
approximates the penetration of particles into the human respiratory
tract. Additional information on this model may be found in a document
entitled, ``Particle Collection Criteria for 10 Micrometer Samplers,''
which is available from the Quality Assurance Division (MD-77),
Environmental Monitoring Systems Laboratory, U.S. Environmental
Protection Agency, Research Triangle Park, NC 27711.
---------------------------------------------------------------------------
(e) For the 50 percent cutpoint parameter, the test result for each
wind speed shall be reported as the particle size at which the curve
specified in Sec. 53.40(d) crosses the 50 percent effectiveness line.
The candidate method passes the 50 percent cutpoint test if the test
result at each wind speed falls within 100.5 m.
(f) The solid particle sampling effectiveness of a test sampler
shall be determined in a wind tunnel using 25 m particles at 2
wind speeds as specified in table D-2. A minimum of three replicate
measurements of sampling effectiveness for the 25 m solid
particles shall be required at both wind speeds for a minimum of 6 test
measurements.
(g) For the solid particle sampling effectiveness parameter, the
test result for each wind speed shall be reported as the difference
between the average of the replicate sampling effectiveness measurements
obtained for the 25 m solid particles and the average of the
replicate measurements obtained for the 25 m liquid particles.
The candidate method passes the solid particle sampling effectiveness
test if the test result for each wind speed is less than, or equal to, 5
percent.
(h) The precision and flow rate stability of three identical test
samplers shall be determined at a suitable test site by simultaneously
sampling the PM10 concentration of the atmosphere for 10
periods of 24 hours.
(i) For the precision parameter, the test result for each of the 10
periods of 24 hours shall be calculated using the procedure in
Sec. 53.43(c). The candidate method passes the precision test if all of
the test results meet the specifications in table D-1.
[[Page 49]]
(j) For the flow rate stability parameter, the test results for each
of the three test samplers and for each of the 10 periods of 24 hours
shall be calculated using the procedure in Sec. 53.43(d). The candidate
method passes the flow rate stability test if all of the test results
meet the specifications in table D-1.
(k) All test data and other documentation obtained from or pertinent
to these tests shall be identified, dated, signed by the analyst
performing the test, and submitted to EPA.
Table D-1--Performance Specifications for PM10 Samplers
------------------------------------------------------------------------
Performance parameter Units Specification
------------------------------------------------------------------------
1. Sampling effectiveness:
A. Liquid particles......... Percent.......... Such that the
expected mass
concentration is
within 10 percent of
that predicted for
the ideal sampler.
B. Solid particles.......... Percent.......... Sampling
effectiveness is no
more than 5 percent
above that obtained
for liquid particles
of same size.
2. 50 Percent cutpoint m....... 10m
aerodynamic
diameter.
3. Precision g/m\3\ 5 g/m\3\ or
or percent. 7 percent for three
collocated samplers.
4. Flow rate stability Percent.......... Average flow rate
over 24 hours within
5
percent of initial
flow rate; all
measured flow rates
over 24 hours within
10
percent of initial
flow rate.
------------------------------------------------------------------------
Sec. 53.41 Test conditions.
(a) Set-up and start-up of all test samplers shall be in strict
accordance with the operating instructions specified in the manual
referred to in Sec. 53.4(b)(3).
(b) If the internal surface or surfaces of the candidate method's
sampler inlet on which the particles removed by the inlet are collected
is a dry surface (i.e., not normally coated with oil or grease), those
surfaces shall be cleaned prior to conducting wind tunnel tests with
solid particles.
(c) Once the test sampler or samplers have been set up and the
performance tests started, manual adjustment shall be permitted only
between test points for the sampling effectiveness and 50 percent
cutpoint tests or between test days for the precision and flow rate
stability tests. The manual adjustments and any periodic maintenance
shall be limited to only those procedures prescribed in the manual
referred to in Sec. 53.4(b)(3). The submitted records shall show clearly
when any manual adjustment or periodic maintenance was made and shall
describe the operations performed.
(d) If a test sampler malfunctions during any of the sampling
effectiveness and 50 percent cutpoint tests, that test run shall be
repeated. If a test sampler malfunctions during any of the precision and
flow rate stability tests, that day's test shall be repeated. A detailed
explanation of all malfunctions and the remedial actions taken shall be
submitted to EPA with the application.
Sec. 53.42 Generation of test atmospheres for wind tunnel tests.
(a) A vibrating orifice aerosol generator shall be used to produce
monodispersed liquid particles of oleic acid tagged with uranine dye and
monodispersed solid particles of ammonium fluoroscein with equivalent
aerodynamic diameters as specified in table D-2. The geometric standard
deviation for each particle size and type generated shall not exceed 1.1
(for primary particles) and the proportion of multiplets (doublets and
triplets) in a test particle atmosphere shall not exceed 10 percent. The
particle delivery system shall consist of a blower system and a wind
tunnel having a test section of sufficiently large cross-sectional area
such that the test sampler, or portion thereof, as installed in the test
section for testing, blocks no more than 15 percent of that area. To be
acceptable, the blower system must be capable of achieving uniform wind
speeds at the speeds specified in table D-2.
Table D-2--Particle Sizes and Wind Speeds for Sampling Effectiveness
Tests
------------------------------------------------------------------------
Wind speed (km/hr)
Particle size (m) a -------------------------------------
2 8 24
------------------------------------------------------------------------
30.5.................. l l l
50.5.................. l l l
70.5.................. l l l
[[Page 50]]
90.5.................. l l l
100.5................. l l l
110.5................. l l l
131.0................. l l l
151.0................. l l l
201.0................. l l l
251.0................. l l/s l/s
------------------------------------------------------------------------
a&thnsp Mass median aerodynamic diameter.
l = liquid particle.
s=solid particle.
Number of liquid particle test points (minimum of 3 replicates for each
combination of particle size and wind speed): 90.
Number of solid particle test points (minimum of 3 replicates for each
combination of particle size and wind speed): 6.
Total number of test points: 96.
(b) The size of the test particles delivered to the test section of
the wind tunnel shall be established using the operating parameters of
the vibrating orifice aerosol generator and shall be verified during the
tests by microscopic examination of samples of the particles collected
on glass slides or other suitable substrates. When sizing liquid
particles on glass slides, the slides should be pretreated with an
oleophobic surfactant and an appropriate flattening factor shall be used
in the calculation of aerodynamic diameter. The particle size, as
established by the operating parameters of the vibrating orifice aerosol
generator, shall be within the tolerance specified in table D-2. The
precision of the particle size verification technique shall be 0.5
m or better, and particle size determined by the verification
technique shall not differ by more than 0.5 m or 10 percent,
whichever is higher, from that established by the operating parameters
of the vibrating orifice aerosol generator.
(c) The population of multiplets in a test particle atmosphere shall
be determined during the tests and shall not exceed 10 percent. Solid
particles shall be checked for dryness and evidence of breakage or
agglomeration during the microscopic examination. If the solid particles
in a test atmosphere are wet or show evidence of significant breakage or
agglomeration (5 percent), the solid particle test atmosphere
is unacceptable for purposes of these tests.
(d) The concentration of particles in the wind tunnel is not
critical. However, the cross-sectional uniformity of the particle
concentration in the sampling zone of the test section shall be
established during the tests using isokinetic samplers. An array of not
less than five evenly spaced isokinetic samplers shall be used to
determine the particle concentration uniformity in the sampling zone. If
the particle concentration measured by any single isokinetic sampler in
the sampling zone differs by more than 10 percent from the mean
concentration, the particle delivery system is unacceptable in terms of
uniformity of particle concentration. The sampling zone shall be a
rectangular area having a horizontal dimension not less than 1.2 times
the width of the test sampler at its inlet opening and a vertical
dimension not less than 25 centimeters. The sampling zone is an area in
the test section of the wind tunnel that is horizontally and vertically
symmetrical with respect to the test sampler inlet opening.
(e) The wind speed in the wind tunnel shall be determined during the
tests using an appropriate technique capable of a precision of 5 percent
or better (e.g., hot-wire anemometry). The mean wind speed in the test
section of the wind tunnel during the tests shall be within 10 percent
of the value specified in table D-2. The wind speed measured at any test
point in the test section shall not differ by more than 10 percent from
the mean wind speed in the test section. The turbulence intensity
(longitudinal component and macroscale) in the test section shall be
determined during the tests using an appropriate technique (e.g., hot-
wire anemometry).
(f) The accuracy of all flow measurements used to calculate the test
atmosphere concentrations and the test results shall be documented to be
within 2 percent, referenced to a primary standard. Any flow
measurement corrections shall be clearly shown. All flow measurements
shall be given in actual volumetric units.
(g) Schematic drawings of the particle delivery system (wind tunnel
and blower system) and other information showing complete procedural
details of the test atmosphere generation, verification, and delivery
techniques
[[Page 51]]
shall be submitted to EPA. All pertinent calculations shall be clearly
presented.
Sec. 53.43 Test procedures.
(a) Sampling effectiveness--(1) Technical definition. The ratio
(expressed as a percentage) of the mass concentration of particles of a
given size reaching the sampler filter or filters to the mass
concentration of particles of the same size approaching the sampler.
(2) Test procedure. (i) Establish a wind speed specified in table D-
2 and measure the wind speed and turbulence intensity (longitudinal
component and macroscale) at a minimum of 12 test points in a cross-
sectional area of the test section of the wind tunnel. The mean wind
speed in the test section must be within 10 percent of the
value specified in table D-2 and the variation at any test point in the
test section may not exceed 10 percent of the mean.
(ii) Generate particles of a size and type specified in table D-2
using a vibrating orifice aerosol generator. Check for the presence of
satellites and adjust the generator as necessary. Calculate the
aerodynamic particle size using the operating parameters of the
vibrating orifice aerosol generator and record. The calculated
aerodynamic diameter must be within the tolerance specified in table D-
2.
(iii) Collect a sample of the particles on a glass slide or other
suitable substrate at the particle injection point. If a glass slide is
used, it should be pretreated with an appropriate oleophobic surfactant
when collecting liquid particles. Use a microscopic technique to size a
minimum of 25 primary particles in three viewing fields (do not include
multiplets). Determine the geometric mean aerodynamic diameter and
geometric standard deviation using the bulk density of the particle type
(and an appropriate flattening factor for liquid particles if collected
on a glass slide). The measured geometric mean aerodynamic diameter must
be within 0.5 m or 10 percent of the aerodynamic diameter
calculated from the operating parameters of the vibrating orifice
aerosol generator. The geometric standard deviation must not exceed 1.1.
(iv) Determine the population of multiplets (doublets and triplets)
in the collected sample by counting a minimum of 100 particles in three
viewing fields. The multiplet population of the particle test atmosphere
must not exceed 10 percent.
(v) Introduce the particles into the wind tunnel and allow the
particle concentration to stabilize.
(vi) Install an array of five or more evenly spaced isokinetic
samplers in the sampling zone (see Sec. 53.42(d)) of the wind tunnel.
Collect particles on appropriate filters (e.g., glass fiber) over a time
period such that the relative error of the measured particle
concentration is less than 5 percent. Relative error is defined as
(p x 100%)/(X), where p is the precision of the fluorometer on the
appropriate range, X is the measured concentration, and the units of p
and X are the same.
(vii) Determine the quantity of material collected with each
isokinetic sampler in the array using a calibrated fluorometer.
Calculate and record the mass concentration for each isokinetic sampler
as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.015
where
i = replicate number and j = isokinetic sampler number.
(viii) Calculate and record the mean mass concentration as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.016
[[Page 52]]
where
n = total number of isokinetic samplers.
(ix) Calculate and record the coefficient of variation of the mass
concentration measurements as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.017
If the value of CViso(i) exceeds 0.10, the particle
concentration uniformity is unacceptable and steps (vi) through (ix)
must be repeated. If adjustment of the vibrating orifice aerosol
generator or changes in the particle delivery system are necessary to
achieve uniformity, steps (ii) through (ix) must be repeated. Remove the
array of isokinetic samplers from the wind tunnel. NOTE: A single
isokinetic sampler, operated at the same nominal flow rate as the test
sampler, may be used in place of the array of isokinetic samplers for
the determination of particle mass concentration used in the calculation
of sampling effectiveness of the test sampler in step (xiii). In this
case, the array of isokinetic samplers must be used to demonstrate
particle concentration uniformity prior to the replicate measurements of
sampling effectiveness.
(x) If a single isokinetic sampler is used, install the sampler in
the wind tunnel with the sampler nozzle centered in the sampling zone
(see Sec. 53.42(d)). Collect particles on an appropriate filter (e.g.,
glass fiber) for a time period such that the relative error of the
measured concentration (as defined in step (vi)) is less than 5 percent.
Determine the quantity of material collected with the isokinetic sampler
using a calibrated fluorometer. Calculate and record the mass
concentration as Ciso(i) as in step vii. Remove the
isokinetic sampler from the wind tunnel.
(xi) Install the test sampler (or portion thereof) in the wind
tunnel with the sampler inlet opening centered in the sampling zone (see
Sec. 53.42(d)). To meet the maximum blockage limit of Sec. 53.42(a) or
for convenience, part of the test sampler may be positioned external to
the wind tunnel provided that neither the geometry of the sampler nor
the length of any connecting tube or pipe is altered. Collect particles
on an appropriate filter or filters (e.g., glass fiber) for a time
period such that the relative error of the measured concentration (as
defined in step (vi)) is less than 5 percent.
(xii) Determine the quantity of material collected with the test
sampler using a calibrated fluorometer. Calculate and record the mass
concentration as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.018
where i=replicate number.
(xiii) Calculate and record the sampling effectiveness of the test
sampler as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.019
where i = replicate number.
Note: If a single isokinetic sampler is used for the determination
of particle mass concentration, replace Ciso(i) with
Ciso(i).
[[Page 53]]
(xiv) Remove the test sampler from the wind tunnel. Repeat steps
(vi) through (xiii), as appropriate, to obtain a minimum of three
replicate measurements of sampling effectiveness.
(xv) Calculate and record the average sampling effectiveness of the
test sampler as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.020
where n=number of replicates.
(xvi) Calculate and record the coefficient of variation for the
replicate sampling effectiveness measurements of the test sampler as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.021
If the value of CVE exceeds 0.10, the test run (steps (ii)
through (xvi)) must be repeated.
(xvii) Repeat steps i through xvi for each wind speed, particle
size, and particle type specified in table D-2.
(xviii) For each of the three wind speeds (nominally 2, 8, and 24
km/hr), correct the liquid particle sampling effectiveness data for the
presence of multiplets (doublets and triplets) in the test particle
atmospheres.
(xix) For each wind speed, plot the corrected liquid particle
sampling effectiveness of the test sampler (Ecorr) as a
function of particle size (dp) on semi-logarithmic graph
paper where dp is the particle size established by the
operating parameters of the vibrating orifice aerosol generator.
Construct a smooth curve through the data.
(xx) For each wind speed, calculate the expected mass concentration
for the test sampler under the assumed particle size distribution and
compare it to the mass concentration predicted for the ideal sampler, as
follows:
(A) Extrapolate the upper and lower ends of the corrected liquid
particle sampling effectiveness curve to 100 percent and 0 percent,
respectively, using smooth curves. Assume that Ecorr = 100
percent at a particle size of 1.0 m and Ecorr = 0
percent at a particle size of 50 m.
(B) Determine the value of Ecorr at each of the particle
sizes specified in the first column of table D-3. Record each
Ecorr value as a decimal between 0 and 1 in the second column
of table D-3.
(C) Multiply the values of Ecorr in column 2 by the
interval mass concentration values in column 3 and enter the products in
column 4 of table D-3.
(D) Sum the values in column 4 and enter the total as the expected
mass concentration for the test sampler at the bottom of column 4 of
table D-3.
(E) Calculate and record the percent difference in expected mass
concentration between the test sampler and the ideal sampler as:
[GRAPHIC] [TIFF OMITTED] TC09NO91.022
where:
Csam(exp) = expected mass concentration for the test sampler,
g/m\3\
Cideal(exp) = expected mass concentration for the ideal
sampler, g/m\3\ (calculated for the ideal sampler and given at
the bottom of column 7 of table D-3.)
(F) The candidate method passes the liquid particle sampling
effectiveness test if the C value for each wind speed meets
the specification in table D-1.
(xxi) For each of the two wind speeds (nominally 8 and 24 km/hr),
calculate the difference between the average sampling effectiveness
value for the 25 m solid particles and the average sampling
effectiveness value for the 25 m liquid particles (uncorrected
for multiplets).
(xxii) The candidate method passes the solid particle sampling
effectiveness test if each such difference meets the specification in
table D-1.
[[Page 54]]
Table D-3--Expected Mass Concentration for PM10 Samplers
--------------------------------------------------------------------------------------------------------------------------------------------------------
Test sampler Ideal Sampler
-----------------------------------------------------------------------------------------------------------------------------------
Particle size (um) Interval mass Expected mass Interval mass Expected mass
Sampling concentration concentration Sampling concentration concentration
effectiveness (g/m\3\) (g/m\3\) effectiveness (g/m\3\) (g/m\3\)
--------------------------------------------------------------------------------------------------------------------------------------------------------
(1) (2) (3) (4) (5) (6) (7)
--------------------------------------------------------------------------------------------------------------------------------------------------------
1.0 1.000 62.813 62.813 1.000 62.813 62.813
1.5 9.554 0.949 9.554 9.067
02.0 2.164 0.942 2.164 2.038
02.5 1.785 0.933 1.785 1.665
03.0 2.084 0.922 2.084 1.921
03.5 2.618 0.909 2.618 2.380
04.0 3.211 0.893 3.211 2.867
04.5 3.784 0.876 3.784 3.315
05.0 4.300 0.857 4.300 3.685
05.5 4.742 0.835 4.742 3.960
06.0 5.105 0.812 5.105 4.145
06.5 5.389 0.786 5.389 4.236
07.0 5.601 0.759 5.601 4.251
07.5 5.746 0.729 5.746 4.189
08.0 5.834 0.697 5.834 4.066
08.5 5.871 0.664 5.871 3.898
09.0 5.864 0.628 5.864 3.683
09.5 5.822 0.590 5.822 3.435
10.0 5.750 0.551 5.750 3.168
10.5 5.653 0.509 5.653 2.877
11.0 8.257 0.465 8.257 3.840
12.0 10.521 0.371 10.521 3.903
13.0 9.902 0.269 9.902 2.664
14.0 9.250 0.159 9.250 1.471
15.0 8.593 0.041 8.593 0.352
16.0 7.948 0.000 7.948 0.000
17.0 7.329 0.000 7.329 0.000
18.0 9.904 0.000 9.904 0.000
20.0 11.366 0.000 11.366 0.000
22.0 9.540 0.000 9.540 0.000
24.0 7.997 0.000 7.997 0.000
26.0 6.704 0.000 6.704 0.000
28.0 5.627 0.000 5.627 0.000
30.0 7.785 0.000 7.785 0.000
35.0 7.800 0.000 7.800 0.000
40.0 5.192 0.000 5.192 0.000
45.0 4.959 0.000 4.959 0.000
Csam(exp) = D Cideal(exp) = 143.889
--------------------------------------------------------------------------------------------------------------------------------------------------------
(b) 50 Percent cutpoint--(1) Technical definition. The particle size
for which the sampling effectiveness of the sampler is 50 percent.
(2) Test procedure. (i) From the corrected liquid particle sampling
effectiveness curves for each of the three wind speeds, determine the
particle size at which the curve crosses the 50 percent effectiveness
line and record as D50 on the corresponding sampling
effectiveness plot.
(ii) The candidate method passes the 50 percent cutpoint test if the
D50 value at each wind speed meets the specification in table
D-1.
(c) Precision--(1) Technical definition. The variation in the
measured particle concentration among identical samplers under typical
sampling conditions.
(2) Test procedure. (i) Set up three identical test samplers at the
test site in strict accordance with the instructions in the manual
referred to in Sec. 53.4(b)(3). Locate the test sampler inlet openings
at the same height and between 2 and 4 meters apart. The samplers shall
be oriented in a manner that will minimize spatial and wind directional
effects on sample collection. Perform a flow calibration for each test
sampler in accordance with the instructions given in the instruction
manual and/or appendix J to part 50 of this chapter. Set the operating
flow rate to the value prescribed in the sampler instruction manual.
[[Page 55]]
Note: For candidate equivalent methods, this test may be used to
satisfy part of the requirements of subpart C of this chapter. In that
case, three reference method samplers are also used at the test site,
measurements with the candidate and reference methods are compared as
specified in Sec. 53.34, and the test site must meet the requirements of
Sec. 53.30(b).
(ii) Measure the PM10 concentration of the atmosphere
using the three test samplers for 10 periods (test days) of 24 hours
each. On each of the 10 test days, measure the initial and final flow
rates of each test sampler. On three of the test days, measure the flow
rate of each test sampler after 6, 12, and 18 hours of operation. All
measurements of flow rate and mass collected must be made in accordance
with the procedures prescribed in the sampler instruction manual and/or
appendix J to part 50 of this chapter. All measurements of flow rate
must be in actual volumetric units. Record the PM10
concentration for each sampler and each test day as C(i)(j)
where i is the sampler number and j is the test day.
(iii) For each test day, calculate and record the average of the
three measured PM10 concentrations as C(j) where j
is the test day. If C(j)30 g/m\3\ for any test day,
data from that test day are unacceptable and the tests for that day must
be repeated.
(iv) Calculate and record the precision for each of the 10 test days
as:
(v) The candidate method passes the precision test if all 10
Pj or RPj values meet the specifications in table
D-1.
(d) Flow rate stability--(1) Technical definition. Freedom from
variation in the operating flow rate of the sampler under typical
sampling conditions.
(2) Test procedure. (i) For each of the three test samplers and each
of the 10 test days of the precision test, record each measured flow
rate as F(i)(j)(t), where i is the sampler number, j is the
test day, and t is the time of flow rate measurement (t=0, 6, 12, 18, or
24 hours).
(ii) For each sampler and for each test day, calculate and record
the average flow rate as:
where n = number of flow rate measurements during the 24-hour test day.
(iii) For each sampler and for each test day, calculate and record
the percent difference between the average flow rate and the initial
flow rate as:
where F(i)(j)(0) is the initial flow rate (t=0).
[[Page 56]]
(iv) For each sampler and for each of the 3 test days on which flow
measurements were obtained at 6-hour intervals throughout the 24-hour
sampling period, calculate and record the percent differences between
each measured flow rate and the initial flow rate as:
where t = 6, 12, 18, or 24 hours.
(v) The candidate method passes the flow rate stability test if all
of the F(i)(j) and F(i)(j)(t)
values meet the specifications in table D-1.
Subpart E--Procedures for Testing Physical (Design) and Performance
Characteristics of Reference Methods and Class I Equivalent Methods for
PM2.5
Source: 62 FR 38799, July 18, 1997, unless otherwise noted.
Sec. 53.50 General provisions.
(a) This subpart sets forth the specific tests that must be carried
out and the test results, evidence, documentation, and other materials
that must be provided to EPA to demonstrate that a PM2.5
sampler associated with a candidate reference method or Class I
equivalent method meets all design and performance specifications set
forth in 40 CFR part 50, appendix L, as well as additional requirements
specified in this subpart E. Some of these tests may also be applicable
to portions of a candidate Class II equivalent method sampler, as
determined under subpart F of this part. Some or all of these tests may
also be applicable to a candidate Class III equivalent method sampler,
as may be determined under Sec. 53.3(a)(4) or Sec. 53.3(b)(3).
(b) Samplers associated with candidate reference methods for
PM2.5 shall be subject to the provisions, specifications, and
test procedures prescribed in Secs. 53.51 through 53.58. Samplers
associated with candidate Class I equivalent methods for
PM2.5 shall be subject to the provisions, specifications, and
test procedures prescribed in all sections of this subpart. Samplers
associated with candidate Class II equivalent methods for
PM2.5 shall be subject to the provisions, specifications, and
test procedures prescribed in all applicable sections of this subpart,
as specified in subpart F of this part.
(c) The provisions of Sec. 53.51 pertain to test results and
documentation required to demonstrate compliance of a candidate method
sampler with the design specifications set forth in 40 CFR part 50,
appendix L. The test procedures prescribed in Secs. 53.52 through 53.59
pertain to performance tests required to demonstrate compliance of a
candidate method sampler with the performance specifications set forth
in 40 CFR part 50, appendix L, as well as additional requirements
specified in this subpart E. These latter test procedures shall be used
to test the performance of candidate samplers against the performance
specifications and requirements specified in each procedure and
summarized in table E-1 of this subpart.
(d) Test procedures prescribed in Sec. 53.59 do not apply to
candidate reference method samplers. These procedures apply primarily to
candidate Class I equivalent method samplers for PM2.5 which
have a sample air flow path configuration upstream of the sample filter
that is modified with respect to that specified for the reference method
sampler, as set forth in 40 CFR part 50, appendix L, figures L-1 to L-
29, such as might be necessary to provide for sequential sample
capability. The additional tests determine the adequacy of aerosol
transport through any altered components or supplemental devices that
are used in a candidate sampler upstream of the sample filter. In
addition to the other test procedures in this subpart, these test
procedures shall be used to further test the performance of such an
equivalent method sampler against the performance specifications given
in the procedure and summarized in table E-1 of this subpart.
(e) A 10-day operational field test of measurement precision is
required under Sec. 53.58 for both candidate reference and equivalent
method samplers. This test requires collocated operation of three
candidate method samplers at a field test site. For candidate
[[Page 57]]
equivalent method samplers, this test may be combined and carried out
concurrently with the test for comparability to the reference method
specified under Sec. 53.34, which requires collocated operation of three
reference method samplers and three candidate equivalent method
samplers.
(f) All tests and collection of test data shall be performed in
accordance with the requirements of reference 1, section 4.10.5 (ISO
9001) and reference 2, part B, section 3.3.1, paragraphs 1 and 2 and
part C, section 4.6 (ANSI/ASQC E4) in appendix A of this subpart. All
test data and other documentation obtained specifically from or
pertinent to these tests shall be identified, dated, signed by the
analyst performing the test, and submitted to EPA in accordance with
subpart A of this part.
Sec. 53.51 Demonstration of compliance with design specifications and manufacturing and test requirements.
(a) Overview. (1) The subsequent paragraphs of this section specify
certain documentation that must be submitted and tests that are required
to demonstrate that samplers associated with a designated reference or
equivalent method for PM2.5 are properly manufactured to meet
all applicable design and performance specifications and have been
properly tested according to all applicable test requirements for such
designation. Documentation is required to show that instruments and
components of a PM2.5 sampler are manufactured in an ISO
9001-registered facility under a quality system that meets ISO-9001
requirements for manufacturing quality control and testing.
(2) In addition, specific tests are required to verify that two
critical features of reference method samplers impactor jet diameter and
the surface finish of surfaces specified to be anodized meet the
specifications of 40 CFR part 50, appendix L. A checklist is required to
provide certification by an ISO-certified auditor that all performance
and other required tests have been properly and appropriately conducted,
based on a reasonable and appropriate sample of the actual operations or
their documented records. Following designation of the method, another
checklist is required, initially and annually, to provide an ISO-
certified auditor's certification that the sampler manufacturing process
is being implemented under an adequate and appropriate quality system.
(3) For the purposes of this section, the definitions of ISO 9001-
registered facility and ISO-certified auditor are found in Sec. 53.1. An
exception to the reliance by EPA on ISO-certified auditors is the
requirement for the submission of the operation or instruction manual
associated with the candidate method to EPA as part of the application.
This manual is required under Sec. 53.4(b)(3). EPA has determined that
acceptable technical judgment for review of this manual may not be
assured by ISO-certified auditors, and approval of this manual will
therefore be performed by EPA.
(b) ISO registration of manufacturing facility. (1) The applicant
must submit documentation verifying that the samplers identified and
sold as part of a designated PM2.5 reference or equivalent
method will be manufactured in an ISO 9001-registered facility and that
the manufacturing facility is maintained in compliance with all
applicable ISO 9001 requirements (reference 1 in appendix A of this
subpart). The documentation shall indicate the date of the original ISO
9001 registration for the facility and shall include a copy of the most
recent certification of continued ISO 9001 facility registration. If the
manufacturer does not wish to initiate or complete ISO 9001 registration
for the manufacturing facility, documentation must be included in the
application to EPA describing an alternative method to demonstrate that
the facility meets the same general requirements as required for
registration to ISO-9001. In this case, the applicant must provide
documentation in the application to demonstrate, by required ISO-
certified auditor's inspections, that a quality system is in place which
is adequate to document and monitor that the sampler system components
and final assembled samplers all conform to the design, performance and
other requirements specified in this part and in 40 CFR part 50,
appendix L.
(2) Phase-in period. For a period of 1 year following the effective
date of this
[[Page 58]]
subpart, a candidate reference or equivalent method for PM2.5
that utilizes a sampler manufactured in a facility that is not ISO 9001-
registered or otherwise approved by EPA under paragraph (b)(1) of this
section may be conditionally designated as a reference or equivalent
method under this part. Such conditional designation will be considered
on the basis of evidence submitted in association with the candidate
method application showing that appropriate efforts are currently
underway to seek ISO 9001 registration or alternative approval of the
facility's quality system under paragraph (b)(1) of this section within
the next 12 months. Such conditional designation shall expire 1 year
after the date of the Federal Register notice of the conditional
designation unless documentation verifying successful ISO 9001
registration for the facility or other EPA-acceptable quality system
review and approval process of the production facility that will
manufacture the samplers is submitted at least 30 days prior to the
expiration date.
(c) Sampler manufacturing quality control. The manufacturer must
ensure that all components used in the manufacture of PM2.5
samplers to be sold as part of a reference or equivalent method and that
are specified by design in 40 CFR part 50, appendix L, are fabricated or
manufactured exactly as specified. If the manufacturer's quality records
show that its quality control (QC) and quality assurance (QA) system of
standard process control inspections (of a set number and frequency of
testing that is less than 100 percent) complies with the applicable QA
provisions of section 4 of reference 4 in appendix A of this subpart and
prevents nonconformances, 100 percent testing shall not be required
until that conclusion is disproved by customer return or other
independent manufacturer or customer test records. If problems are
uncovered, inspection to verify conformance to the drawings,
specifications, and tolerances shall be performed. Refer also to
paragraph (e) of this section--final assembly and inspection
requirements.
(d) Specific tests and supporting documentation required to verify
conformance to critical component specifications--(1) Verification of
PM2.5 impactor jet diameter. The diameter of the jet of each
impactor manufactured for a PM2.5 sampler under the impactor
design specifications set forth in 40 CFR part 50, appendix L, shall be
verified against the tolerance specified on the drawing, using standard,
NIST-traceable ZZ go/no go plug gages. This test shall be a final check
of the jet diameter following all fabrication operations, and a record
shall be kept of this final check. The manufacturer shall submit
evidence that this procedure is incorporated into the manufacturing
procedure, that the test is or will be routinely implemented, and that
an appropriate procedure is in place for the disposition of units that
fail this tolerance test.
(2) Verification of surface finish. The anodization process used to
treat surfaces specified to be anodized shall be verified by testing
treated specimen surfaces for weight and corrosion resistance to ensure
that the coating obtained conforms to the coating specification. The
specimen surfaces shall be finished in accordance with military standard
specification 8625F, Type II, Class I (reference 4 in appendix A of this
subpart) in the same way the sampler surfaces are finished, and tested,
prior to sealing, as specified in section 4.5.2 of reference 4 in
appendix A of this subpart.
(e) Final assembly and inspection requirements. Each sampler shall
be tested after manufacture and before delivery to the final user. Each
manufacturer shall document its post-manufacturing test procedures. As a
minimum, each test shall consist of the following: Tests of the overall
integrity of the sampler, including leak tests; calibration or
verification of the calibration of the flow measurement device,
barometric pressure sensor, and temperature sensors; and operation of
the sampler with a filter in place over a period of at least 48 hours.
The results of each test shall be suitably documented and shall be
subject to review by an ISO-certified auditor.
(f) Manufacturer's audit checklists. Manufacturers shall require an
ISO-certified auditor to sign and date a statement indicating that the
auditor
[[Page 59]]
is aware of the appropriate manufacturing specifications contained in 40
CFR part 50, appendix L, and the test or verification requirements in
this subpart. Manufacturers shall also require an ISO-certified auditor
to complete the checklists, shown in figures E-1 and E-2 of this
subpart, which describe the manufacturer's ability to meet the
requirements of the standard for both designation testing and product
manufacture.
(1) Designation testing checklist. The completed statement and
checklist as shown in figure E-1 of this subpart shall be submitted with
the application for reference or equivalent method determination.
(2) Product manufacturing checklist. Manufacturers shall require an
ISO-certified auditor to complete a Product Manufacturing Checklist
(figure E-2 of this subpart), which evaluates the manufacturer on its
ability to meet the requirements of the standard in maintaining quality
control in the production of reference or equivalent devices. The
initial completed checklist shall be submitted with the application for
reference or equivalent method determination. Also, this checklist
(figure E-2 of this subpart) must be completed and submitted annually to
retain a reference or equivalent method designation for a
PM2.5 method.
(3) Phase-in period. If the conditions of paragraph (b)(2) of this
section apply, a candidate reference or equivalent method for
PM2.5 may be conditionally designated as a reference or
equivalent method under this part 53 without the submission of the
checklists described in paragraphs (f)(1) and (f)(2) of this section.
Such conditional designation shall expire 1 year after the date of the
Federal Register notice of the conditional designation unless the
checklists are submitted at least 30 days prior to the expiration date.
[62 FR 38799, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Sec. 53.52 Leak check test.
(a) Overview. In section 7.4.6 of 40 CFR part 50, appendix L, the
sampler is required to include the facility, including components,
instruments, operator controls, a written procedure, and other
capabilities as necessary, to allow the operator to carry out a leak
test of the sampler at a field monitoring site without additional
equipment. This test procedure is intended to test the adequacy and
effectiveness of the sampler's leak check facility. Because of the
variety of potential sampler configurations and leak check procedures
possible, some adaptation of this procedure may be necessary to
accommodate the specific sampler under test. The test conditions and
performance specifications associated with this test are summarized in
table E-1 of this subpart. The candidate test sampler must meet all test
parameters and test specifications to successfully pass this test.
(b) Technical definitions. (1) External leakage includes the total
flow rate of external ambient air which enters the sampler other than
through the sampler inlet and which passes through any one or more of
the impactor, filter, or flow rate measurement components.
(2) Internal leakage is the total sample air flow rate that passes
through the filter holder assembly without passing through the sample
filter.
(c) Required test equipment. (1) Flow rate measurement device, range
70 mL/min to 130 mL/min, 2 percent certified accuracy, NIST-traceable.
(2) Flow rate measurement adaptor (40 CFR part 50, appendix L,
figure L-30) or equivalent adaptor to facilitate measurement of sampler
flow rate at the top of the downtube.
(3) Impermeable membrane or disk, 47 mm nominal diameter.
(4) Means, such as a micro-valve, of providing a simulated leak flow
rate through the sampler of approximately 80 mL/min under the conditions
specified for the leak check in the sampler's leak check procedure.
(5) Teflon sample filter, as specified in section 6 of 40 CFR part
50, appendix L.
(d) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests. The accuracy
of flow rate meters shall be verified at the highest and lowest
[[Page 60]]
pressures and temperatures used in the tests and shall be checked at
zero and one or more non-zero flow rates within 7 days of use for this
test.
(e) Test setup. (1) The test sampler shall be set up for testing as
described in the sampler's operation or instruction manual referred to
in Sec. 53.4(b)(3). The sampler shall be installed upright and set up in
its normal configuration for collecting PM2.5 samples, except
that the sample air inlet shall be removed and the flow rate measurement
adaptor shall be installed on the sampler's downtube.
(2) The flow rate control device shall be set up to provide a
constant, controlled flow rate of 80 mL/min into the sampler downtube
under the conditions specified for the leak check in the sampler's leak
check procedure.
(3) The flow rate measurement device shall be set up to measure the
controlled flow rate of 80 mL/min into the sampler downtube under the
conditions specified for the leak check in the sampler's leak check
procedure.
(f) Procedure. (1) Install the impermeable membrane in a filter
cassette and install the cassette into the sampler. Carry out the
internal leak check procedure as described in the sampler's operation/
instruction manual and verify that the leak check acceptance criterion
specified in table E-1 of this subpart is met.
(2) Replace the impermeable membrane with a Teflon filter and
install the cassette in the sampler. Remove the inlet from the sampler
and install the flow measurement adaptor on the sampler's downtube.
Close the valve of the adaptor to seal the flow system. Conduct the
external leak check procedure as described in the sampler's operation/
instruction manual and verify that the leak check acceptance criteria
specified in table E-1 of this subpart are met.
(3) Arrange the flow control device, flow rate measurement device,
and other apparatus as necessary to provide a simulated leak flow rate
of 80 mL/min into the test sampler through the downtube during the
specified external leak check procedure. Carry out the external leak
check procedure as described in the sampler's operation/instruction
manual but with the simulated leak of 80 mL/min.
(g) Test results. The requirements for successful passage of this
test are:
(1) That the leak check procedure indicates no significant external
or internal leaks in the test sampler when no simulated leaks are
introduced.
(2) That the leak check procedure properly identifies the occurrence
of the simulated external leak of 80 mL/min.
Sec. 53.53 Test for flow rate accuracy, regulation, measurement accuracy, and cut-off.
(a) Overview. This test procedure is designed to evaluate a
candidate sampler's flow rate accuracy with respect to the design flow
rate, flow rate regulation, flow rate measurement accuracy, coefficient
of variability measurement accuracy, and the flow rate cut-off function.
The tests for the first four parameters shall be conducted over a 6-hour
time period during which reference flow measurements are made at
intervals not to exceed 5 minutes. The flow rate cut-off test, conducted
separately, is intended to verify that the sampler carries out the
required automatic sample flow rate cut-off function properly in the
event of a low-flow condition. The test conditions and performance
specifications associated with this test are summarized in table E-1 of
this subpart. The candidate test sampler must meet all test parameters
and test specifications to successfully pass this test.
(b) Technical definitions. (1) Sample flow rate means the
quantitative volumetric flow rate of the air stream caused by the
sampler to enter the sampler inlet and pass through the sample filter,
measured in actual volume units at the temperature and pressure of the
air as it enters the inlet.
(2) The flow rate cut-off function requires the sampler to
automatically stop sample flow and terminate the current sample
collection if the sample flow rate deviates by more than the variation
limits specified in table E-1 of this subpart (10 percent
from the nominal sample flow rate) for more than 60 seconds during a
sample collection period. The sampler is also required to properly
notify the operator
[[Page 61]]
with a flag warning indication of the out-of-specification flow rate
condition and if the flow rate cut-off results in an elapsed sample
collection time of less than 23 hours.
(c) Required test equipment. (1) Flow rate meter, suitable for
measuring and recording the actual volumetric sample flow rate at the
sampler downtube, with a minimum range of 10 to 25 L/min, 2 percent
certified, NIST-traceable accuracy. Optional capability for continuous
(analog) recording capability or digital recording at intervals not to
exceed 30 seconds is recommended. While a flow meter which provides a
direct indication of volumetric flow rate is preferred for this test, an
alternative certified flow measurement device may be used as long as
appropriate volumetric flow rate corrections are made based on
measurements of actual ambient temperature and pressure conditions.
(2) Ambient air temperature sensor, with a resolution of 0.1 deg.C
and certified to be accurate to within 0.5 deg.C (if needed). If the
certified flow meter does not provide direct volumetric flow rate
readings, ambient air temperature measurements must be made using
continuous (analog) recording capability or digital recording at
intervals not to exceed 5 minutes.
(3) Barometer, range 600 mm Hg to 800 mm Hg, certified accurate to 2
mm Hg (if needed). If the certified flow meter does not provide direct
volumetric flow rate readings, ambient pressure measurements must be
made using continuous (analog) recording capability or digital recording
at intervals not to exceed 5 minutes.
(4) Flow measurement adaptor (40 CFR part 50, appendix L, figure L-
30) or equivalent adaptor to facilitate measurement of sample flow rate
at the sampler downtube.
(5) Valve or other means to restrict or reduce the sample flow rate
to a value at least 10 percent below the design flow rate (16.67 L/min).
If appropriate, the valve of the flow measurement adaptor may be used
for this purpose.
(6) Means for creating an additional pressure drop of 55 mm Hg in
the sampler to simulate a heavily loaded filter, such as an orifice or
flow restrictive plate installed in the filter holder or a valve or
other flow restrictor temporarily installed in the flow path near the
filter.
(7) Teflon sample filter, as specified in section 6 of 40 CFR part
50, appendix L (if required).
(d) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests. The accuracy
of flow-rate meters shall be verified at the highest and lowest
pressures and temperatures used in the tests and shall be checked at
zero and at least one flow rate within 3 percent of 16.7 L/
min within 7 days prior to use for this test. Where an instrument's
measurements are to be recorded with an analog recording device, the
accuracy of the entire instrument-recorder system shall be calibrated or
verified.
(e) Test setup. (1) Setup of the sampler shall be as required in
this paragraph (e) and otherwise as described in the sampler's operation
or instruction manual referred to in Sec. 53.4(b)(3). The sampler shall
be installed upright and set up in its normal configuration for
collecting PM2.5 samples. A sample filter and (or) the device
for creating an additional 55 mm Hg pressure drop shall be installed for
the duration of these tests. The sampler's ambient temperature, ambient
pressure, and flow rate measurement systems shall all be calibrated per
the sampler's operation or instruction manual within 7 days prior to
this test.
(2) The inlet of the candidate sampler shall be removed and the flow
measurement adaptor installed on the sampler's downtube. A leak check as
described in the sampler's operation or instruction manual shall be
conducted and must be properly passed before other tests are carried
out.
(3) The inlet of the flow measurement adaptor shall be connected to
the outlet of the flow rate meter.
(4) For the flow rate cut-off test, the valve or means for reducing
sampler flow rate shall be installed between the flow measurement
adaptor and the downtube or in another location within the sampler such
that the sampler flow
[[Page 62]]
rate can be manually restricted during the test.
(f) Procedure. (1) Set up the sampler as specified in paragraph (e)
of this section and otherwise prepare the sampler for normal sample
collection operation as directed in the sampler's operation or
instruction manual. Set the sampler to automatically start a 6-hour
sample collection period at a convenient time.
(2) During the 6-hour operational flow rate portion of the test,
measure and record the sample flow rate with the flow rate meter at
intervals not to exceed 5 minutes. If ambient temperature and pressure
corrections are necessary to calculate volumetric flow rate, ambient
temperature and pressure shall be measured at the same frequency as that
of the certified flow rate measurements. Note and record the actual
start and stop times for the 6-hour flow rate test period.
(3) Following completion of the 6-hour flow rate test period,
install the flow rate reduction device and change the sampler flow rate
recording frequency to intervals of not more than 30 seconds. Reset the
sampler to start a new sample collection period. Manually restrict the
sampler flow rate such that the sampler flow rate is decreased slowly
over several minutes to a flow rate slightly less than the flow rate
cut-off value (15.0 L/min). Maintain this flow rate for at least 2.0
minutes or until the sampler stops the sample flow automatically.
Manually terminate the sample period, if the sampler has not terminated
it automatically.
(g) Test results. At the completion of the test, validate the test
conditions and determine the test results as follows:
(1) Mean sample flow rate. (i) From the certified measurements
(Qref) of the test sampler flow rate obtained by use of the
flow rate meter, tabulate each flow rate measurement in units of L/min.
If ambient temperature and pressure corrections are necessary to
calculate volumetric flow rate, each measured flow rate shall be
corrected using its corresponding temperature and pressure measurement
values. Calculate the mean flow rate for the sample period
(Qref,ave) as follows:
Equation 1
[GRAPHIC] [TIFF OMITTED] TR18JY97.063
where:
n equals the number of discrete certified flow rate measurements over
the 6-hour test period.
(ii)(A) Calculate the percent difference between this mean flow rate
value and the design value of 16.67 L/min, as follows:
Equation 2
[GRAPHIC] [TIFF OMITTED] TR18JY97.064
(B) To successfully pass the mean flow rate test, the percent
difference calculated in Equation 2 of this paragraph (g)(1)(ii) must be
within 5 percent.
(2) Sample flow rate regulation. (i) From the certified measurements
of the test sampler flow rate, calculate the sample coefficient of
variation (CV) of the discrete measurements as follows:
Equation 3
[GRAPHIC] [TIFF OMITTED] TR18JY97.065
(ii) To successfully pass the flow rate regulation test, the
calculated coefficient of variation for the certified flow rates must
not exceed 2 percent.
(3) Flow rate measurement accuracy. (i) Using the mean volumetric
flow rate reported by the candidate test sampler at the completion of
the 6-hour test period (Qind,ave), determine the accuracy of
the reported mean flow rate as:
Equation 4
[GRAPHIC] [TIFF OMITTED] TR18JY97.066
(ii) To successfully pass the flow rate measurement accuracy test,
the percent difference calculated in Equation
[[Page 63]]
4 of this paragraph (g)(3) shall not exceed 2 percent.
(4) Flow rate coefficient of variation measurement accuracy. (i)
Using the flow rate coefficient of variation indicated by the candidate
test sampler at the completion of the 6-hour test (%CVind),
determine the accuracy of this reported coefficient of variation as:
Equation 5
[GRAPHIC] [TIFF OMITTED] TR18JY97.067
(ii) To successfully pass the flow rate CV measurement accuracy
test, the absolute difference in values calculated in Equation 5 of this
paragraph (g)(4) must not exceed 0.3 (CV%).
(5) Flow rate cut-off. (i) Inspect the measurements of the sample
flow rate during the flow rate cut-off test and determine the time at
which the sample flow rate decreased to a value less than the cut-off
value specified in table E-1 of this subpart. To pass this test, the
sampler must have automatically stopped the sample flow at least 30
seconds but not more than 90 seconds after the time at which the sampler
flow rate was determined to have decreased to a value less than the cut-
off value.
(ii) At the completion of the flow rate cut-off test, download the
archived data from the test sampler and verify that the sampler's
required Flow-out-of-spec and Incorrect sample period flag indicators
are properly set.
Sec. 53.54 Test for proper sampler operation following power interruptions.
(a) Overview. (1) This test procedure is designed to test certain
performance parameters of the candidate sampler during a test period in
which power interruptions of various duration occur. The performance
parameters tested are:
(i) Proper flow rate performance of the sampler.
(ii) Accuracy of the sampler's average flow rate, CV, and sample
volume measurements.
(iii) Accuracy of the sampler's reported elapsed sampling time.
(iv) Accuracy of the reported time and duration of power
interruptions.
(2) This test shall be conducted during operation of the test
sampler over a continuous 6-hour test period during which the sampler's
flow rate shall be measured and recorded at intervals not to exceed 5
minutes. The performance parameters tested under this procedure, the
corresponding minimum performance specifications, and the applicable
test conditions are summarized in table E-1 of this subpart. Each
performance parameter tested, as described or determined in the test
procedure, must meet or exceed the associated performance specification
to successfully pass this test.
(b) Required test equipment. (1) Flow rate meter, suitable for
measuring and recording the actual volumetric sample flow rate at the
sampler downtube, with a minimum range of 10 to 25 L/min, 2 percent
certified, NIST-traceable accuracy. Optional capability for continuous
(analog) recording capability or digital recording at intervals not to
exceed 5 minutes is recommended. While a flow meter which provides a
direct indication of volumetric flow rate is preferred for this test, an
alternative certified flow measurement device may be used as long as
appropriate volumetric flow rate corrections are made based on
measurements of actual ambient temperature and pressure conditions.
(2) Ambient air temperature sensor (if needed for volumetric
corrections to flow rate measurements), with a resolution of 0.1 deg.C,
certified accurate to within 0.5 deg.C, and continuous (analog)
recording capability or digital recording at intervals not to exceed 5
minutes.
(3) Barometer (if needed for volumetric corrections to flow rate
measurements), range 600 mm Hg to 800 mm Hg, certified accurate to 2 mm
Hg, with continuous (analog) recording capability or digital recording
at intervals not to exceed 5 minutes.
(4) Flow measurement adaptor (40 CFR part 50, appendix L, figure L-
30) or equivalent adaptor to facilitate measurement of sample flow rate
at the sampler downtube.
(5) Means for creating an additional pressure drop of 55 mm Hg in
the sampler to simulate a heavily loaded filter, such as an orifice or
flow restrictive
[[Page 64]]
plate installed in the filter holder or a valve or other flow restrictor
temporarily installed in the flow path near the filter.
(6) Teflon sample filter, as specified in section 6 of 40 CFR part
50, appendix L (if required).
(7) Time measurement system, accurate to within 10 seconds per day.
(c) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests. The accuracy
of flow rate meters shall be verified at the highest and lowest
pressures and temperatures used in the tests and shall be checked at
zero and at least one flow rate within 3 percent of 16.7 L/
min within 7 days prior to use for this test. Where an instrument's
measurements are to be recorded with an analog recording device, the
accuracy of the entire instrument-recorder system shall be calibrated or
verified.
(d) Test setup. (1) Setup of the sampler shall be performed as
required in this paragraph (d) and otherwise as described in the
sampler's operation or instruction manual referred to in
Sec. 53.4(b)(3). The sampler shall be installed upright and set up in
its normal configuration for collecting PM2.5 samples. A
sample filter and (or) the device for creating an additional 55 mm Hg
pressure drop shall be installed for the duration of these tests. The
sampler's ambient temperature, ambient pressure, and flow measurement
systems shall all be calibrated per the sampler's operating manual
within 7 days prior to this test.
(2) The inlet of the candidate sampler shall be removed and the flow
measurement adaptor installed on the sample downtube. A leak check as
described in the sampler's operation or instruction manual shall be
conducted and must be properly passed before other tests are carried
out.
(3) The inlet of the flow measurement adaptor shall be connected to
the outlet of the flow rate meter.
(e) Procedure. (1) Set up the sampler as specified in paragraph (d)
of this section and otherwise prepare the sampler for normal sample
collection operation as directed in the sampler's operation or
instruction manual. Set the sampler to automatically start a 6-hour
sample collection period at a convenient time.
(2) During the entire 6-hour operational flow rate portion of the
test, measure and record the sample flow rate with the flow rate meter
at intervals not to exceed 5 minutes. If ambient temperature and
pressure corrections are necessary to calculate volumetric flow rate,
ambient temperature and pressure shall be measured at the same frequency
as that of the certified flow rate measurements. Note and record the
actual start and stop times for the 6-hour flow rate test period.
(3) During the 6-hour test period, interrupt the AC line electrical
power to the sampler 5 times, with durations of 20 seconds, 40 seconds,
2 minutes, 7 minutes, and 20 minutes (respectively), with not less than
10 minutes of normal electrical power supplied between each power
interruption. Record the hour and minute and duration of each power
interruption.
(4) At the end of the test, terminate the sample period (if not
automatically terminated by the sampler) and download all archived
instrument data from the test sampler.
(f) Test results. At the completion of the sampling period, validate
the test conditions and determine the test results as follows:
(1) Mean sample flow rate. (i) From the certified measurements
(Qref) of the test sampler flow rate, tabulate each flow rate
measurement in units of L/min. If ambient temperature and pressure
corrections are necessary to calculate volumetric flow rate, each
measured flow rate shall be corrected using its corresponding
temperature and pressure measurement values. Calculate the mean flow
rate for the sample period (Qref,ave) as follows:
Equation 6
[GRAPHIC] [TIFF OMITTED] TR18JY97.068
where:
n equals the number of discrete certified flow rate measurements over
the 6-hour
[[Page 65]]
test period, excluding flow rate values obtained during periods of power
interruption.
(ii)(A) Calculate the percent difference between this mean flow rate
value and the design value of 16.67 L/min, as follows:
Equation 7
[GRAPHIC] [TIFF OMITTED] TR18JY97.069
(B) To successfully pass this test, the percent difference
calculated in Equation 7 of this paragraph (f)(1)(ii) must be within
5 percent.
(2) Sample flow rate regulation. (i) From the certified measurements
of the test sampler flow rate, calculate the sample coefficient of
variation of the discrete measurements as follows:
Equation 8
[GRAPHIC] [TIFF OMITTED] TR18JY97.070
(ii) To successfully pass this test, the calculated coefficient of
variation for the certified flow rates must not exceed 2 percent.
(3) Flow rate measurement accuracy. (i) Using the mean volumetric
flow rate reported by the candidate test sampler at the completion of
the 6-hour test (Qind,ave), determine the accuracy of the
reported mean flow rate as:
Equation 9
[GRAPHIC] [TIFF OMITTED] TR18JY97.071
(ii) To successfully pass this test, the percent difference
calculated in Equation 9 of this paragraph (f)(3) shall not exceed 2
percent.
(4) Flow rate CV measurement accuracy. (i) Using the flow rate
coefficient of variation indicated by the candidate test sampler at the
completion of the 6-hour test (%CVind), determine the
accuracy of the reported coefficient of variation as:
Equation 10
[GRAPHIC] [TIFF OMITTED] TR18JY97.072
(ii) To successfully pass this test, the absolute difference in
values calculated in Equation 10 of this paragraph (f)(4) must not
exceed 0.3 (CV%).
(5) Verify that the sampler properly provided a record and visual
display of the correct year, month, day-of-month, hour, and minute with
an accuracy of 2 minutes, of the start of each power
interruption of duration greater than 60 seconds.
(6) Calculate the actual elapsed sample time, excluding the periods
of electrical power interruption. Verify that the elapsed sample time
reported by the sampler is accurate to within 20 seconds for
the 6-hour test run.
(7) Calculate the sample volume as Qref.ave multiplied by
the sample time, excluding periods of power interruption. Verify that
the sample volume reported by the sampler is within 2 percent of the
calculated sample volume to successfully pass this test.
(8) Inspect the downloaded instrument data from the test sampler and
verify that all data are consistent with normal operation of the
sampler.
[62 FR 38799, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Sec. 53.55 Test for effect of variations in power line voltage and ambient temperature.
(a) Overview. (1) This test procedure is a combined procedure to
test various performance parameters under variations in power line
voltage and ambient temperature. Tests shall be conducted in a
temperature controlled environment over four 6-hour time periods during
which reference temperature and flow rate measurements shall be made at
intervals not to exceed 5 minutes. Specific parameters to be evaluated
at line voltages of 105 and 125 volts and temperatures of -20 deg.C and
=40 deg.C are as follows:
(i) Sample flow rate.
(ii) Flow rate regulation.
(iii) Flow rate measurement accuracy.
(iv) Coefficient of variability measurement accuracy.
[[Page 66]]
(v) Ambient air temperature measurement accuracy.
(vi) Proper operation of the sampler when exposed to power line
voltage and ambient temperature extremes.
(2) The performance parameters tested under this procedure, the
corresponding minimum performance specifications, and the applicable
test conditions are summarized in table E-1 of this subpart. Each
performance parameter tested, as described or determined in the test
procedure, must meet or exceed the associated performance specification
given. The candidate sampler must meet all specifications for the
associated PM2.5 method to pass this test procedure.
(b) Technical definition. Sample flow rate means the quantitative
volumetric flow rate of the air stream caused by the sampler to enter
the sampler inlet and pass through the sample filter, measured in actual
volume units at the temperature and pressure of the air as it enters the
inlet.
(c) Required test equipment. (1) Environmental chamber or other
temperature-controlled environment or environments, capable of obtaining
and maintaining temperatures at -20 deg.C and =40 deg.C as required
for the test with an accuracy of 2 deg.C. The test
environment(s) must be capable of maintaining these temperatures within
the specified limits continuously with the additional heat load of the
operating test sampler in the environment. Henceforth, where the test
procedures specify a test or environmental ``chamber,'' an alternative
temperature-controlled environmental area or areas may be substituted,
provided the required test temperatures and all other test requirements
are met.
(2) Variable voltage AC power transformer, range 100 Vac to 130 Vac,
with sufficient current capacity to operate the test sampler
continuously under the test conditions.
(3) Flow rate meter, suitable for measuring and recording the actual
volumetric sample flow rate at the sampler downtube, with a minimum
range of 10 to 25 actual L/min, 2 percent certified, NIST-traceable
accuracy. Optional capability for continuous (analog) recording
capability or digital recording at intervals not to exceed 5 minutes is
recommended. While a flow meter which provides a direct indication of
volumetric flow rate is preferred for this test, an alternative
certified flow measurement device may be used as long as appropriate
volumetric flow rate corrections are made based on measurements of
actual ambient temperature and pressure conditions.
(4) Ambient air temperature recorder, range -30 deg.C to =50
deg.C, with a resolution of 0.1 deg.C and certified accurate to within
0.5 deg.C. Ambient air temperature measurements must be made using
continuous (analog) recording capability or digital recording at
intervals not to exceed 5 minutes.
(5) Barometer, range 600 mm Hg to 800 mm Hg, certified accurate to 2
mm Hg. If the certified flow rate meter does not provide direct
volumetric flow rate readings, ambient pressure measurements must be
made using continuous (analog) recording capability or digital recording
at intervals not to exceed 5 minutes.
(6) Flow measurement adaptor (40 CFR part 50, appendix L, figure L-
30) or equivalent adaptor to facilitate measurement of sampler flow rate
at the sampler downtube.
(7) Means for creating an additional pressure drop of 55 mm Hg in
the sampler to simulate a heavily loaded filter, such as an orifice or
flow restrictive plate installed in the filter holder or a valve or
other flow restrictor temporarily installed in the flow path near the
filter.
(8) AC RMS voltmeter, accurate to 1.0 volt.
(9) Teflon sample filter, as specified in section 6 of 40 CFR part
50, appendix L (if required).
(d) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests. The accuracy
of flow rate meters shall be verified at the highest and lowest
pressures and temperatures used in the tests and shall be checked at
zero and at least one flow rate within 3 percent of 16.7 L/
min within 7 days prior to use for this test. Where an instrument's
[[Page 67]]
measurements are to be recorded with an analog recording device, the
accuracy of the entire instrument-recorder system shall be calibrated or
verified.
(e) Test setup. (1) Setup of the sampler shall be performed as
required in this paragraph (e) and otherwise as described in the
sampler's operation or instruction manual referred to in
Sec. 53.4(b)(3). The sampler shall be installed upright and set up in
the temperature-controlled chamber in its normal configuration for
collecting PM2.5 samples. A sample filter and (or) the device
for creating an additional 55 mm Hg pressure drop shall be installed for
the duration of these tests. The sampler's ambient temperature, ambient
pressure, and flow measurement systems shall all be calibrated per the
sampler's operating manual within 7 days prior to this test.
(2) The inlet of the candidate sampler shall be removed and the flow
measurement adaptor installed on the sampler's downtube. A leak check as
described in the sampler's operation or instruction manual shall be
conducted and must be properly passed before other tests are carried
out.
(3) The inlet of the flow measurement adaptor shall be connected to
the outlet of the flow rate meter.
(4) The ambient air temperature recorder shall be installed in the
test chamber such that it will accurately measure the temperature of the
air in the vicinity of the candidate sampler without being unduly
affected by the chamber's air temperature control system.
(f) Procedure. (1) Set up the sampler as specified in paragraph (e)
of this section and otherwise prepare the sampler for normal sample
collection operation as directed in the sampler's operation or
instruction manual.
(2) The test shall consist of four test runs, one at each of the
following conditions of chamber temperature and electrical power line
voltage (respectively):
(i) -20 deg.C 2 deg.C and 105 1 Vac.
(ii) -20 deg.C 2 deg.C and 125 1 Vac.
(iii) =40 deg.C 2 deg.C and 105 1 Vac.
(iv) =40 deg.C 2 deg.C and 125 1 Vac.
(3) For each of the four test runs, set the selected chamber
temperature and power line voltage for the test run. Upon achieving each
temperature setpoint in the chamber, the candidate sampler and flow
meter shall be thermally equilibrated for a period of at least 2 hours
prior to the test run. Following the thermal conditioning time, set the
sampler to automatically start a 6-hour sample collection period at a
convenient time.
(4) During each 6-hour test period:
(i) Measure and record the sample flow rate with the flow rate meter
at intervals not to exceed 5 minutes. If ambient temperature and
pressure corrections are necessary to calculate volumetric flow rate,
ambient temperature and pressure shall be measured at the same frequency
as that of the certified flow rate measurements. Note and record the
actual start and stop times for the 6-hour flow rate test period.
(ii) Determine and record the ambient (chamber) temperature
indicated by the sampler and the corresponding ambient (chamber)
temperature measured by the ambient temperature recorder specified in
paragraph (c)(4) of this section at intervals not to exceed 5 minutes.
(iii) Measure the power line voltage to the sampler at intervals not
greater than 1 hour.
(5) At the end of each test run, terminate the sample period (if not
automatically terminated by the sampler) and download all archived
instrument data from the test sampler.
(g) Test results. For each of the four test runs, examine the
chamber temperature measurements and the power line voltage
measurements. Verify that the temperature and line voltage met the
requirements specified in paragraph (f) of this section at all times
during the test run. If not, the test run is not valid and must be
repeated. Determine the test results as follows:
(1) Mean sample flow rate. (i) From the certified measurements
(Qref) of the test sampler flow rate, tabulate each flow rate
measurement in units of L/min. If ambient temperature and pressure
corrections are necessary to calculate volumetric flow rate, each
measured flow rate shall be corrected using its corresponding
temperature
[[Page 68]]
and pressure measurement values. Calculate the mean flow rate for each
sample period (Qref,ave) as follows:
Equation 11
[GRAPHIC] [TIFF OMITTED] TR18JY97.073
where:
n equals the number of discrete certified flow rate measurements over
each 6-hour test period.
(ii)(A) Calculate the percent difference between this mean flow rate
value and the design value of 16.67 L/min, as follows:
Equation 12
[GRAPHIC] [TIFF OMITTED] TR18JY97.074
(B) To successfully pass this test, the percent difference
calculated in Equation 12 of this paragraph (g)(1)(ii) must be within
5 percent for each test run.
(2) Sample flow rate regulation. (i) From the certified measurements
of the test sampler flow rate, calculate the sample coefficient of
variation of the discrete measurements as follows:
Equation 13
[GRAPHIC] [TIFF OMITTED] TR18JY97.075
(ii) To successfully pass this test, the calculated coefficient of
variation for the certified flow rates must not exceed 2 percent.
(3) Flow rate measurement accuracy. (i) Using the mean volumetric
flow rate reported by the candidate test sampler at the completion of
each 6-hour test (Qind,ave), determine the accuracy of the
reported mean flow rate as:
Equation 14
[GRAPHIC] [TIFF OMITTED] TR18JY97.076
(ii) To successfully pass this test, the percent difference
calculated in Equation 14 of this paragraph (g)(3) shall not exceed 2
percent for each test run.
(4) Flow rate coefficient of variation measurement accuracy. (i)
Using the flow rate coefficient of variation indicated by the candidate
test sampler (%CVind), determine the accuracy of the reported
coefficient of variation as:
Equation 15
[GRAPHIC] [TIFF OMITTED] TR18JY97.077
(ii) To successfully pass this test, the absolute difference
calculated in Equation 15 of this paragraph (g)(4) must not exceed 0.3
(CV%) for each test run.
(5) Ambient temperature measurement accuracy. (i) Calculate the
absolute value of the difference between the mean ambient air
temperature indicated by the test sampler and the mean ambient (chamber)
air temperature measured with the ambient air temperature recorder as:
Equation 16
[GRAPHIC] [TIFF OMITTED] TR18JY97.078
where:
Tind,ave = mean ambient air temperature indicated by the test
sampler, deg.C; and
ref,ave = mean ambient air temperature measured by the
reference temperature instrument, deg.C.
(ii) The calculated temperature difference must be less than 2
deg.C for each test run.
(6) Sampler functionality. To pass the sampler functionality test,
the following two conditions must both be met for each test run:
(i) The sampler must not shutdown during any portion of the 6-hour
test.
(ii) An inspection of the downloaded data from the test sampler
verifies that all the data are consistent with normal operation of the
sampler.
Sec. 53.56 Test for effect of variations in ambient pressure.
(a) Overview. (1) This test procedure is designed to test various
sampler performance parameters under variations in ambient (barometric)
pressure. Tests shall be conducted in a pressure-controlled environment
over two 6-hour time periods during which reference pressure and flow
rate measurements
[[Page 69]]
shall be made at intervals not to exceed 5 minutes. Specific parameters
to be evaluated at operating pressures of 600 and 800 mm Hg are as
follows:
(i) Sample flow rate.
(ii) Flow rate regulation.
(iii) Flow rate measurement accuracy.
(iv) Coefficient of variability measurement accuracy.
(v) Ambient pressure measurement accuracy.
(vi) Proper operation of the sampler when exposed to ambient
pressure extremes.
(2) The performance parameters tested under this procedure, the
corresponding minimum performance specifications, and the applicable
test conditions are summarized in table E-1 of this subpart. Each
performance parameter tested, as described or determined in the test
procedure, must meet or exceed the associated performance specification
given. The candidate sampler must meet all specifications for the
associated PM2.5 method to pass this test procedure.
(b) Technical definition. Sample flow rate means the quantitative
volumetric flow rate of the air stream caused by the sampler to enter
the sampler inlet and pass through the sample filter, measured in actual
volume units at the temperature and pressure of the air as it enters the
inlet.
(c) Required test equipment. (1) Hypobaric chamber or other
pressure-controlled environment or environments, capable of obtaining
and maintaining pressures at 600 mm Hg and 800 mm Hg required for the
test with an accuracy of 5 mm Hg. Henceforth, where the test procedures
specify a test or environmental chamber, an alternative pressure-
controlled environmental area or areas may be substituted, provided the
test pressure requirements are met. Means for simulating ambient
pressure using a closed-loop sample air system may also be approved for
this test; such a proposed method for simulating the test pressure
conditions may be described and submitted to EPA at the address given in
Sec. 53.4(a) prior to conducting the test for a specific individual
determination of acceptability.
(2) Flow rate meter, suitable for measuring and recording the actual
volumetric sampler flow rate at the sampler downtube, with a minimum
range of 10 to 25 L/min, 2 percent certified, NIST-traceable accuracy.
Optional capability for continuous (analog) recording capability or
digital recording at intervals not to exceed 5 minutes is recommended.
While a flow meter which provides a direct indication of volumetric flow
rate is preferred for this test, an alternative certified flow
measurement device may be used as long as appropriate volumetric flow
rate corrections are made based on measurements of actual ambient
temperature and pressure conditions.
(3) Ambient air temperature recorder (if needed for volumetric
corrections to flow rate measurements) with a range -30 deg.C to =50
deg.C, certified accurate to within 0.5 deg.C. If the certified flow
meter does not provide direct volumetric flow rate readings, ambient
temperature measurements must be made using continuous (analog)
recording capability or digital recording at intervals not to exceed 5
minutes.
(4) Barometer, range 600 mm Hg to 800 mm Hg, certified accurate to 2
mm Hg. Ambient air pressure measurements must be made using continuous
(analog) recording capability or digital recording at intervals not to
exceed 5 minutes.
(5) Flow measurement adaptor (40 CFR part 50, appendix L, figure L-
30) or equivalent adaptor to facilitate measurement of sampler flow rate
at the sampler downtube.
(6) Means for creating an additional pressure drop of 55 mm Hg in
the sampler to simulate a heavily loaded filter, such as an orifice or
flow restrictive plate installed in the filter holder or a valve or
other flow restrictor temporarily installed in the flow path near the
filter.
(7) Teflon sample filter, as specified in section 6 of 40 CFR part
50, appendix L (if required).
(d) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests.
[[Page 70]]
The accuracy of flow rate meters shall be verified at the highest and
lowest pressures and temperatures used in the tests and shall be checked
at zero and at least one flow rate within 3 percent of 16.7
L/min within 7 days prior to use for this test. Where an instrument's
measurements are to be recorded with an analog recording device, the
accuracy of the entire instrument-recorder system shall be calibrated or
verified.
(e) Test setup. (1) Setup of the sampler shall be performed as
required in this paragraph (e) and otherwise as described in the
sampler's operation or instruction manual referred to in
Sec. 53.4(b)(3). The sampler shall be installed upright and set up in
the pressure-controlled chamber in its normal configuration for
collecting PM2.5 samples. A sample filter and (or) the device
for creating an additional 55 mm Hg pressure drop shall be installed for
the duration of these tests. The sampler's ambient temperature, ambient
pressure, and flow measurement systems shall all be calibrated per the
sampler's operating manual within 7 days prior to this test.
(2) The inlet of the candidate sampler shall be removed and the flow
measurement adaptor installed on the sampler's downtube. A leak check as
described in the sampler's operation or instruction manual shall be
conducted and must be properly passed before other tests are carried
out.
(3) The inlet of the flow measurement adaptor shall be connected to
the outlet of the flow rate meter.
(4) The barometer shall be installed in the test chamber such that
it will accurately measure the air pressure to which the candidate
sampler is subjected.
(f) Procedure. (1) Set up the sampler as specified in paragraph (e)
of this section and otherwise prepare the sampler for normal sample
collection operation as directed in the sampler's operation or
instruction manual.
(2) The test shall consist of two test runs, one at each of the
following conditions of chamber pressure:
(i) 600 mm Hg.
(ii) 800 mm Hg.
(3) For each of the two test runs, set the selected chamber pressure
for the test run. Upon achieving each pressure setpoint in the chamber,
the candidate sampler shall be pressure-equilibrated for a period of at
least 30 minutes prior to the test run. Following the conditioning time,
set the sampler to automatically start a 6-hour sample collection period
at a convenient time.
(4) During each 6-hour test period:
(i) Measure and record the sample flow rate with the flow rate meter
at intervals not to exceed 5 minutes. If ambient temperature and
pressure corrections are necessary to calculate volumetric flow rate,
ambient temperature and pressure shall be measured at the same frequency
as that of the certified flow rate measurements. Note and record the
actual start and stop times for the 6-hour flow rate test period.
(ii) Determine and record the ambient (chamber) pressure indicated
by the sampler and the corresponding ambient (chamber) pressure measured
by the barometer specified in paragraph (c)(4) of this section at
intervals not to exceed 5 minutes.
(5) At the end of each test period, terminate the sample period (if
not automatically terminated by the sampler) and download all archived
instrument data for the test run from the test sampler.
(g) Test results. For each of the two test runs, examine the chamber
pressure measurements. Verify that the pressure met the requirements
specified in paragraph (f) of this section at all times during the test.
If not, the test run is not valid and must be repeated. Determine the
test results as follows:
(1) Mean sample flow rate. (i) From the certified measurements
(Qref) of the test sampler flow rate, tabulate each flow rate
measurement in units of L/min. If ambient temperature and pressure
corrections are necessary to calculate volumetric flow rate, each
measured flow rate shall be corrected using its corresponding
temperature and pressure measurement values. Calculate the mean flow
rate for the sample period (Qref,ave) as follows:
[[Page 71]]
Equation 17
[GRAPHIC] [TIFF OMITTED] TR18JY97.079
where:
n equals the number of discrete certified flow measurements over the 6-
hour test period.
(ii)(A) Calculate the percent difference between this mean flow rate
value and the design value of 16.67 L/min, as follows:
Equation 18
[GRAPHIC] [TIFF OMITTED] TR18JY97.080
(B) To successfully pass this test, the percent difference
calculated in Equation 18 of this paragraph (g)(1) must be within
5 percent for each test run.
(2) Sample flow rate regulation. (i) From the certified measurements
of the test sampler flow rate, calculate the sample coefficient of
variation of the discrete measurements as follows:
Equation 19
[GRAPHIC] [TIFF OMITTED] TR18JY97.081
(ii) To successfully pass this test, the calculated coefficient of
variation for the certified flow rates must not exceed 2 percent.
(3) Flow rate measurement accuracy. (i) Using the mean volumetric
flow rate reported by the candidate test sampler at the completion of
each 6-hour test (Qind,ave), determine the accuracy of the
reported mean flow rate as:
Equation 20
[GRAPHIC] [TIFF OMITTED] TR18JY97.082
(ii) To successfully pass this test, the percent difference
calculated in Equation 20 of this paragraph (g)(3) shall not exceed 2
percent for each test run.
(4) Flow rate CV measurement accuracy. (i) Using the flow rate
coefficient of variation indicated by the candidate test sampler at the
completion of the 6-hour test (%CVind), determine the
accuracy of the reported coefficient of variation as:
Equation 21
[GRAPHIC] [TIFF OMITTED] TR18JY97.083
(ii) To successfully pass this test, the absolute difference in
values calculated in Equation 21 of this paragraph (g)(4) must not
exceed 0.3 (CV%) for each test run.
(5) Ambient pressure measurement accuracy. (i) Calculate the
absolute difference between the mean ambient air pressure indicated by
the test sampler and the ambient (chamber) air pressure measured with
the reference barometer as:
Equation 22
[GRAPHIC] [TIFF OMITTED] TR18JY97.084
where:
Pind,ave = mean ambient pressure indicated by the test
sampler, mm Hg; and
Pref,ave = mean barometric pressure measured by the reference
barometer, mm Hg.
(ii) The calculated pressure difference must be less than 10 mm Hg
for each test run to pass the test.
(6) Sampler functionality. To pass the sampler functionality test,
the following two conditions must both be met for each test run:
(i) The sampler must not shut down during any part of the 6-hour
tests; and
(ii) An inspection of the downloaded data from the test sampler
verifies that all the data are consistent with normal operation of the
sampler.
[62 FR 38799, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Sec. 53.57 Test for filter temperature control during sampling and post-sampling periods.
(a) Overview. This test is intended to measure the candidate
sampler's ability to prevent excessive overheating of the
PM2.5 sample collection filter (or filters) under conditions
of elevated
[[Page 72]]
solar insolation. The test evaluates radiative effects on filter
temperature during a 4-hour period of active sampling as well as during
a subsequent 4-hour non-sampling time period prior to filter retrieval.
Tests shall be conducted in an environmental chamber which provides the
proper radiant wavelengths and energies to adequately simulate the sun's
radiant effects under clear conditions at sea level. For additional
guidance on conducting solar radiative tests under controlled
conditions, consult military standard specification 810-E (reference 6
in appendix A of this subpart). The performance parameters tested under
this procedure, the corresponding minimum performance specifications,
and the applicable test conditions are summarized in table E-1 of this
subpart. Each performance parameter tested, as described or determined
in the test procedure, must meet or exceed the associated performance
specification to successfully pass this test.
(b) Technical definition. Filter temperature control during sampling
is the ability of a sampler to maintain the temperature of the
particulate matter sample filter within the specified deviation (5
deg.C) from ambient temperature during any active sampling period. Post-
sampling temperature control is the ability of a sampler to maintain the
temperature of the particulate matter sample filter within the specified
deviation from ambient temperature during the period from the end of
active sample collection of the PM2.5 sample by the sampler
until the filter is retrieved from the sampler for laboratory analysis.
(c) Required test equipment. (1) Environmental chamber providing the
means, such as a bank of solar-spectrum lamps, for generating or
simulating thermal radiation in approximate spectral content and
intensity equivalent to solar insolation of 1000 50 W/
m2 inside the environmental chamber. To properly simulate the
sun's radiative effects on the sampler, the solar bank must provide the
spectral energy distribution and permitted tolerances specified in table
E-2 of this subpart. The solar radiation source area shall be such that
the width of the candidate sampler shall not exceed one-half the
dimensions of the solar bank. The solar bank shall be located a minimum
of 76 cm (30 inches) from any surface of the candidate sampler. To meet
requirements of the solar radiation tests, the chamber's internal volume
shall be a minimum of 10 times that of the volume of the candidate
sampler. Air velocity in the region of the sampler must be maintained
continuously during the radiative tests at 2.0 0.5 m/sec.
(2) Ambient air temperature recorder, range -30 deg.C to =50
deg.C, with a resolution of 0.1 deg.C and certified accurate to within
0.5 deg.C. Ambient air temperature measurements must be made using
continuous (analog) recording capability or digital recording at
intervals not to exceed 5 minutes.
(3) Flow measurement adaptor (40 CFR part 50, appendix L, figure L-
30) or equivalent adaptor to facilitate measurement of sampler flow rate
at the sampler downtube.
(4) Miniature temperature sensor(s), capable of being installed in
the sampler without introducing air leakage and capable of measuring the
sample air temperature within 1 cm of the center of the filter,
downstream of the filter; with a resolution of 0.1 deg.C, certified
accurate to within 0.5 deg.C, NIST-traceable, with continuous (analog)
recording capability or digital recording at intervals of not more than
5 minutes.
(5) Solar radiometer, to measure the intensity of the simulated
solar radiation in the test environment, range of 0 to approximately
1500 W/m2. Optional capability for continuous (analog)
recording or digital recording at intervals not to exceed 5 minutes is
recommended.
(6) Sample filter or filters, as specified in section 6 of 40 CFR
part 50, appendix L.
(d) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests. The accuracy
of flow rate meters shall be verified at the highest and lowest
pressures and temperatures used in the tests and shall be checked at
zero and at least one flow rate within 3 percent
[[Page 73]]
of 16.7 L/min within 7 days prior to use for this test. Where an
instrument's measurements are to be recorded with an analog recording
device, the accuracy of the entire instrument-recorder system shall be
calibrated or verified.
(e) Test setup. (1) Setup of the sampler shall be performed as
required in this paragraph (e) and otherwise as described in the
sampler's operation or instruction manual referred to in
Sec. 53.4(b)(3). The sampler shall be installed upright and set up in
the solar radiation environmental chamber in its normal configuration
for collecting PM2.5 samples (with the inlet installed). The
sampler's ambient and filter temperature measurement systems shall be
calibrated per the sampler's operating manual within 7 days prior to
this test. A sample filter shall be installed for the duration of this
test. For sequential samplers, a sample filter shall also be installed
in each available sequential channel or station intended for collection
of a sequential sample (or at least 5 additional filters for magazine-
type sequential samplers) as directed by the sampler's operation or
instruction manual.
(2) The miniature temperature sensor shall be temporarily installed
in the test sampler such that it accurately measures the air temperature
1 cm from the center of the filter on the downstream side of the filter.
The sensor shall be installed such that no external or internal air
leakage is created by the sensor installation. The sensor's dimensions
and installation shall be selected to minimize temperature measurement
uncertainties due to thermal conduction along the sensor mounting
structure or sensor conductors. For sequential samplers, similar
temperature sensors shall also be temporarily installed in the test
sampler to monitor the temperature 1 cm from the center of each filter
stored in the sampler for sequential sample operation.
(3) The solar radiant energy source shall be installed in the test
chamber such that the entire test sampler is irradiated in a manner
similar to the way it would be irradiated by solar radiation if it were
located outdoors in an open area on a sunny day, with the radiation
arriving at an angle of between 30 deg. and 45 deg. from vertical. The
intensity of the radiation received by all sampler surfaces that receive
direct radiation shall average 1000 50 W/m2,
measured in a plane perpendicular to the incident radiation. The
incident radiation shall be oriented with respect to the sampler such
that the area of the sampler's ambient temperature sensor (or
temperature shield) receives full, direct radiation as it would or could
during normal outdoor installation. Also, the temperature sensor must
not be shielded or shaded from the radiation by a sampler part in a way
that would not occur at other normal insolation angles or directions.
(4) The solar radiometer shall be installed in a location where it
measures thermal radiation that is generally representative of the
average thermal radiation intensity that the upper portion of the
sampler and sampler inlet receive. The solar radiometer shall be
oriented so that it measures the radiation in a plane perpendicular to
its angle of incidence.
(5) The ambient air temperature recorder shall be installed in the
test chamber such that it will accurately measure the temperature of the
air in the chamber without being unduly affected by the chamber's air
temperature control system or by the radiant energy from the solar
radiation source that may be present inside the test chamber.
(f) Procedure. (1) Set up the sampler as specified in paragraph (e)
of this section and otherwise prepare the sampler for normal sample
collection operation as directed in the sampler's operation or
instruction manual.
(2) Remove the inlet of the candidate test sampler and install the
flow measurement adaptor on the sampler's downtube. Conduct a leak check
as described in the sampler's operation or instruction manual. The leak
test must be properly passed before other tests are carried out.
(3) Remove the flow measurement adaptor from the downtube and re-
install the sampling inlet.
(4) Activate the solar radiation source and verify that the
resulting energy distribution prescribed in table E-2 of this subpart is
achieved.
[[Page 74]]
(5) Program the test sampler to conduct a single sampling run of 4
continuous hours. During the 4-hour sampling run, measure and record the
radiant flux, ambient temperature, and filter temperature (all filter
temperatures for sequential samplers) at intervals not to exceed 5
minutes.
(6) At the completion of the 4-hour sampling phase, terminate the
sample period, if not terminated automatically by the sampler. Continue
to measure and record the radiant flux, ambient temperature, and filter
temperature or temperatures for 4 additional hours at intervals not to
exceed 5 minutes. At the completion of the 4-hour post-sampling period,
discontinue the measurements and turn off the solar source.
(7) Download all archived sampler data from the test run.
(g) Test results. Chamber radiant flux control. Examine the
continuous record of the chamber radiant flux and verify that the flux
met the requirements specified in table E-2 of this subpart at all times
during the test. If not, the entire test is not valid and must be
repeated.
(1) Filter temperature measurement accuracy. (i) For each 4-hour
test period, calculate the absolute value of the difference between the
mean filter temperature indicated by the sampler (active filter) and the
mean filter temperature measured by the reference temperature sensor
installed within 1 cm downstream of the (active) filter as:
Equation 23
[GRAPHIC] [TIFF OMITTED] TR18JY97.085
where:
Tind,filter = mean filter temperature indicated by the test
sampler, deg.C; and
Tref,filter = mean filter temperature measured by the
reference temperature sensor, deg.C.
(ii) To successfully pass the indicated filter temperature accuracy
test, the calculated difference between the measured means
(Tdiff,filter) must not exceed 2 deg.C for each 4-hour test
period.
(2) Ambient temperature measurement accuracy. (i) For each 4-hour
test period, calculate the absolute value of the difference between the
mean ambient air temperature indicated by the test sampler and the mean
ambient air temperature measured by the reference ambient air
temperature recorder as:
Equation 24
[GRAPHIC] [TIFF OMITTED] TR18JY97.086
where:
Tind,ambient = mean ambient air temperature indicated by the
test sampler, deg.C; and
Tref,ambient = mean ambient air temperature measured by the
reference ambient air temperature recorder, deg.C.
(ii) To successfully pass the indicated ambient temperature accuracy
test, the calculated difference between the measured means
(Tdiff,ambient) must not exceed 2 deg.C for each 4-hour test
period.
(3) Filter temperature control accuracy. (i) For each temperature
measurement interval over each 4-hour test period, calculate the
difference between the filter temperature indicated by the reference
temperature sensor and the ambient temperature indicated by the test
sampler as:
Equation 25
[GRAPHIC] [TIFF OMITTED] TR18JY97.087
(ii) Tabulate and inspect the calculated differences as a function
of time. To successfully pass the indicated filter temperature control
test, the calculated difference between the measured values must not
exceed 5 deg.C for any consecutive intervals covering more than a 30-
minute time period.
(iii) For sequential samplers, repeat the test calculations for each
of the stored sequential sample filters. All stored filters must also
meet the 5 deg.C temperature control test.
[62 FR 38799, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Sec. 53.58 Operational field precision and blank test.
(a) Overview. This test is intended to determine the operational
precision of the candidate sampler during a minimum of 10 days of field
operation, using three collocated test samplers. Measurements of
PM2.5 are made at a test site with all of the samplers and
then compared to determine replicate
[[Page 75]]
precision. Candidate sequential samplers are also subject to a test for
possible deposition of particulate matter on inactive filters during a
period of storage in the sampler. This procedure is applicable to both
reference and equivalent methods. In the case of equivalent methods,
this test may be combined and conducted concurrently with the
comparability test for equivalent methods (described in subpart C of
this part), using three reference method samplers collocated with three
candidate equivalent method samplers and meeting the applicable site and
other requirements of subpart C of this part.
(b) Technical definition. (1) Field precision is defined as the
standard deviation or relative standard deviation of a set of
PM2.5 measurements obtained concurrently with three or more
collocated samplers in actual ambient air field operation.
(2) Storage deposition is defined as the mass of material
inadvertently deposited on a sample filter that is stored in a
sequential sampler either prior to or subsequent to the active sample
collection period.
(c) Test site. Any outdoor test site having PM2.5
concentrations that are reasonably uniform over the test area and that
meet the minimum level requirement of paragraph (g)(2) of this section
is acceptable for this test.
(d) Required facilities and equipment. (1) An appropriate test site
and suitable electrical power to accommodate three test samplers are
required.
(2) Teflon sample filters, as specified in section 6 of 40 CFR part
50, appendix L, conditioned and preweighed as required by section 8 of
40 CFR part 50, appendix L, as needed for the test samples.
(e) Test setup. (1) Three identical test samplers shall be installed
at the test site in their normal configuration for collecting
PM2.5 samples in accordance with the instructions in the
associated manual referred to in Sec. 53.4(b)(3) and should be in
accordance with applicable supplemental guidance provided in reference 3
in appendix A of this subpart. The test samplers' inlet openings shall
be located at the same height above ground and between 2 and 4 meters
apart horizontally. The samplers shall be arranged or oriented in a
manner that will minimize the spatial and wind directional effects on
sample collection of one sampler on any other sampler.
(2) Each test sampler shall be successfully leak checked,
calibrated, and set up for normal operation in accordance with the
instruction manual and with any applicable supplemental guidance
provided in reference 3 in appendix A of this subpart.
(f) Test procedure. (1) Install a conditioned, preweighed filter in
each test sampler and otherwise prepare each sampler for normal sample
collection. Set identical sample collection start and stop times for
each sampler. For sequential samplers, install a conditioned, preweighed
specified filter in each available channel or station intended for
automatic sequential sample filter collection (or at least 5 additional
filters for magazine-type sequential samplers), as directed by the
sampler's operation or instruction manual. Since the inactive sequential
channels are used for the storage deposition part of the test, they may
not be used to collect the active PM2.5 test samples.
(2) Collect either a 24-hour or a 48-hour atmospheric
PM2.5 sample simultaneously with each of the three test
samplers.
(3) Following sample collection, retrieve the collected sample from
each sampler. For sequential samplers, retrieve the additional stored
(blank, unsampled) filters after at least 5 days (120 hours) storage in
the sampler if the active samples are 24-hour samples, or after at least
10 days (240 hours) if the active samples are 48-hour samples.
(4) Determine the measured PM2.5 mass concentration for
each sample in accordance with the applicable procedures prescribed for
the candidate method in appendix L, 40 CFR part 50 of this chapter, in
the associated manual referred to in Sec. 53.4(b)(3) and in accordance
with supplemental guidance in reference 2 in appendix A of this subpart.
For sequential samplers, also similarly determine the storage deposition
as the net weight gain of each blank, unsampled filter after the 5-day
(or 10-day) period of storage in the sampler.
(5) Repeat this procedure to obtain a total of 10 sets of any
combination of
[[Page 76]]
24-hour or 48-hour PM2.5 measurements over 10 test periods.
For sequential samplers, repeat the 5-day (or 10-day) storage test of
additional blank filters once for a total of two sets of blank filters.
(g) Calculations. (1) Record the PM2.5 concentration for
each test sampler for each test period as Ci,j, where i is
the sampler number (i = 1,2,3) and j is the test period (j = 1,2, . . .
10).
(2)(i) For each test period, calculate and record the average of the
three measured PM2.5 concentrations as Cj where j
is the test period:
Equation 26
[GRAPHIC] [TIFF OMITTED] TR18JY97.088
(ii) If Cave,j 10 g/m3 for any test
period, data from that test period are unacceptable, and an additional
sample collection set must be obtained to replace the unacceptable data.
(3)(i) Calculate and record the precision for each of the 10 test
days as:
Equation 27
[GRAPHIC] [TIFF OMITTED] TR18JY97.089
(ii) If Cave,j is below 40 g/m3 for
24-hour measurements or below 30 g/m3 for 48-hour
measurements; or
Equation 28
[GRAPHIC] [TIFF OMITTED] TR18JY97.090
(iii) If Cave,j is above 40 g/m3 for
24-hour measurements or above 30 g/m3 for 48-hour
measurements.
(h) Test results. (1) The candidate method passes the precision test
if all 10 Pj or RPj values meet the specifications
in table E-1 of this subpart.
(2) The candidate sequential sampler passes the blank filter storage
deposition test if the average net storage deposition weight gain of
each set of blank filters (total of the net weight gain of each blank
filter divided by the number of filters in the set) from each test
sampler (six sets in all) is less than 50 g.
Sec. 53.59 Aerosol transport test for Class I equivalent method samplers.
(a) Overview. This test is intended to verify adequate aerosol
transport through any modified or air flow splitting components that may
be used in a Class I candidate equivalent method sampler such as may be
necessary to achieve sequential sampling capability. This test is
applicable to all Class I candidate samplers in which the aerosol flow
path (the flow path through which sample air passes upstream of sample
collection filter) differs from that specified for reference method
samplers as specified in 40 CFR part 50, appendix L. The test
requirements and performance specifications for this test are summarized
in table E-1 of this subpart.
(b) Technical definitions. (1) Aerosol transport is the percentage
of a laboratory challenge aerosol which penetrates to the active sample
filter of the candidate equivalent method sampler.
(2) The active sample filter is the exclusive filter through which
sample air is flowing during performance of this test.
(3) A no-flow filter is a sample filter through which no sample air
is intended to flow during performance of this test.
(4) A channel is any of two or more flow paths that the aerosol may
take, only one of which may be active at a time.
(5) An added component is any physical part of the sampler which is
different in some way from that specified for a reference method sampler
in 40 CFR part 50, appendix L, such as a device or means to allow or
cause the aerosol to be routed to one of several channels.
(c) Required facilities and test equipment. (1) Aerosol generation
system, as specified in Sec. 53.62(c)(2).
(2) Aerosol delivery system, as specified in Sec. 53.64(c)(2).
(3) Particle size verification equipment, as specified in
Sec. 53.62(c)(3).
[[Page 77]]
(4) Fluorometer, as specified in Sec. 53.62(c)(7).
(5) Candidate test sampler, with the inlet and impactor or impactors
removed, and with all internal surfaces of added components electroless
nickel coated as specified in Sec. 53.64(d)(2).
(6) Filters that are appropriate for use with fluorometric methods
(e.g., glass fiber).
(d) Calibration of test measurement instruments. Submit
documentation showing evidence of appropriately recent calibration,
certification of calibration accuracy, and NIST-traceability (if
required) of all measurement instruments used in the tests. The accuracy
of flow rate meters shall be verified at the highest and lowest
pressures and temperatures used in the tests and shall be checked at
zero and at least one flow rate within 3 percent of 16.7 L/
min within 7 days prior to use for this test. Where an instrument's
measurements are to be recorded with an analog recording device, the
accuracy of the entire instrument-recorder system shall be calibrated or
verified.
(e) Test setup. (1) The candidate test sampler shall have its inlet
and impactor or impactors removed. The lower end of the down tube shall
be reconnected to the filter holder, using an extension of the downtube,
if necessary. If the candidate sampler has a separate impactor for each
channel, then for this test, the filter holder assemblies must be
connected to the physical location on the sampler where the impactors
would normally connect.
(2) The test particle delivery system shall be connected to the
sampler downtube so that the test aerosol is introduced at the top of
the downtube.
(f) Test procedure. (1) All surfaces of the added or modified
component or components which come in contact with the aerosol flow
shall be thoroughly washed with 0.01 N NaOH and then dried.
(2) Generate aerosol. (i) Generate aerosol composed of oleic acid
with a uranine fluorometric tag of 3 0.25 m
aerodynamic diameter using a vibrating orifice aerosol generator
according to conventions specified in Sec. 53.61(g).
(ii) Check for the presence of satellites and adjust the generator
to minimize their production.
(iii) Calculate the aerodynamic particle size using the operating
parameters of the vibrating orifice aerosol generator. The calculated
aerodynamic diameter must be 3 0.25 m aerodynamic
diameter.
(3) Verify the particle size according to procedures specified in
Sec. 53.62(d)(4)(i).
(4) Collect particles on filters for a time period such that the
relative error of the resulting measured fluorometric concentration for
the active filter is less than 5 percent.
(5) Determine the quantity of material collected on the active
filter using a calibrated fluorometer. Record the mass of fluorometric
material for the active filter as Mactive (i) where i = the
active channel number.
(6) Determine the quantity of material collected on each no-flow
filter using a calibrated fluorometer. Record the mass of fluorometric
material on each no-flow filter as Mno-flow.
(7) Using 0.01 N NaOH, wash the surfaces of the added component or
components which contact the aerosol flow. Determine the quantity of
material collected using a calibrated fluorometer. Record the mass of
fluorometric material collected in the wash as Mwash.
(8) Calculate the aerosol transport as:
Equation 29
[GRAPHIC] [TIFF OMITTED] TR18JY97.091
where:
i = the active channel number.
(9) Repeat paragraphs (f)(1) through (8) of this section for each
channel, making each channel in turn the exclusive active channel.
(g) Test results. The candidate Class I sampler passes the aerosol
transport test if T(i) is at least 97 percent for each
channel.
[[Page 78]]
Table E-1 to Subpart E--Summary of Test Requirements for
Reference and Class I Equivalent Methods for PM2.5
----------------------------------------------------------------------------------------------------------------
Part 50,
Subpart E Procedure Performance Test Performance Test Conditions Appendix L
Specification Reference
----------------------------------------------------------------------------------------------------------------
Sec. 53.52 Sampler leak check Sampler leak check External leakage: Controlled leak Sec. 7.4.6
test. facility 80 mL/min, max flow rate of 80
Internal leakage: mL/min
80 mL/min, max
----------------------------------------------------------------------------------------------------------------
Sec. 53.53 Base flow rate test... Sample flow rate: 1. 16.67 5%, L/min operational test Sec. 7.4.2
2. Regulation 2. 2%, max plus flow rate Sec. 7.4.3
3. Meas. accuracy 3. 2%, max cut-off test Sec. 7.4.4
4. CV accuracy 4. 0.3%, max (b) Nominal Sec. 7.4.5
5. Cut-off 5. Flow rate cut- conditions
off if flow rate (c) Additional 55
deviates more mm Hg pressure
than 10% from drop to simulate
design flow rate loaded filter
for >6030 seconds restriction used
for cut-off test
----------------------------------------------------------------------------------------------------------------
Sec. 53.54 Power interruption Sample flow rate: 1. 16.675%, L/min operational test Sec. 7.4.2
2. Regulation 2. 2%, max (b) Nominal Sec. 7.4.3
3. Meas. accuracy 3. 2%, max conditions Sec. 7.4.5
4. CV accuracy 4. 0.3%, max (c) Additional 55 Sec. 7.4.12
5. Occurrence time 5. 2 mm Hg pressure Sec. 7.4.13
of power min if >60 drop to simulate Sec. 7.4.15.4
interruptions seconds loaded filter Sec. 7.4.15.5
6. Elapsed sample 6. 20 (d) 6 power
time seconds interruptions of
7. Sample volume 7. plus-minus2%, various durations
max
----------------------------------------------------------------------------------------------------------------
Sec. 53.55 Temperature and line Sample flow rate: 1. 16.675%, L/min operational test Sec. 7.4.2
2. Regulation 2. 2 %, max (b) Nominal Sec. 7.4.3
3. Meas. accuracy 3. 2 %, max conditions Sec. 7.4.5
4. CV accuracy 4. 0.3 %, max (c) Additional 55 Sec. 7.4.8
5. Temperature 5. 2 deg.C mm Hg pressure Sec. 7.4.15.1
meas. accuracy drop to simulate
6. Proper operation loaded filter
(d) Ambient
temperature at -
20 and +40 deg.C
(e) Line voltage:
105 Vac to 125
Vac
----------------------------------------------------------------------------------------------------------------
Sec. 53.56 Barometric pressure Sample flow rate: 1. 16.675%, L/min operational test Sec. 7.4.2
2. Regulation 2. 2%, max (b) Nominal Sec. 7.4.3
3. Meas. accuracy 3. 2%, max conditions Sec. 7.4.5
4. CV accuracy 4. 0.3%, max (c) Additional 55 Sec. 7.4.9
5. Pressure meas. 5. 10 mm Hg mm Hg pressure
accuracy drop to simulate
6. Proper operation loaded filter
(d) Barometric
pressure at 600
and 800 mm Hg.
----------------------------------------------------------------------------------------------------------------
Sec. 53.57 Filter temperature 1. Filter temp 1. 2 deg.C (a) 4-hour Sec. 7.4.8
control test. meas. accuracy 2. 2 deg.C simulated solar Sec. 7.4.10
2. Ambient temp. 3. Not more than 5 radiation, Sec. 7.4.11
meas. accuracy deg.C above sampling
3. Filter temp ambient temp. for (b) 4-hour
control accuracy, more than 30 min simulated solar
sampling and non- radiation, non-
sampling sampling
(c) Solar flux of
10005
0W/m2
----------------------------------------------------------------------------------------------------------------
Sec. 53.58 Field precision test.. 1. Measurement 1. Pj 2 g/ (a) 3 collocated Sec. 5.1
precision m3 for conc. 40 samplers at 1 Sec. 7.3.5
2. Storage g/m3 (24- site for at least Sec. 8
deposition test hr) or 30 g/m3 (48-hr); (b) PM2.5 conc.10 j 5% for conc. m>g/m3
>40 g/m3 (c) 24- or 48-hour
(24-hr) or >30 samples
g/m3 (48- (d) 5- or 10-day
hr) storage period
2. 50 g, for inactive
max weight gain stored filters
----------------------------------------------------------------------------------------------------------------
[[Page 79]]
The Following Requirement is Applicable to Candidate Equivalent Methods Only
----------------------------------------------------------------------------------------------------------------
Sec. 53.59 Aerosol transport test Aerosol transport 97%, min, for all Determine aerosol
channels transport through
any new or
modified
components with
respect to the
reference method
sampler before
the filter for
each channel.
----------------------------------------------------------------------------------------------------------------
[62 FR 38799, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Table E-2 to Subpart E--Spectral Energy Distribution and
Permitted Tolerance for Conducting Radiative Tests
------------------------------------------------------------------------
Spectral Region
Characteristic -----------------------------------------------------
Ultraviolet Visible Infrared
------------------------------------------------------------------------
Bandwidth (m) 0.32 to 0.40
Irradiance (W/m2) 5 450 to 550 439
56
Allowed Tolerance 35% 10%
Subpart F--Procedures for Testing Performance Characteristics of Class
II Equivalent Methods for PM2.5
Source: 62 FR 38814, July 18, 1997, unless otherwise noted.
Sec. 53.60 General provisions.
(a) This subpart sets forth the specific requirements that a
PM2.5 sampler associated with a candidate Class II equivalent
method must meet to be designated as an equivalent method for
PM2.5. This subpart also sets forth the explicit test
procedures that must be carried out and the test results, evidence,
documentation, and other materials that must be provided to EPA to
demonstrate that a sampler meets all specified requirements for
designation as an equivalent method.
(b) A candidate method described in an application for a reference
or equivalent method application submitted under Sec. 53.4 shall be
determined by the EPA to be a Class II candidate equivalent method on
the basis of the definition of a Class II equivalent method given in
Sec. 53.1.
(c) Any sampler associated with a Class II candidate equivalent
method (Class II sampler) must meet all requirements for reference
method samplers and Class I equivalent method samplers specified in
subpart E of this part, as appropriate. In addition, a Class II sampler
must meet the additional requirements as specified in paragraph (d) of
this section.
(d) Except as provided in paragraphs (d) (1), (2), and (3) of this
section, all Class II samplers are subject to the additional tests and
performance requirements specified in Sec. 53.62 (full wind tunnel
test), Sec. 53.65 (loading test), and Sec. 53.66 (volatility test).
Alternative tests and performance requirements, as described in
paragraphs (d)(1), (2), and (3) of this section, are optionally
available for certain Class II samplers which meet the requirements for
reference method or Class I samplers given in 40 CFR part 50, appendix
L, and in subpart E of this part, except for specific deviations of the
inlet, fractionator, or filter.
(1) Inlet deviation. A sampler which has been determined to be a
Class II sampler solely because the design or construction of its inlet
deviates from the design or construction of the inlet specified in 40
CFR part 50, appendix L, for reference method samplers shall not be
subject to the requirements of Sec. 53.62 (full wind tunnel test),
provided that it meets all requirements of Sec. 53.63 (wind tunnel inlet
aspiration test), Sec. 53.65 (loading test), and Sec. 53.66 (volatility
test).
(2) Fractionator deviation. A sampler which has been determined to
be a Class II sampler solely because the design or construction of its
particle size fractionator deviates from the design or construction of
the particle size fractionator specified in 40 CFR part 50, appendix L
for reference method samplers shall not be subject to the requirements
of Sec. 53.62 (full wind tunnel test), provided that it meets all
requirements of Sec. 53.64 (static fractionator test), Sec. 53.65
(loading test), and Sec. 53.66 (volatility test).
(3) Filter size deviation. A sampler which has been determined to be
a Class II sampler solely because its effective filtration area deviates
from that of the reference method filter specified in 40 CFR part 50,
appendix L, for reference method samplers shall not be subject to the
requirements of Sec. 53.62 (full wind tunnel test) nor Sec. 53.65
(loading test), provided it meets all requirements of Sec. 53.66
(volatility test).
(e) The test specifications and acceptance criteria for each test
are summarized in table F-1 of this subpart. The candidate sampler must
demonstrate performance that meets the acceptance criteria for each
applicable test to be designated as an equivalent method.
(f) Overview of various test procedures for Class II samplers--(1)
Full wind tunnel test. This test procedure is designed to ensure that
the candidate sampler's effectiveness (aspiration of an ambient aerosol
and penetration of the sub 2.5-micron fraction to its sample filter)
will be comparable to that of a reference method sampler. The candidate
sampler is challenged at wind speeds of 2 and 24 km/hr with monodisperse
aerosols of the size specified in table F-2 of this subpart. The
experimental test results are then integrated with three
[[Page 82]]
idealized ambient distributions (typical, fine, and coarse) to yield the
expected mass concentration measurement for each. The acceptance
criteria are based on the results of this numerical analysis and the
particle diameter for which the sampler effectiveness is 50 percent.
(2) Wind tunnel inlet aspiration test. The wind tunnel inlet
aspiration test directly compares the inlet of the candidate sampler to
the inlet of a reference method sampler with the single-sized, liquid,
monodisperse challenge aerosol specified in table F-2 of this subpart at
wind speeds of 2 km/hr and 24 km/hr. The acceptance criteria, presented
in table F-1 of this subpart, is based on the relative aspiration
between the candidate inlet and the reference method inlet.
(3) Static fractionator test. The static fractionator test
determines the effectiveness of the candidate sampler's 2.5-micron
fractionator under static conditions for aerosols of the size specified
in table F-2 of this subpart. The numerical analysis procedures and
acceptance criteria are identical to those in the full wind tunnel test.
(4) Loading test. The loading test is conducted to ensure that the
performance of a candidate sampler is not significantly affected by the
amount of particulate deposited on its interior surfaces between
periodic cleanings. The candidate sampler is artificially loaded by
sampling a test environment containing aerosolized, standard test dust.
The duration of the loading phase is dependent on both the time between
cleaning as specified by the candidate method and the aerosol mass
concentration in the test environment. After loading, the candidate's
performance must then be evaluated by Sec. 53.62 (full wind tunnel
evaluation), Sec. 53.64 (wind tunnel inlet aspiration test), or
Sec. 53.64 (static fractionator test). If the results of the appropriate
test meet the criteria presented in table F-1 of this subpart, then the
candidate sampler passes the loading test under the condition that it be
cleaned at least as often as the cleaning frequency proposed by the
candidate method and that has been demonstrated to be acceptable by this
test.
(5) Volatility test. The volatility test challenges the candidate
sampler with a polydisperse, semi-volatile liquid aerosol. This aerosol
is simultaneously sampled by the candidate method sampler and a
reference method sampler for a specified time period. Clean air is then
passed through the samplers during a blow-off time period. Residual mass
is then calculated as the weight of the filter after the blow-off phase
is subtracted from the initial weight of the filter. Acceptance criteria
are based on a comparison of the residual mass measured by the candidate
sampler (corrected for flow rate variations from that of the reference
method) to the residual mass measured by the reference method sampler
for several specified clean air sampling time periods.
(g) Test data. All test data and other documentation obtained from
or pertinent to these tests shall be identified, dated, signed by the
analyst performing the test, and submitted to EPA as part of the
equivalent method application. Schematic drawings of each particle
delivery system and other information showing complete procedural
details of the test atmosphere generation, verification, and delivery
techniques for each test performed shall be submitted to EPA. All
pertinent calculations shall be clearly presented. In addition,
manufacturers are required to submit as part of the application, a
Designation Testing Checklist (Figure F-1 of this subpart) which has
been completed and signed by an ISO-certified auditor.
Sec. 53.61 Test conditions for PM2.5 reference method equivalency.
(a) Sampler surface preparation. Internal surfaces of the candidate
sampler shall be cleaned and dried prior to performing any Class II
sampler test in this subpart. The internal collection surfaces of the
sampler shall then be prepared in strict accordance with the operating
instructions specified in the sampler's operating manual referred to in
section 7.4.18 of 40 CFR part 50, appendix L.
(b) Sampler setup. Set up and start up of all test samplers shall be
in strict accordance with the operating instructions specified in the
manual referred
[[Page 83]]
to in section 7.4.18 of 40 CFR part 50, appendix L, unless otherwise
specified within this subpart.
(c) Sampler adjustments. Once the test sampler or samplers have been
set up and the performance tests started, manual adjustment shall be
permitted only between test points for all applicable tests. Manual
adjustments and any periodic maintenance shall be limited to only those
procedures prescribed in the manual referred to in section 7.4.18 of 40
CFR part 50, appendix L. The submitted records shall clearly indicate
when any manual adjustment or periodic maintenance was made and shall
describe the operations performed.
(d) Sampler malfunctions. If a test sampler malfunctions during any
of the applicable tests, that test run shall be repeated. A detailed
explanation of all malfunctions and the remedial actions taken shall be
submitted as part of the equivalent method application.
(e) Particle concentration measurements. All measurements of
particle concentration must be made such that the relative error in
measurement is less than 5.0 percent. Relative error is defined as (s
x 100 percent)/(X), where s is the sample standard deviation of the
particle concentration detector, X is the measured concentration, and
the units of s and X are identical.
(f) Operation of test measurement equipment. All test measurement
equipment shall be set up, calibrated, and maintained by qualified
personnel according to the manufacturer's instructions. All appropriate
calibration information and manuals for this equipment shall be kept on
file.
(g) Vibrating orifice aerosol generator conventions. This section
prescribes conventions regarding the use of the vibrating orifice
aerosol generator (VOAG) for the size-selective performance tests
outlined in Secs. 53.62, 53.63, 53.64, and 53.65.
(1) Particle aerodynamic diameter. The VOAG produces near-
monodisperse droplets through the controlled breakup of a liquid jet.
When the liquid solution consists of a non-volatile solute dissolved in
a volatile solvent, the droplets dry to form particles of near-
monodisperse size.
(i) The physical diameter of a generated spherical particle can be
calculated from the operating parameters of the VOAG as:
Equation 1
[GRAPHIC] [TIFF OMITTED] TR18JY97.094
where:
Dp = particle physical diameter, m;
Q = liquid volumetric flow rate, m3/sec;
Cvol = volume concentration (particle volume produced per
drop volume), dimensionless; and
f = frequency of applied vibrational signal, 1/sec.
(ii) A given particle's aerodynamic behavior is a function of its
physical particle size, particle shape, and density. Aerodynamic
diameter is defined as the diameter of a unit density
(o = 1g/cm3) sphere having the same
settling velocity as the particle under consideration. For converting a
spherical particle of known density to aerodynamic diameter, the
governing relationship is:
Equation 2
[GRAPHIC] [TIFF OMITTED] TR18JY97.095
where:
Dae = particle aerodynamic diameter, m;
p = particle density, g/cm3;
o = aerodynamic particle density = 1 g/
cm3;
CDp = Cunningham's slip correction factor for physical
particle diameter, dimensionless; and
CDae = Cunningham's slip correction factor for aerodynamic
particle diameter, dimensionless.
(iii) At room temperature and standard pressure, the Cunningham's
slip correction factor is solely a function of particle diameter:
Equation 3
[GRAPHIC] [TIFF OMITTED] TR18JY97.096
or
[[Page 84]]
Equation 4
[GRAPHIC] [TIFF OMITTED] TR18JY97.097
(iv) Since the slip correction factor is itself a function of
particle diameter, the aerodynamic diameter in equation 2 of paragraph
(g)(1)(ii) of this section cannot be solved directly but must be
determined by iteration.
(2) Solid particle generation. (i) Solid particle tests performed in
this subpart shall be conducted using particles composed of ammonium
fluorescein. For use in the VOAG, liquid solutions of known volumetric
concentration can be prepared by diluting fluorescein powder
(C20H12O5, FW = 332.31, CAS 2321-07-5)
with aqueous ammonia. Guidelines for preparation of fluorescein
solutions of the desired volume concentration (Cvol) are
presented by Vanderpool and Rubow (1988) (Reference 2 in appendix A of
this subpart). For purposes of converting particle physical diameter to
aerodynamic diameter, an ammonium fluorescein density of 1.35 g/
cm3 shall be used.
(ii) Mass deposits of ammonium fluorescein shall be extracted and
analyzed using solutions of 0.01 N ammonium hydroxide.
(3) Liquid particle generation. (i) Tests prescribed in Sec. 53.63
for inlet aspiration require the use of liquid particle tests composed
of oleic acid tagged with uranine to enable subsequent fluorometric
quantitation of collected aerosol mass deposits. Oleic acid
(C18H34O2, FW = 282.47, CAS 112-80-1)
has a density of 0.8935 g/cm3. Because the viscosity of oleic
acid is relatively high, significant errors can occur when dispensing
oleic acid using volumetric pipettes. For this reason, it is recommended
that oleic acid solutions be prepared by quantifying dispensed oleic
acid gravimetrically. The volume of oleic acid dispensed can then be
calculated simply by dividing the dispensed mass by the oleic acid
density.
(ii) Oleic acid solutions tagged with uranine shall be prepared as
follows. A known mass of oleic acid shall first be diluted using
absolute ethanol. The desired mass of the uranine tag should then be
diluted in a separate container using absolute ethanol. Uranine
(C20H10O5Na2, FW = 376.3,
CAS 518-47-8) is the disodium salt of fluorescein and has a density of
1.53 g/cm3. In preparing uranine tagged oleic acid particles,
the uranine content shall not exceed 20 percent on a mass basis. Once
both oleic acid and uranine solutions are properly prepared, they can
then be combined and diluted to final volume using absolute ethanol.
(iii) Calculation of the physical diameter of the particles produced
by the VOAG requires knowledge of the liquid solution's volume
concentration (Cvol). Because uranine is essentially
insoluble in oleic acid, the total particle volume is the sum of the
oleic acid volume and the uranine volume. The volume concentration of
the liquid solution shall be calculated as:
Equation 5
[GRAPHIC] [TIFF OMITTED] TR18JY97.098
where:
Vu = uranine volume, ml;
Voleic = oleic acid volume, ml;
Vsol = total solution volume, ml;
Mu = uranine mass, g;
u = uranine density, g/cm3;
Moleic = oleic acid mass, g; and
oleic = oleic acid density, g/cm3.
(iv) For purposes of converting the particles' physical diameter to
aerodynamic diameter, the density of the generated particles shall be
calculated as:
Equation 6
[GRAPHIC] [TIFF OMITTED] TR18JY97.099
(v) Mass deposits of oleic acid shall be extracted and analyzed
using solutions of 0.01 N sodium hydroxide.
[62 FR 38814, July 18, 1997; 63 FR 7714, Feb. 17, 1998]
Sec. 53.62 Test procedure: Full wind tunnel test.
(a) Overview. The full wind tunnel test evaluates the effectiveness
of the candidate sampler at 2 km/hr and 24 km/hr for aerosols of the
size specified in table F-2 of this subpart (under the
[[Page 85]]
heading, ``Full Wind Tunnel Test''). For each wind speed, a smooth curve
is fit to the effectiveness data and corrected for the presence of
multiplets in the wind tunnel calibration aerosol. The cutpoint diameter
(Dp50) at each wind speed is then determined from the
corrected effectiveness curves. The two resultant penetration curves are
then each numerically integrated with three idealized ambient particle
size distributions to provide six estimates of measured mass
concentration. Critical parameters for these idealized distributions are
presented in table F-3 of this subpart.
(b) Technical definitions. Effectiveness is the ratio (expressed as
a percentage) of the mass concentration of particles of a specific size
reaching the sampler filter or filters to the mass concentration of
particles of the same size approaching the sampler.
(c) Facilities and equipment required--(1) Wind tunnel. The particle
delivery system shall consist of a blower system and a wind tunnel
having a test section of sufficiently large cross-sectional area such
that the test sampler, or portion thereof, as installed in the test
section for testing, blocks no more than 15 percent of the test section
area. The wind tunnel blower system must be capable of maintaining
uniform wind speeds at the 2 km/hr and 24 km/hr in the test section.
(2) Aerosol generation system. A vibrating orifice aerosol generator
shall be used to produce monodisperse solid particles of ammonium
fluorescein with equivalent aerodynamic diameters as specified in table
F-2 of this subpart. The geometric standard deviation for each particle
size generated shall not exceed 1.1 (for primary particles) and the
proportion of multiplets (doublets and triplets) in all test particle
atmosphere shall not exceed 10 percent of the particle population. The
aerodynamic particle diameter, as established by the operating
parameters of the vibrating orifice aerosol generator, shall be within
the tolerance specified in table F-2 of this subpart.
(3) Particle size verification equipment. The size of the test
particles shall be verified during this test by use of a suitable
instrument (e.g., scanning electron microscope, optical particle sizer,
time-of-flight apparatus). The instrument must be capable of measuring
solid and liquid test particles with a size resolution of 0.1 m
or less. The accuracy of the particle size verification technique shall
be 0.15 m or better.
(4) Wind speed measurement. The wind speed in the wind tunnel shall
be determined during the tests using an appropriate technique capable of
a precision of 2 percent and an accuracy of 5 percent or better (e.g.,
hot-wire anemometry). For the wind speeds specified in table F-2 of this
subpart, the wind speed shall be measured at a minimum of 12 test points
in a cross-sectional area of the test section of the wind tunnel. The
mean wind speed in the test section must be within 10
percent of the value specified in table F-2 of this subpart, and the
variation at any test point in the test section may not exceed 10
percent of the measured mean.
(5) Aerosol rake. The cross-sectional uniformity of the particle
concentration in the sampling zone of the test section shall be
established during the tests using an array of isokinetic samplers,
referred to as a rake. Not less than five evenly spaced isokinetic
samplers shall be used to determine the particle concentration spatial
uniformity in the sampling zone. The sampling zone shall be a
rectangular area having a horizontal dimension not less than 1.2 times
the width of the test sampler at its inlet opening and a vertical
dimension not less than 25 centimeters.
(6) Total aerosol isokinetic sampler. After cross-sectional
uniformity has been confirmed, a single isokinetic sampler may be used
in place of the array of isokinetic samplers for the determination of
particle mass concentration used in the calculation of sampling
effectiveness of the test sampler in paragraph (d)(5) of this section.
In this case, the array of isokinetic samplers must be used to
demonstrate particle concentration uniformity prior to the replicate
measurements of sampling effectiveness.
(7) Fluorometer. A fluorometer used for quantifying extracted
aerosol mass deposits shall be set up, maintained,
[[Page 86]]
and calibrated according to the manufacturer's instructions. A series of
calibration standards shall be prepared to encompass the minimum and
maximum concentrations measured during size-selective tests. Prior to
each calibration and measurement, the fluorometer shall be zeroed using
an aliquot of the same solvent used for extracting aerosol mass
deposits.
(8) Sampler flow rate measurements. All flow rate measurements used
to calculate the test atmosphere concentrations and the test results
must be accurate to within 2 percent, referenced to a NIST-
traceable primary standard. Any necessary flow rate measurement
corrections shall be clearly documented. All flow rate measurements
shall be performed and reported in actual volumetric units.
(d) Test procedures--(1) Establish and verify wind speed. (i)
Establish a wind speed specified in table F-2 of this subpart.
(ii) Measure the wind speed at a minimum of 12 test points in a
cross-sectional area of the test section of the wind tunnel using a
device as described in paragraph (c)(4) of this section.
(iii) Verify that the mean wind speed in the test section of the
wind tunnel during the tests is within 10 percent of the value specified
in table F-2 of this subpart. The wind speed measured at any test point
in the test section shall not differ by more than 10 percent from the
mean wind speed in the test section.
(2) Generate aerosol. (i) Generate particles of a size specified in
table F-2 of this subpart using a vibrating orifice aerosol generator.
(ii) Check for the presence of satellites and adjust the generator
as necessary.
(iii) Calculate the physical particle size using the operating
parameters of the vibrating orifice aerosol generator and record.
(iv) Determine the particle's aerodynamic diameter from the
calculated physical diameter and the known density of the generated
particle. The calculated aerodynamic diameter must be within the
tolerance specified in table F-2 of this subpart.
(3) Introduce particles into the wind tunnel. Introduce the
generated particles into the wind tunnel and allow the particle
concentration to stabilize.
(4) Verify the quality of the test aerosol. (i) Extract a
representative sample of the aerosol from the sampling test zone and
measure the size distribution of the collected particles using an
appropriate sizing technique. If the measurement technique does not
provide a direct measure of aerodynamic diameter, the geometric mean
aerodynamic diameter of the challenge aerosol must be calculated using
the known density of the particle and the measured mean physical
diameter. The determined geometric mean aerodynamic diameter of the test
aerosol must be within 0.15 m of the aerodynamic diameter
calculated from the operating parameters of the vibrating orifice
aerosol generator. The geometric standard deviation of the primary
particles must not exceed 1.1.
(ii) Determine the population of multiplets in the collected sample.
The multiplet population of the particle test atmosphere must not exceed
10 percent of the total particle population.
(5) Aerosol uniformity and concentration measurement. (i) Install an
array of five or more evenly spaced isokinetic samplers in the sampling
zone (paragraph (c)(5) of this section). Collect particles on
appropriate filters over a time period such that the relative error of
the measured particle concentration is less than 5.0 percent.
(ii) Determine the quantity of material collected with each
isokinetic sampler in the array using a calibrated fluorometer.
Calculate and record the mass concentration for each isokinetic sampler
as:
Equation 7
[GRAPHIC] [TIFF OMITTED] TR18JY97.100
where:
i = replicate number;
j = isokinetic sampler number;
M