[Title 40 CFR ]
[Code of Federal Regulations (annual edition) - July 1, 1998 Edition]
[From the U.S. Government Printing Office]
[[Page i]]
40
Protection of Environment
PARTS 53 TO 59
Revised as of July 1, 1998
CONTAINING
A CODIFICATION OF DOCUMENTS
OF GENERAL APPLICABILITY
AND FUTURE EFFECT
AS OF JULY 1, 1998
With Ancillaries
Published by
the Office of the Federal Register
National Archives and Records
Administration
as a Special Edition of
the Federal Register
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U.S. GOVERNMENT PRINTING OFFICE
WASHINGTON : 1998
For sale by U.S. Government Printing Office
Superintendent of Documents, Mail Stop: SSOP, Washington, DC 20402-9328
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Table of Contents
Page
Explanation................................................. v
Title 40:
Chapter I--Environmental Protection Agency................ 3
Finding Aids:
Material Approved for Incorporation by Reference.......... 299
Table of CFR Titles and Chapters.......................... 301
Alphabetical List of Agencies Appearing in the CFR........ 319
Table of OMB Control Numbers.............................. 329
List of CFR Sections Affected............................. 349
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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.
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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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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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INCORPORATION BY REFERENCE
What is incorporation by reference? Incorporation by reference was
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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), and Acts Requiring Publication
in the Federal Register (Table II). 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.
[[Page vii]]
A List of CFR Sections Affected (LSA) is published monthly, keyed to
the revision dates of the 50 CFR titles.
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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For inquiries concerning CFR reference assistance, call 202-523-5227
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Raymond A. Mosley,
Director,
Office of the Federal Register.
July 1, 1998.
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THIS TITLE
Title 40--Protection of Environment is composed of twenty-three
volumes. The parts in these volumes are arranged in the following order:
parts 1-49, parts 50-51, parts 52.01-52.1018, part 52.1019-end, parts
53-59, part 60, parts 61-62, part 63, parts 64-71, parts 72-80, parts
81-85, part 86, parts 87-135, 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, 1998.
Chapter I--Environmental Protection Agency appears in all twenty-two
volumes. A Pesticide Tolerance Commodity/Chemical Index appears 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. For the convenience of the user, Sec. 9.1 appears in the
Finding Aids section of the volumes containing part 50 to the end.
For this volume, Kenneth R. Payne was Chief Editor. The Code of
Federal Regulations publication program is under the direction of
Frances D. McDonald, assisted by Alomha S. Morris.
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[[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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SUBCHAPTER C--AIR PROGRAMS (CONTINUED)
Editorial Note: 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, parts 61-62, part 63, parts 64-71, parts 72-80, parts 81-85, part
86, and parts 87-135.
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........................ 128
57 Primary nonferrous smelter orders........... 130
58 Ambient air quality surveillance............ 204
59
[Reserved]
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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 F-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 Supbart 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............. .................. > >
PM2.5............................... Reference............. Manual................ L >
[[Page 19]]
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
[[Page 20]]
range. Appropriate test data shall be submitted for each range sought to
be included in a reference or equivalent 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
[[Page 21]]
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, 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
[[Page 24]]
diluted with zero air to the final required concentration.
(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
(Rj), g/m3............. 30-300 10-200 10-200
Minimum number of test sites..... 2 1 2
Number of candidate method
samplers per site............... 3 3 3
Number of reference method
samplers per site............... 3 3 3
Minimum number of acceptable
sample sets per site for PM10:
Rj 80 g/m3......... 3
Rj > 80 g/m3........ 3
Total.................... 10
Minimum number of acceptable
sample sets per site for PM2.5:
[[Page 46]]
Single test site for Class I
candidate equivalent
methods:
Rj 40 g/m3 for
24-hr or Rj 30 g/m3 for 48-hr samples 3
Rj > 40 g/m3 for
24-hr or Rj > 30 g/m3 for 48-hr samples 3
Sites at which the PM2.5/PM10
ratio must be > 0.75:
Rj 40 g/m3 for
24-hr or Rj 30 g/m3 for 48-hr samples 3
Rj > 40 g/m3 for
24-hr or Rj > 30 g/m3 for 48-hr samples 3
Sites at which the PM2.5/PM10
ratio must be 0.40:
Rj 30 g/m3 for
24-hr or Rj 20 g/m3 for 48-hr samples 3
Rj > 30 g/m3 for
24-hr or Rj > 20 g/m3 for 48-hr samples 3
Total, each site................. 10 10
Precision of replicate reference
method measurements, Pj or RPj
respectively, maximum........... 5 g/m3 or
7% 2 g/m3 or
5% 2 g/m3 or
5%
Slope of regression relationship. 1g/m3..... 0
0.97
0.97