EPA-340/1 -82-005a Standards of Performance for New Stationary
United States Office of Air Quality Planning EPA-340/1 -82-005a
Environmental Protection and Standards June 1982
Agency Washington DC 20460
Stationary Source Compliance Series
<>EPA Standards
of Performance
for New Stationary
Sources -
Volume 1:
Introduction,
Summary and
Standards
A Compilation
As of May 1, 1982
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EPA-340/1-82-005a
Standards of Performance
for New Stationary Sources -
Volume 1 :
Introduction, Summary and Standards
A Compilation as of May 1, 1982
by
PEDCo Environmental, Inc.
Cincinnati, Ohio 45246
Contract No. 68-01-6310
EPA Project Officer: Kirk Foster
Prepared for .
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Air, Noise and Radiation
Stationary Source Compliance Division
Washington, D.C. 20460
June 1982
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The Stationary Source Compliance series of reports is issued by the Office of
Air, Noise and Radiation, U.S. Environmental Protection Agency, to assist the
Regional Offices in activities related to compliance with implementation
plans, new source emission standards, and hazardous emission standards to be
developed under the Clean Air Act. Copies of Stationary Source Compliance
reports are available - as supplies permit - from the U.S. Environmental
Protection Agency, Office of Administration, General Services Division, MD-35,
Research Triangle Park, North Carolina 27711, or may be obtained, for a nomi-
nal cost, from the National Technical Information Service, 5285 Port Royal
Road, Springfield, Virginia 22151.
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PREFACE
This document is a compilation of the New Source Performance Standards
promulgated under Section 111 of the Clean Air Act, represented in full as
amended. The information contained herein supersedes all previous compila-
tions published by the U.S. Environmental Protection Agency prior to 1982.
The format of this document permits easy and convenient replacement of
material as new standards are proposed or promulgated or existing standards
revised. However, the increase in size since the previous compilation has
necessitated division into three volumes: Volume 1 contains Sections I
through III; Volume 2 contains only Section IV; Volume 3 contains Section V.
Section I is an introduction to the standards and explains their purpose and
interprets the working concepts which have developed through their imple-
mentation. Section II contains a "quick-look" summary of each standard,
including the dates of proposal, promulgation, and any subsequent revisions.
Section III is the complete standards with all amendments incorporated into
the material. Each amendment is referenced to the specific full text in
Section V. Section IV (Volume 2) has all proposed amendments divided by
section affected. It also contains a complete list of proposed regulations,
including Reference Methods and Performance Specifications. Section V (Volume
3) is the full text of all revisions, including the preamble which explains
the rationale behind each revision. It also contains a chronological list of
all Federal Register activity pertaining to the New Source Performance Stan-
dards. To facilitate the addition of future materials, the punched, loose-
leaf format was selected. This approach permits the document to be placed in
i i 1
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a three-ring binder or to be secured by rings, rivets, or other fasteners;
future revisions can then be easily inserted.
Future supplements to New Source Performance Standards - A Compilation
will be issued on an as needed basis by the Stationary Source Compliance
Division. Comments and suggestions regarding this document should be directed
to: Standards Handbooks, Stationary Source Compliance Division (EN-341), U.S.
Environmental Protection Agency, Washington, D.C. 20460.
iv
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TABLE OF CONTENTS
VOLUME 1
I. INTRODUCTION TO STANDARDS OF PERFORMANCE FOR NEW
STATIONARY SOURCES
II. SUMMARY OF STANDARDS AND REVISIONS
III. PART 60 - STANDARDS OF PERFORMANCE FOR NEW
STATIONARY SOURCES
SUBPART A - GENERAL PROVISIONS
Section
60.1 Applicability
60.2 Definitions
60.3 Abbreviations
60.4 Address
60.5 Determination of construction or modification
60.6 Review of plans
60.7 Notification and recordkeeping
60.8 Performance tests
60.9 Availability of information
60.10 State authority
60.11 Compliance with standards and'maintenance requirements
60.12 Circumvention
60.13 Monitoring requirements
60.14 Modification
60.15 Reconstruction
60.16 Priority List
Page
1-1
II-l
III-l
III-4
III-4
III-4
III-5
111-10
111-10
111-10
111-10
III-ll
III-ll
III-ll
III-ll
III-ll
111-13
111-14
111-14
Section
60.20
60.21
60.22
SUBPART B - ADOPTION AND SUBMITTAL OF STATE PLANS
FOR DESIGNATED FACILITIES
Applicability 111-15
Definitions 111-15
Publication of guideline documents, emission guidelines, 111-15
final compliance times
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TABLE OF CONTENTS
Section Page
60.23 Adoption and submittal of state plans; public hearings 111-15
60.24 Emission standards and compliance schedules 111-16
60.25 Emission inventories, source surveillance reports 111-16
60.26 Legal authority 111-17
60.27 Actions by the Administrator 111-17
60.28 Plan revisions by the State 111-17
60.29 Plan revisions by the Administrator 111-17
SUBPART C - EMISSION GUIDELINES AND COMPLIANCE TIMES 111-18
SUBPART D - STANDARDS OF PERFORMANCE FOR FOSSIL-FUEL-FIRED
STEAM GENERATORS FOR WHICH CONSTRUCTION IS
COMMENCED AFTER AUGUST 17, 1971
Section
60.40 Applicability and designation of affected facility 111-19
60.41 Definitions III-19
60.42 Standard for particulate matter 111-19
60.43 Standard for sulfur dioxide 111-19
60.44 Standard for nitrogen oxides 111-19
60.45 Emission and fuel monitoring 111-20
60.46 Test methods and procedures III-21
60.47 Innovative technology waivers 111-22
APPENDIX I - DETERMINATION OF SULFUR DIOXIDE EMISSIONS FROM FOSSIL
FUEL FIRED COMBUSTION SOURCES (Continuous Bubbler
Method)
111-31
Section
60.40a
60.41a
60.42a
SUBPART Da - STANDARDS OF PERFORMANCE FOR ELECTRIC UTILITY
STEAM GENERATING UNITS FOR WHICH CONSTRUCTION IS
COMMENCED AFTER SEPTEMBER 18, 1978
Applicability and designation of affected facility
Definitions
Standard for particulate matter
vi
111-33
111-33
111-34
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TABLE OF CONTENTS
Section
60.43a Standard for sulfur dioxide
60.44a Standard for nitrogen oxides
60.45a Commercial demonstration permit
60.46a Compliance provisions
60.47a Emission monitoring
60.48a Compliance determination procedures and methods
60.49a Reporting requirements
Page
111-34
111-35
111-35
111-36
111-36
111-37
111-38
Section
60.50
60.51
60.52
60.53
60.54
SUBPART E - STANDARDS OF PERFORMANCE FOR INCINERATORS
Applicability and designation of affected facility 111-40
Definitions 111-40
Standard for particulate matter 111-40
Monitoring of operations 111-40
Test methods and procedures II1-40
Section
60.60
60.61
60.62
60.63
60.64
SUBPART F - STANDARDS OF PERFORMANCE FOR PORTLAND
CEMENT PLANTS
Applicability and designation of affected facility 111-41
Definitions 111-41
Standard for particulate 111-41
Monitoring of operations 111-41
Test methods and procedures II1-41
Section
60.70
60.71
60.72
SUBPART G - STANDARDS OF PERFORMANCE FOR
NITRIC ACID PLANTS
Applicability and designation of affected facility
Definitions
Standard for nitrogen oxides
111-42
111-42
111-42
vi i
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TABLE OF CONTENTS
Section
60.73
60.74
Emission monitoring
Test methods and procedures
Page
111-42
111-42
Section
60.80
60.81
60.82
60.83
60.84
60.85
SUBPART H - STANDARDS OF PERFORMANCE FOR
SULFURIC ACID PLANTS
Applicability and designation of affected facility
Definitions
Standard for sulfur dioxide
Standard for acid mist
Emission monitoring
Test methods and procedures
111-43
111-43
111-43
111-43
111-43
111-43
Section
60.90
60.91
60.92
60.93
SUBPART I - STANDARDS OF PERFORMANCE FOR
ASPHALT CONCRETE PLANTS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Test methods
111-44
111-44
111-44
111-44
SUBPART 0 - STANDARDS OF PERFORMANCE FOR
PETROLEUM REFINERIES
Section
60.100 Applicability and designation of affected facility
60.101 Definitions
60.102 Standard for particulate matter
60.103 Standard for carbon monoxide
60.104 Standard for sulfur dioxide
60.105 Emission monitoring
60.106 Test methods and procedures
111-45
111-45
111-45
111-45
111-45
111-45
II1-46
vm
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TABLE OF CONTENTS
Page
Section
60.110
60.111
60.112
60.113
SUBPART K - STANDARDS OF PERFORMANCE FOR STORAGE VESSELS
FOR PETROLEUM LIQUIDS CONSTRUCTED AFTER JUNE 11, 1973,
AND PRIOR TO MAY 19, 1978
Applicability and designation of affected facility
Definitions
Standard for volatile organic compounds (VOC)
Monitoring of operations
111-48
111-48
111-48
111-48
Section
60.110a
60.Ilia
60.112a
60.113a
60.114a
60.115a
SUBPART Ka - STANDARDS OF PERFORMANCE FOR STORAGE VESSELS
FOR PETROLEUM LIQUIDS CONSTRUCTED AFTER MAY 18, 1978
Applicability and designation of affected facility 111-49
Definitions 111-49
Standard for volatile organic compounds (VOC) 111-49
Testing and procedures 111-50
Equivalent equipment and procedures 111-50
Monitoring of operations 111-51
Section
60.120
60.121
60.122
60.123
SUBPART L - STANDARDS OF PERFORMANCE FOR
SECONDARY LEAD SMELTERS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Test methods and procedures
111-52
111-52
111-52
111-52
IX
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TABLE OF CONTENTS
Page
Section
60.130
60.131
60.132
60.133
SUBPART M - STANDARDS OF PERFORMANCE FOR SECONDARY
BRASS AND BRONZE INGOT PRODUCTION PLANTS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Test methods and procedures
111-53
111-53
111-53
111-53
Section
60.140
60.141
60.142
60.143
60.144
SUBPART N - STANDARDS OF PERFORMANCE FOR
IRON AND STEEL PLANTS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Monitoring of operations
Test methods and procedures
111-54
111-54
111-54
111-54
111-54
Section
60.150
60.151
60.152
60.153
60.154
SUBPART 0 - STANDARDS OF PERFORMANCE FOR
SEWAGE TREATMENT PLANTS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Monitoring of operations
Test methods and procedures
111-55
111-55
111-55
111-55
111-55
Section
60.160
60.161
SUBPART P - STANDARDS OF PERFORMANCE FOR
PRIMARY COPPER SMELTERS
Applicability and designation of affected facility
Definitions
111-56
111-56
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TABLE OF CONTENTS
60.162 Standard for participate matter
60.163 Standard for sulfur dioxide
60.164 Standard for visible emissions
60.165 Monitoring of operations
60.166 Test methods and procedures
Page
111-56
111-56
111-56
111-56
111-57
SUBPART Q - STANDARDS OF PERFORMANCE FOR
PRIMARY ZINC SMELTERS
Section
60.170 Applicability and designation of affected facility
60.171 Definitions
60.172 Standard for particulate matter
60.173 Standard for sulfur dioxide
60.174 Standard for visible emissions
60.175 Monitoring of operations
60.176 Test methods and procedures
111-58
111-58
111-58
111-58
111-58
III-58
111-58
SUBPART R - STANDARDS OF PERFORMANCE FOR
PRIMARY LEAD SMELTERS
Section
60.180 Applicability and designation of affected facility
60.181 Definitions
60.182 Standard for particulate matter
60.183 Standard for sulfur dioxide
60.184 Standard for visible emissions
60.185 Monitoring of operations
60.186 Test methods and procedures
111-59
111-59
111-59
111-59
111-59
111-59
111-59
XI
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TABLE OF CONTENTS
Page
Section
60.190
60.191
60.192
60.193
60.194
60.195
SUBPART S - STANDARDS OF PERFORMANCE FOR
PRIMARY ALUMINUM REDUCTION PLANTS
Applicability and designation of affected facility
Definitions
Standard for fluorides
Standard for visible emissions
Monitoring of operations
Test methods and procedures
111-60
111-60
111-60
111-60
111-60
111-60
Section
60.200
60.201
60.202
60.203
60.204
SUBPART T - STANDARDS OF PERFORMANCE FOR PHOSPHATE
FERTILIZER INDUSTRY: WET PROCESS PHOSPHORIC ACID PLANTS
Applicability and designation of affected facility 111-62
Definitions 111-62
Standard for fluorides 111-62
Monitoring of operations 111-62
Test methods and procedures 111-62
Section
60.210
60.211
60.212
60.213
60.214
SUBPART U - STANDARDS OF PERFORMANCE FOR PHOSPHATE
FERTILIZER INDUSTRY: SUPERPHOSPHORIC ACID PLANTS
Applicability and designation of affected facility 111-63
Definitions 111-63
Standard for fluorides 111-63
Monitoring of operations 111-63
Test methods and procedures 111-63
XII
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TABLE OF CONTENTS
Page
Section
60.220
60.221
60.222
60.223
60.224
SUBPART V - STANDARDS OF PERFORMANCE FOR PHOSPHATE
FERTILIZER INDUSTRY:' DIAMMONIUM PHOSPHATE PLANTS
Applicability and designation of affected facility
Definitions
Standard for fluorides
Monitoring of operations
Test methods and procedures
111-64
111-64
111-64
111-64
111-64
Section
60.230
60.231
60.232
60.233
60.234
SUBPART W - STANDARDS OF PERFORMANCE FOR PHOSPHATE
FERTILIZER INDUSTRY: TRIPLE SUPERPHOSPHATE PLANTS
Applicability and designation of affected facility 111-65
Definitions 111-65
Standard for fluorides 111-65
Monitoring of operations 111-65
Test methods and procedures 111-65
Section
60.240
60.241
60.242
60.243
60.244
SUBPART X - STANDARDS OF PERFORMANCE FOR THE PHOSPHATE
FERTILIZER INDUSTRY: GRANULAR TRIPLE SUPERPHOSPHATE
STORAGE FACILITIES
Applicability and designation of affected facility 111-66
Definitions 111-66
Standard for fluorides 111-66
Monitoring of operations 111-66
Test methods and procedures 111-66
xm
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TABLE OF CONTENTS
Page
Section
60.250
60.251
60.252
60.253
60.254
SUBPART Y - STANDARDS OF PERFORMANCE FOR
COAL PREPARATION PLANTS
Applicability and designation of affected facility
Definitions
Standards for participate matter
Monitoring of operations
Test methods and procedures
111-67
111-67
111-67
111-67
111-67
SUBPART Z - STANDARDS OF PERFORMANCE FOR FERROALLOY
PRODUCTION FACILITIES
Section
60.260 Applicability and designation of affected facility 111-68
60.261 Definitions 111-68
60.262 Standard for participate matter 111-68
60.263 Standard for carbon monoxide 111-68
60.264 Emission monitoring 111-68
60.265 Monitoring of operations 111-68
60.266 Test methods and procedures 111-69
Section
60.270
60.271
60.272
60.273
60.274
60.275
SUBPART AA - STANDARDS OF PERFORMANCE FOR STEEL
PLANTS: ELECTRIC ARC FURNACES
Applicability and designation of affected facility 111-71
Definitions 111-71
Standard for particulate matter 111-71
Emission monitoring 111-71
Monitoring of operations 111-71
Test methods and procedures 111-72
xiv
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TABLE OF CONTENTS
Page
Section
60.280
60.281
60.282
60.283
60.284
60.285
SUBPART BB - STANDARDS OF PERFORMANCE
FOR KRAFT PULP MILLS
Applicability and designation of affected facility
Definitions
Standard for ^articulate matter
Standard for total reduced sulfur (TRS)
Monitoring of emissions and operations
Test methods and procedures
111-73
111-73
111-73
111-73
111-74
111-74
SUBPART CC - STANDARDS OF PERFORMANCE FOR
GLASS MANUFACTURING PLANTS
Section
60.290 Applicability and design of affected facility
60.291 Definitions
60.292 Standards for particulate matter
60.293 Reserved
60.294 Reserved
60.295 Reserved
60.296 Test methods and procedures
111-76
111-76
111-76
111-76
111-76
111-76
111-76
Section
60.300
60.301
60.302
60.303
60.304
SUBPART DD - STANDARDS OF PERFORMANCE
FOR GRAIN ELEVATORS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Test methods and procedures
Modification
111-78
111-78
111-78
111-78
111-78
xv
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TABLE OF CONTENTS
Page
Section
60.330
60.331
60.332
60.333
60.334
60.335
SUBPART GG - STANDARDS OF PERFORMANCE
FOR STATIONARY GAS TURBINES
Applicability and designation of affected facility
Definitions
Standard for nitrogen oxides
Standard for sulfur dioxide
Monitoring of operations
Test methods and procedures
111-80
II1-80
111-80
111-81
111-81
111-81
Section
60.340
60.341
60.342
60.343
60.344
SUBPART HH - STANDARDS OF PERFORMANCE
FOR LIME MANUFACTURING PLANTS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Monitoring of emissions and operations
Test methods and procedures
111-83
111-83
111-83
111-83
111-83
Section
60.370
60.371
60.372
60.373
60.374
SUBPART KK - STANDARDS OF PERFORMANCE FOR
LEAD-ACID BATTERY MANUFACTURING PLANTS
Applicability and designation of affected facility
Definitions
Standards for lead
Monitoring of emissions and operations
Test methods and procedures
111-84
111-84
111-84
111-84
111-84
xvi
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TABLE OF CONTENTS
Page
SUBPART MM - STANDARDS OF PERFORMANCE FOR
AUTOMOBILE AND LIGHT-DUTY TRUCK SURFACE COATING OPERATIONS
Section
60.390 Applicability and designation of affected facility 111-86
60.391 Definitions 111-86
60.392 Standards for volatile organic compounds 111-87
60.393 Performance test and compliance provisions 111-87
60.394 Monitoring of emissions and operations 111-88
60.395 Reporting and recordkeeping requirements 111-88
60.396 Reference methods and procedures 111-89
60.397 Modifications 111-89
Section
60.400
60.401
60.402
60.403
60.404
SUBPART NN - STANDARDS OF PERFORMANCE FOR
PHOSPHATE ROCK PLANTS
Applicability and designation of affected facility
Definitions
Standard for particulate matter
Monitoring of emissions and operations
Test methods and procedures
111-90
111-90
111-90
111-90
111-90
SUBPART PP - STANDARDS OF PERFORMANCE
FOR AMMONIUM SULFATE MANUFACTURE.
60.420 Applicability and designation of affected facility
60.421 Definitions
60.422 Standards for particulate matter
60.423 Monitoring of operations
60.424 Test methods and procedures
111-92
111-92
111-92
111-92
111-92
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TABLE OF CONTENTS
APPENDIX A - REFERENCE METHODS
Method 1 - Sample and velocity traverses for stationary
sources
Method 2 - Determination of stack gas velocity and volumetric
flow rate (Type S Pi tot Tube)
Method 3 - Gas analysis for carbon dioxide, excess air, and
dry molecular weight
Method 4 - Determination of moisture in stack gases
Method 5 - Determination of particulate emissions from
stationary sources
Method 6 - Determination of sulfur dioxide emissions from
stationary sources
Method 7 - Determination of nitrogen oxide emissions from
stationary sources
Method 8 - Determination of sulfuric acid mist and sulfur
dioxide emissions from stationary sources
Method 9 - Visual determination of the opacity of emissions
from stationary sources
Alternate Method 1 - Determination of the opacity of emissions
from stationary sources remotely by Lidar
Method 10 - Determination of carbon monoxide emissions from
stationary sources
i
Method 11 - Determination of hydrogen sulfide content of fuel
gas streams in petroleum refineries
Method 12 - Determination of inorganic lead emissions from
stationary sources
Method ISA - Determination of total fluoride emissions from
stationary sources - SPADNS Zirconium Lake Method
Method 13B - Determination of total fluoride emissions from
stationary sources - Specific Ion Electrode
method
Method 14 - Determination of fluoride emissions from potroom
roof monitors of primary aluminum plants
Page
Ill-Appendix A-l
Ill-Appendix A-4
Ill-Appendix A-14
Ill-Appendix A-17
Ill-Appendix A-21
Ill-Appendix A-28
Ill-Appendix A-30
Ill-Appendix A-33
Ill-Appendix A-36
Ill-Appendix A-40
Ill-Appendix A-54
Ill-Appendix A-56
III-Appendis A-60
Ill-Appendix A-65
Ill-Appendix A-70
Ill-Appendix A-72
xvm
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TABLE OF CONTENTS
Method 15 - Determination of hydrogen sulfide, carbonyl
sulfide, and carbon desulfide emissions from
stationary sources
Method 16 - Semicontinuous determination of sulfur emissions
from stationary sources
Method 17 - Determination of particulate emissions from
stationary sources (in-stack filtration method)
Method 19 - Determination of sulfur dioxide removal
efficiency and particulate, sulfur dioxide and
nitrogen oxides emission rates from electric
utility steam generators
Method 20 - Determination of nitrogen oxides, sulfur dioxide,
and oxygen emissions from stationary gas turbines
Method 24 - Determination of volatile matter content, water
content, density, volume solids, and weight solids
of surface coatings
Method 25 - Determination of total gaseous nonmethane organic
emissions as carbon
APPENDIX B - PERFORMANCE SPECIFICATIONS
APPENDIX C - DETERMINATION OF EMISSION RATE CHANGE
APPENDIX D - REQUIRED EMISSION INVENTORY INFORMATION
ADDENDUM 1 - TABLE OF CONTENTS, VOLUME 2
ADDENDUM 2 - TABLE OF CONTENTS, VOLUME 3
VOLUME 2 - PROPOSED AMENDMENTS (Section IV)
VOLUME 3 - FULL TEXT OF REVISIONS (Section V)
Page
Ill-Appendix A-80
Ill-Appendix A-83
Ill-Appendix A-91
Ill-Appendix A-102
Ill-Appendix A-108
Ill-Appendix A-115
Ill-Appendix A-116
Ill-Appendix B-l
Ill-Appendix C-l
Ill-Appendix D-l
xix
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I. INTRODUCTION
Building on prior Federal, State, and local control agency legislation
and experience, the Clean Air Act of 1970 authorized a national program of air
pollution prevention and control. This program included national ambient
standards and State implementation plans; emission standards for mobile
sources; fuel additive standards; hazardous pollutant standards; and—for the
first time—nationwide, uniform, technology-based standards of performance for
new and modified stationary sources. The standards in this latter category,
which are authorized by Section 111 of the Act, are commonly referred to as
New Source Performance Standards (NSPS). The Clean Air Act amendments of 1977
reinforced the provisions of the NSPS by requiring the preparation of a list
of all major stationary sources and the promulgation of standards for these
sources.
The major purpose of Section 111 of the Clean Air Act is to prevent new
air pollution problems. Consistent with this, the section requires that
standards of performance reflect the degree of emission control achievable by
application of the best system of continuous emission reduction that the
Administrator determines has been adequately demonstrated, taking into con-
sideration cost, health and environmental impacts not related to air quality,
and energy requirements. This technology is commonly referred to as best
demonstrated technology (BDT). The NSPS apply to specific equipment and
processes and apply only to those units that are constructed, reconstructed,
1-1
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or modified after the proposal date of the respective standard. Because NSPS
regulate performance, the owner or operator of a source may select any control
system desired as long as it achieves the standard.
In terms of air quality benefits, NSPS complement the ambient air
quality/ State Implementation Plan (SIP) programs by preventing degradation of
ambient air quality while allowing maximum opportunity for industrial growth.
These standards also indirectly limit emissions of toxic and potentially
hazardous compounds and, by limiting sulfur dioxide (SCO and nitrogen oxides
(NO ), reduce the potential for acid rain.
X
The development of NSPS involves a detailed technical and economic inves-
tigation of a source category. During this investigation, process and cost
information is obtained, emission tests are performed, and alternatives are
analyzed. The findings are documented in a background information document
(BID) which is reviewed for technical accuracy by the affected industries and
by other interested outside organizations. Before the NSPS are proposed, they
are submitted in draft form, along with the BID's, to the National Air Pollu-
tion Control Techniques Advisory Committee for review. This committee is made
up of experts representing industry, control agencies, and environmental
public interest groups. The proposed standards are then published in the
Federal Register, and the BID's are made available for public comment. A
public hearing is held and formal comments are received before final adoption
of the standards.
Persons affected by an NSPS should refer to the respective BID's for a
more detailed background of the technology and performance reflected by the
standards. A limited printing of these documents is made at the time each
standard is developed and copies are available, until supplies are exhausted,
1-2
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by contacting: U.S. EPA Library Services (MD-35), U.S. Environmental Protec-
tion Agency, Research Triangle Park, North Carolina 27711, (919) 541-2777.
Copies are also available through the National Technical Information Service
(NTIS).
The NSPS development process, by providing industry and other interested
groups an opportunity to focus their attention and resources on technology-
based standards for specific source categories in a single forum, permits more
effective and efficient use of resources than would be possible in case-by-
case determinations. The technical and economic documentation that is devel-
oped through this process not only reduces uncertainty, but also the time and
resources required to reach any subsequent case-by-case determinations re-
quired by State and local regulations or other sections of the Clean Air Act.
As more sources of pollution are investigated and new technology is developed,
the New Source Performance Standards will continue to be updated to achieve
their primary purpose of preventing new air pollution problems.
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SECTION II
SUMMARY OF STANDARDS
AND REVISIONS
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II. SUMMARY OF STANDARDS AND REVISIONS
In order to make the information in this document more easily accessi-
ble, a summary has been prepared of all New Source Performance Standards
promulgated since their inception in December 1971. Anyone who must use the
Federal Register frequently to refer to regulations published by Federal
agencies is well aware of the problems of sifting through the many pages to
extract the "meat" of a regulation. Although regulatory language is neces-
sary to make the intent of a regulation clear, a more concise reference to
use when looking up a particular standard would be helpful. With this in
mind, the following table was developed to assist those who work with the
NSPS. It includes the categories of stationary sources and the affected
facilities to which the standards apply; the pollutants which are regulated
and the levels to which they must be controlled; and the requirements for
monitoring emissions and operating parameters.
Before developing standards for a particular source category, EPA must
first identify the pollutants emitted and determine that they contribute
significantly to air pollution which endangers public health or welfare.
The standards are then developed and proposed in the Federal Register.
After a period of time during which the public is encouraged to submit
comments to the proposal, appropriate revisions are made to the regulations
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-------
and they are promulgated in the Federal Register. To cite such a promulga-
tion, it is common to refer to it by volume and page number, i.e., 36 FR
24876, which means Volume 36, Page 24876 of the Federal Register. The table
gives such references for the proposal, promulgation, and subsequent revi-
sions of each standard listed.
This summary is provided as a "quick reference" only and should not be
used for enforcement purposes or regulatory determination. Please refer to
the standards in Section III or the full text of promulgated regulations in
Section V (Volume 3) for complete details concerning the New Source Perform-
ance Standards.
II-2
-------
Source category
Subpart D - Fossil -Fuel Fired
Steam Generators for Which
Construction is Commenced
After August 17, 1971
Proposed/effective
8/17/71 (36 FR 15704)
Promulgated
12/23/71 (36 FR 24876)
Revised
7/26/72 (37 FR 14877)
10/15/73 (38 FR 28564)
6/14/74 (39 FR 20790)
1/16/75 (40 FR 2803)
10/6/75 (40 FR 46250)
12/22/75 (40 FR 59204)
11/22/76 (41 FR 51397)
1/31/77 (42 FR 5936)
7/25/77 (42 FR 37936)
8/15/77 (42 FR 41122)
8/17/77 (42 FR 41122)
12/5/77 (42 FR 61537)
3/3/78 (43 FR 8800)
3/7/78 (43 FR 9276)
1/17/79 (44 FR 3491)
6/11/79 (44 FR 33580)
12/28/79 (44 FR 76786)
2/6/80 (45 FR 8211)
5/29/80 (45 FR 36077)
7/14/80 (45 FR 47146)
11/13/81 (46 FR 55975)
11/24/81 (46 FR 57497)
1/15/82 (47 FR 2314)
Affected
facility
Coal , coal /wood
residue fired boilers
>250 million Btu/h
Oil, oil/wood residue
fired boilers
>250 million Btu/h
Gas, gas/wood residue
fired boilers
>250 million Btu/h
Mixed fossil fuel
fired boilers
>250 million Btu/h
Lignite, lignite/wood
residue
>250 million Btu/h
Pollutant
Particulate
Opacity
S0?
N0x
Particulate
Opacity
so2
N0x
Particulate
Opacity
NO
X
Particulate
Opacity
S02
NOX (except lignite
or 25/c coal refuse)
Particulate
Opacity
S02
NOX (as of 12/22/76)
Emission level
c
0.10 lb/10° Btu
20» ; 27% 6 min/h*
1.2 lb/106 Btu
0.70 lb/10b Btu
0.10 lb/106 Btu
20%; 27Z 6,min/h
0.80 lb/10? Btu
0.30 lb/10 Btu
f
0.10 lb/10 Btu
20%; 27S 6,min/h
0.20 lb/10 Btu
C
0.10 lb/10° Btu
20'o; 27"- 6 min/h
Prorated
Prorated
c
0.10 lb/10° Btu
202; 27:;. 6 min/h
1.2 lb/106 Btu
0.60 lb/10
-------
Source category
Subpart Da - Electric
utility steam gen-
erating units for
which construction
is commenced after
September 18, 1978
Proposed/effective
9/19/78 (43 FR 42154)
Promulgated
6/11/79 (44 FR 33580)
Revised
2/6/80 (45 FR 8211)
Affected facility
Boilers >73 MW
(>250 million
Btu/h) firing
solid and solid
derived fuel
Pollutant
Particulate
Opacity
S02
S02 - solvent
refined coal
S02 - 100%
anthracite;
non- conti-
nental
NOX - coal de-
rived fuels;
subbi luminous;
shale oil
NOX - >25%
lignite mined
in ND, SO, MT,
combusted in
slag tap
furnace
NOX - lignite;
bituminous
anthracite;
other fuels
Emission level
13 ng/J (0.03 Ib/mil-
lion Btu)
20%; 27% 6 min/h
520 ng/J (1.20 lb/
million Btu)
or
<260 ng/J (0.60 lb/
million Btu)
520 ng/J (1.20 lb/
million Btu)
520 ng/J (1.20 lb/
million Btu)
210 ng/J (0.50 lb/
million Btu)
340 ng/J (0.80 lb/
million Btu)
260 ng/J (0.60 lb/
million Btu)
Potential '
combustion
concentration
3000 ng/J (7.0
Ib/million Btu)
See 60.48a(b)
See 60.48a(b)
See 60.48a(b)
S90 ng/J (2.30
Ib/million Btu)
990 ng/J (2.30
Ib/million Btu)
990 ng/J (2.30
Ib/million Btu) •
Reduction of
potential com-
bustion con-
centration, %
99
90
70
85
Exempt
65
65
65
Monitoring
requirement
No requirement
Continuous
Continuous
Continuous
Continuous
Continuous
Continuous
Continuous
Continuous
-------
I
in
Source category
Affected facility
Boilers >73 MW
(>250 million
Btu/h) firing
liquid fuel
Boilers >73 MW
(>250 million Btu)
firing gaseous
fuels
Pollutant
Particulate
Opacity
so2
£.
SO? (non-
continental )
NO
X
Particulate
Opacity
S02
c
S02 (non-
continental )
NO,
X
Emission level
13 ng/J (0.03 lb/
million Btu)
20%; 27% 6 min/h
340 ng/J (0.80 lb/
million Btu)
or
<86 ng/J (0.20 lb/
million Btu)
340 ng/J (0.80 lb/
million Btu)
130 ng/J (0.30 lb/
million Btu)
13 ng/J (0.03 lb/
million Btu)
20%; 27% 6 min/h
340 ng/J (0.80 lb/
million Btu)
or
<86 ng/J (0.20 lb
million Btu)
340 ng/J (0.80 lb/
million Btu)
86 ng/J (0.20 lb/
million Btu)
Potential '
combustion
concentration
75 ng/J (0.17
Ib/million Btu)
See 60.48a(b)
See 60.48a(b)
See 60.48a(b)
310 ng/J (0.72
Ib/million Btu)
See 60.48a(b)
See 60.48a(b)
See 60.48a(b)
290 ng/J (0.67
Ib/million Btu)
Reduction of
potential com-
bustion con-
centration, %
70
90
0
Exempt
30
90
0
Exempt
25
Monitoring
requirement
No requirement
Continuous
Continuous
Continuous
Continuous
Continuous
No requirement
No requirement
Continuous*
Continuous*
Continuous*
Continuous
*Except when using only natural gas.
-------
Source category
Subpart E - Incinerators
Proposed/effective
8/17/71 (36 FR 15704)
Promulgated
12/23/71 (36 FR 24876)
Revised
6/14/74 (36 FR 20790)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart F - Portland Cement
Plants
Proposed/effective
8/17/71 (36 FR 15704)
Promulgated
12/23/71 (36 FR 24876)
Revised
6V14/74 (39 FR 20790)
11/12/74 (39 FR 39872)
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Affected
facility
Incinerators
>50 tons/day
Kiln
Clinker cooler
Fugitive emission
points
Pollutant
Particulate
Particulate
Opacity
Particulate
Opacity
Opacity
Emission level
0.08 gr/dscf (0.18
g/dscm) corrected
to 12" C02
0.30 Ib/ton
20%
0.10 Ib/ton
10%
10?;
Monitoring
requirement
No requirement
Daily charging
rates and hours
No requirement
No requirement
No requirement
No requirement
Mo requirement
Daily production
and feed kiln
rates
-------
I
•vj
Source category
Subpart G - Nitric Acid Plants
Proposed/effective
8/17/71 (36 FR 15704)
Promulgated
12/23/71 (36 FR 24876)
Revised
5/23/73 (38 FR 13562)
10/15/73 (38 FR 28564)
6/14/74 (39 FR 20790)
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart H - Sulfuric Acid Plants
Proposed/effective
8/17/71 (36 FR 15704)
Promulgated
12/23/71 (36 FR 24876)
Revised
5/23/73 (38 FR 13562)
10/15/73 (38 FR 28564)
6/14/74 (39 FR 20790)
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Affected
facility
Process equipment
Process equipment
•
Pollutant
Opacity
N0y
X
SO
£
Acid mist
Opacity
Emission level
10%
3.0 Ib/ton
4.0 Ib/ton
0.15 Ib/ton
10%
Monitoring
requirement
No requirement
Continuous
Daily production
rates and hours
Continuous
No requirement
No requirement
-------
I
00
Source category
Subpart I - Asphalt Concrete
Plants
Proposed/effective
6/11/73 (38 FR 15406)
Promulgated
3/8/74 (39 FR 9308)
Revised
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
8/31/79 (44 FR 51225)
Reviewed
8/31/79 (44 FR 51225)
Subpart J - Petroleum Refineries
Proposed/effective
6/11/73 (38 FR 15406)
10/4/76 (41 FR 43866)
Promulgated
3/8/74 (39 FR 9308)
Revised
10/6/75 (40 FR 46250)
6/24/77 (42 FR 32426)
7/25/77 (42 FR 37936)
8/4/77 (42 FR 39389)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
3/15/78 (43 FR 10866)
3/12/79 (44 FR 13480)
10/25/79 (44 FR 61542)
12/1/80 (45 FR 79452)
Affected
facility
Dryers; screening and
weighing systems;
storage, transfer,
and loading systems;
dust handling equip-
ment
Catalytic cracker
(with incinerator or
waste heat boiler)
Fuel gas
combustion
Claus sulfur recovery
plants >20 LTD/day
(as of 10/4/76)
Pollutant
Particulate
Opacity
Particulate
Opacity
CO
SO
c.
so
£
Emission level
0.04 gr/dscf
(90 mg/dscm)
20?:
1.0 lb/1000 Ib
(1.0 kg/1000 kg)
Additional 0.10
lb/106 Btu (43.0
g/MJ)
30%; 6 min. exemption
0.05%
0.10 gr H2S/dscf
(230 mg/dscm) fuel
gas content
0.025% with oxidation
or reduction and in-
cineration; 0.0302 with
reduction only
Monitoring
requirement
No requirement
No requirement
No requirement
No requirement
Continuous
Continuous
Continuous
Continuous
Continuous
-------
Source category
Subpart K - Storage Vessels for
Petroleum Liquids Constructed
After June 11, 1973 and Prior
to May 19, 1978
Proposed/effective
6/11/73 (38 FR 15406)
Promulgated
3/8/74 (39 FR 9308)
Revised
4/17/74 (39 FR 13776)
6/14/74 (39 FR 20790)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
4/4/80 (45 FR 23374)
Affected
facility
Storage tanks
>65,000 gal. capacity
(246,052 liters) as
of 6/11/73
and
>40,000 gal . capacity
(151,412 liters) as
of 3/8/74
Pollutant
Volatile organic
compounds (VOC)
Emission level
Vapor pressure
1.5-11.1 psia (78-
570 mm Hg), equip
with floating roof,
vapor recovery
system, or equiv-
alent
Vapor pressure >11 .1
psia (570 mm Hg),
equip with vapor
recovery system or
equivalent
Monitoring
requirement
No requirement
No requirement
Type of liquid, period
of storage and maximum
vapor pressure
-------
Source category
Affected
facility
Pollutant
Emission level
Monitoring
requirement
i
o
Subpart Ka - Storage Vessels for
Petroleum Liquids Constructed
After May 18, 1978
Proposed/effective
5/18/78 (43 FR 21616)
Promulgated
4/4/80 (45 FR 23374)
Revised
12/18/80 (45 FR 83228)
Storage tanks
>40,000 gal. capacity
(151,416 liters)
Volatile organic
compounds (VOC)
Vapor pressure
1.5-11.1 psia (10.3-
76.6 kPa), equip with
floating roof or fixed
roof with internal
floating cover (both
must meet specifica-
tions) or vapor re-
covery and disposal
system reducing emis-
sions at least 95:i
Vapor pressure >11.1
psia (76.6 kPa),
equip with vapor
recovery and
disposal system
reducing emissions
at least 95S
No requirement
No requirement
Type of liquid, period
of storage, and maximum
vapor pressure
-------
Source category
Subpart L - Secondary Lead
Smel ters
Proposed/effective
6/11/73 (38 FR 15406)
Promulgated
3/8/74 (39 FR 9308)
Revised
4/17/74 (39 FR 13776)
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart M - Secondary Brass,
Bronze, and Ingot Production
Plants
Proposed/effective
6/11/73 (38 FR 15406)
Promulgated
3/8/74 (39 FR 9308)
Revised
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Affected
facility
Reverberatory and
blast furnaces
Pot furnaces
>550 Ib/capacity
Reverberatory
furnace
Blast and electric
furnaces
Pollutant
Particulate
Opacity
Opacity
Particulate
Opacity
Opacity
Emission level
0.022 gr/dscf
(50 mg/dscm)
20":
10::-.
0.022 gr/dscf
(50 mg/dscm)
20:;
102
Monitoring
requirement
No requirement
No requirement
No requirement
No requirement
No requirement
No requirement
-------
Source category
Subpart N - Iron and Steel Plants
Proposed/effective
6/11/73 (38 FR 15406)
Promulgated
3/8/74 (39 FR 9308)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
4/13/78 (43 FR 15600)
Subpart 0 - Sewage Treatment
Plants
Proposed/effective
6/11/73 (38 FR 15406)
Promulgated
3/8/74 (39 FR 9308)
Revised
4/17/74 (39 FR 13776)
5/3/74 (39 FR 15396)
10/6/75 (40 FR 46250)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
Affected
facility
Basic oxygen
process furnace
Sludge incinerators
>10» from municipal
sewage treatment or
>2,205 Ib/day muni-
cipal sewage sludge
Pollutant
Particulate
Opacity
Particulate
Opacity
Emission level
0.022 gr/dscf
(50 mg/dscm)
105S (20% exception/
cycle)
1.30 Ib/ton
(0.65 g/kg)
20°/,
Monitoring
requirement
No requirement
No requirement
Time and duration
of each cycle;
exhaust gas diver-
sion; scrubber pres-
sure loss; water
supply pressure
No requirement
No requirement
Mass or volume of
sludge; mass of
any municipal
solid waste
-------
I
CO
Source category
Subpart P - Primary Copper
Smelters
Proposed/effective
10/16/74 (39 FR 37040)
Promulgated
1/15/76 (41 FR 2331)
Revised
2/26/76 (41 FR 8346)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart Q - Primary Zinc Smelters
Proposed/ef f ecti ve
10/16/74 (39 FR 37040)
Promulgated
1/15/76 (41 FR 2331 )
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Affected
facility
Dryer
Roaster, smelting
furnace,* copper
converter
*Reverberatory furnaces
that process high-im-
purity feed materials
are exempt from SOp
standard
Sintering machine
Roaster
Pollutant
Particulate
Opacity
S02
Opacity
Particulate
Opacity
S02
Opacity
Emission level
0.022 gr/dscf
(50 mg/dscm)
20-,
0.065S
20.;
0.022 gr/dscf
(50 mg/dscm)
20?
0.065-
201:
Monitoring
requirement
No requirement
Continuous
Continuous
No requirement
Monthly record of
charge and weight
percent of arsenic,
antimony, lead, and
zinc
No requirement
Continuous
Continuous
No requirement
-------
I
-p.
Source category
Subpart R - Primary Lead Smelters
Proposed/ef fecti ve
10/16/74 (39 FR 37040)
Promulgated
1/15/76 (41 FR 2331)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart S - Primary Aluminum
Reduction Plants
Proposed/effective
10/23/74 (39 FR 37730)
Promulgated
1/26/75 (41 FR 3825)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
6/30/80 (45 FR 4420?)
12/15/81 (46 FR 61125)
Affected
facility
Blast or reverberatory
furnace, sintering
machine discharge end
Sintering machine,
electric smelting
furnace, converter
Potroom group
Anode bake plants
Pollutant
Particulate
Opacity
S02
Opacity
Opacity
Total fluorides
(a) Soderberg
(b) Prebake
Total fluorides
Opacity
Emission level
0.022 gr/dscf
(50 mg/dscm)
20:
0.065S
20'
ior,
2.0-2.6 Ib/ton
1.9-2.5 Ib/ton
0.1 Ib/ton
20",
Monitoring
requirement
No requirement
Continuous
Continuous
No requirement
No requirement
No requirement
No requirement
No requirement
No requirement
Daily weight, pro-
duction rate of
aluminum and anode,
raw material feed
rate, cell or
potl ine voltages
-------
Source category
Affected
facility
Pollutant
Emission level
Monitoring
requirement
Subpart T - Phosphate Fertilizer
Industry
Proposed/effective
10/22/74 (39 FR 37602)
Promulgated
8/6/75 (40 FR 33152)
Revised
7/25/77 (42 FR 37936)
3/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Wet process
phosphoric acid
Total fluorides
0.02 Ib/ton
No requirement
Mass flow rate,
daily equivalent
P2C>5 feed, total
pressure drop
across scrubbing
system
01 Subpart U - Phosphate Fertilizer
Industry
Proposed/effective
10/22/74 (39 FR 37602)
Promulgated
8/6/75 (40 FR 33152)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Superphosphoric acid
Total fluorides
0.01 Ib/ton
No requirement
Mass flow rate,
daily equivalent
P2(>5 feed, total
pressure drop
across scrubbing
system
-------
I
cr>
Source category
Subpart V - Phosphate Fertilizer
Industry
Proposed/effective
10/24/74 (39 FR 37602)
Promulgated
8/6/75 (40 FR 33152)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart W - Phosphate Fertilizer
Industry
Proposed/effective
10/22/74 (39 FR 37602)
Promulgated
8/6/75 (40 FR 33152)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Affected
f ac i 1 i ty
Diammonium phosphate
Triple superphosphate
Pollutant
Total fluorides
Total fluorides
Emission level
0.06 Ib/ton
0.2 Ib/ton
Monitoring
requirement
No requirement
Mass flow rate,
daily equivalent
F>2C)5 feed, total
pressure drop
across scrubbing
system
No requirement
Mass flow rate,
daily equivalent
?205 feed, total
pressure drop
across scrubbing
system
-------
Source category
Subpart X - Phosphate Fertilizer
Industry
Proposed/ef f ect i ve
10/22/74 (39 FR 37602)
Promulgated
8/6/75 (40 FR 33152)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Subpart Y - Coal Preparation
Plants
Proposed/effective
10/24/74 (39 FR 37922)
Promulgated
1/15/76 (41 FR 2232)
Revised
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
9/7/77 (42 FR 44812)
3/3/78 (43 FR 8800)
Reviewed
4/14/81 (46 FR 21769)
Affected
facility
Granular triple super-
phosphate
Thermal dryer
Pneumatic coal
cleaning equipment
Processing and con-
veying equipment,
storage systems,
transfer and loading
systems
Pollutant
Total fluorides
Particulate
Opacity
Particulate
Opacity
Opacity
Emission level
5.0 x 10"4
Ib/h/ton
0.031 gr/dscf
(0.070 g/dscm)
20%
0.018 gr/dscf
(0.040 g/dscm)
10°:
20?,
Monitoring
requirement
No requirement
Mass flow rate,
daily equivalent
?205 feed, total
pressure drop
across scrubbing
system
Temperature,
Scrubber
pressure loss,
Water pressure
No requirement
No requirement
No requirement
No requirement
-------
Source category
Affected
facility
Pollutant
Emission level
Monitoring
requirement
Co
Subpart Z - Ferroalloy Production
Facilities
Proposed/effective
10/21/74 (39 FR 37470)
Promulgated
5/4/76 (41 FR 18497)
Revised
5/20/76 (41 FR 20659)
7/25/77 (42 FR 37936)
8/17/77 (42 FR 41424)
3/3/78 (43 FR 8800)
Electric submerged
arc furnaces
Particulate
Dust handling equip-
ment
Opacity
CO
Opacity
0.99 Ib/MW-h
(0.45 kg/MW-h)
("high silicon alloys"
0.51 Ib/MW-h
(0.23 kg/MW-h)
(chrome and manganese
alloys)
No visible emissions
may escape furnace
capture system
No visible emissions
may escape tapping
system for >40rJ of
each tapping period
20% volume basis
10X
No requirement
Flow rate
monitoring in
hood
Flow rate
monitoring in
hood
Continuous
No requirement
No requirement
-------
Source category
Subpart AA - Steel Plants
Proposed/ef f ecti ve
10/21/74 (39 FR 37466)
Promulgated
9/23/75 (40 FR 43850)
Revised
7/25/77 (40 FR 37936)
8/17/77 (42 FR 41424)
9/7/77 (42 FR 44812)
3/3/78 (43 FR 8800)
Affected
facility
Electric arc furnaces
Dust handling equip-
ment
Pollutant
Particulate
Opacity
(a) control device
(b) shop roof
Opacity
Emission level
0.0052 gr/dscf
(12 mg/dscm)
3%
0% except
<20X-charging
<40£- tapping
IDS
Monitoring
requirement
No requirement
Continuous
Flow rate
monitoring in
capture hood,
Pressure
monitoring
in DSE system
No requirement
-------
I
ro
o
Source category
Subpart BB - Kraft Pulp Mills
Proposed/ef f ecti ve
9/24/76 (41 FR 42012)
Promulgated
2/23/78 (43 FR 7568)
Revi sed
8/7/78 (43 FR 34784)
Affected
facility
Recovery furnace
Smelt dissolving
tank
Lime kiln
Digester, brown stack
washer, evaporator.
oxidation, or strip-
per systems
Pollutant
Parti cul ate
Opacity
TRS
(a) straight recovery
(b) cross recovery
Particulate
TRS
Particulate
(a) gaseous fuel
(b) liquid fuel
TRS
TRS
Emission level
0.044 gr/dscf
(0.10 g/dscm)
corrected to 8%
oxygen
35?
5 ppm by volume
corrected to 8"
oxygen
25 ppm by volume
corrected to 87-
oxygen
0.2 Ib/ton
(0.1 g/kg)
0.0168 Ib/ton
.(0.0084 g/kg)
0.067 gr/dscf
(0.15 g/dscm)
corrected to 10"
oxygen
0.13 gr/dscf
(0.30 g/dscm)
corrected to 10'^
oxygen
8 ppm by volume
corrected to 102
oxygen
5 ppm by volume
corrected to 10'
oxygen*
•exceptions; see
standards
Monitoring
requirement
No requirement
Continuous
Continuous
No requirement
No requirement
No requirement
No requirement
Continuous
Continuous
Effluent gas incineration
temperature; scrubber
1 iquid
supply pressure and gas
stream pressure loss
-------
Source category
Affected
facility
Pollutant
Emission level
Monitoring
requirement
Subpart CC - Glass
Manufacturing plants
Proposed/effective
6/15/79 (44 FR 34840)
Promulgated
10/7/80 (45 FR 66741)
i
ro
Glass melting furnace
producing > 4,550 kg
glass/day firing gas-
eous fuel:*
Container glass
Pressed & blown glass
Borosilicate
Soda-Lime & Lead
Other
Wool fiberglass
Flat glass
Glass melting furnace
producing > 4,550 kg
glass/day firing
liquid fuel:*
Container glass
Pressed & blown glass
Borosilicate
Soda-Lime & Lead
Other
Wool fiberglass
Flat glass
*
Proportionate incre-
ments allowed for
simultaneous gaseous
and liquid firing
Particulate
Participate
No requirement
0.1 g/kg glass
0.5 g/kg glass
0.1 g/kg glass
0.25 g/kg glass
0.25 g/kg glass
0.225 g/kg glass
0.13 g/kg glass
0.65 g/kg glass
0.13 g/kg glass
0.325 g/kg glass
0.325 g/kg glass
0.225 g/kg glass
No requirement
-------
I
ro
ro
Source category
Subpart 00 - Grain Elevators
Proposed/effective.
8/3/78 (43 FR 34349)
Promulgated
8/3/78 (43 FR 34340)
*
Affected
facility
Column and rack
dryers
Process equipment
other than dryers
Fugitive emissions:
Truck unloading;
rail car loading
or unloading
Grain handling
Truck loading
Barge, ship
loading
Pollutant
Opacity
Particulate
Opacity
Opacity
Opacity
Opacity
Opacity
Emission level
o/;
0.01 gr/dscf
(0.023 g/dscm)
0'*
5',;
OS
10%
20*
Monitoring
requirement
No requirement
No requirement
No requirement
No requirement
No requirement
No requirement
No requirement
-------
Source category
Subpart GG - Stationary
Gas Turbines
Proposed/effective
10/3/77 (42 FR 53782)
Promulgated
9/10/79 (44 FR 52792)
Revised
1/27/82 (47 FR 3767)
Affected
f ac i 1 i ty
Gas turbines >10.7
GJ/h (>10 million
Btu/h)
Gas turbines >10.7 and
5.107.2 GJ/h (^10
mill ion and <100
million Btu/h)*
Gas turbines >107.2
GJ/h (100 million
Btu/h)*
Gas turbines >107.2
GJ/h (100 million
Btu/h) used in oil/
gas production or
transportation not
in MSA*
*Emergency, military
(Other than garrison),
military training,
firefighting, and R&D
turbines exempt from
NO standards
X
Pollutant
SO
L
N0y (effective
1073/82)
N0x
A
NO
Emission level
0.015% (150 ppm) at
15% oxygen on dry
basis or fuel with
<0.8% sulfur
0.015% (150 ppm) at
15% oxygen on dry basis
referenced to ISO
standard day condi-
tions*
0.0075?;; (75 ppm) at
15% oxygen on dry basis
referenced to ISO
standard day condi-
tions*
0.015% (150 ppm) at
155'. oxygen on dry
basis referenced to
ISO standard day
conditions*
*Adjustments allowed
for thermal effi-
ciency >25~- or fuels
with >0.015 nitrogen
content
Monitoring
requirement
Sulfur and nitrogen
content of fuel
Continuous fuel consumption
and water/fuel ratio if
using NOX control by water
injection
-------
I
ro
Source category
Subpart HH - Lime Manufacturing
Plants
Proposed/effective
5/3/77 (42 FR 22506)
Promulgated
3/7/78 (43 FR 9452)
Affected
facil ity
Rotary lime kiln
Lime hydrator
Pollutant
Particulate
Opacity
Particulate
Emission level
0.30 Ib/ton
(0.15 kg/Mg)
10%
0.15 Ib/ton
(0.075 kg/Mg)
Monitoring
requirement
No requirement
Continuous except when
using wet scrubber
No requirement
Mass of feed to rotary
lime kiln and hydrator
-------
I
ro
Source category
Subpart KK - Lead-Acid Battery
Manufacturing Plants
Proposed/effective
1/14/80 (45 FR 2790)
Promulgated
4/16/82 (47 FR 16564)
Affected
facility
Facilities producing or
with design capacity
>6.5 tons/day (5.9
Mg/day) lead in batter-
ies using:
Grid casting
Lead oxide manufac-
turing
Lead reclamation
Paste mixing, three-
process operations,
and any other lead-
emitting operations
Lead Reclamation
All other affected
facilities
Pollutant
Lead
Lead
Lead
Lead
Opacity
Opacity
Emission level
0.000176 gr/dscf ex-
haust (0.40 mg/dscm)
0.010 Ib/ton lead feed
(5.0 mg/kg)
0.00198 gr/dscf exhaust
(4.50 mg/dscm)
0.00044 gr/dscf exhaust
(1 .00 mg/dscm)
5?
0%
Note: common control
device ducting, see
formula at 60.372
Monitoring
requirement
No requirement
No requirement
No requirement
No requirement
No requirement
No requirement
Pressure drop across
scrubbing system
-------
Source category
Affected
facility
Pollutant
Emission level
Monitoring
requirement
Subpart MM - Automobile and Light-
Duty Truck Surface Coating Opera-
tions
Proposed/effective
10/5/79 (44 FR 57792)
Promulgated
12/24/80 (45 FR 85410)
i
rj
(Tl
Prime coating
Guide coating
Top coating
Exempt: plastic
components and all-
plastic bodies on
separate lines
VOC
VOC
VOC
0.16 kg/liter of ap-
plied coating solids/
per each prime coat
operation
1.40 kg/liter of ap-
plied coating solids/
per each guide coat
operation
1.47 kg/liter of ap-
plied coating solids/
per each top coat
operation
No requirement*
No requirement*
No requirement*
*Permanent record of
incinerator tempera-
ture, if applicable.
-------
Source category
Subpart NN - Phosphate Rock Plants
Proposed/effective
9/21/79 (44 FR 54970)
Promulgated
4/16/82 (47 FR 16582)
Affected
facility
Facilities with pro-
duction capabilities
>4 tons/h (3.6 Mg/h):
Dryer
Calciner
Unbeneficiated or
blend
Beneficiated
Dryer and calciner
Grinder
Ground rock handling
and storage
Exempt: production or
preparation for ele-
mental phosphorus
production
Pollutant
Particulate
Particulate
Particulate
Opacity
Particulate
Opacity
Opacity
Emission level
0.06 Ib/ton feed
0.23 Ib/ton feed
(0.12 kg/Mg)
0.11 Ib/ton feed
(0.055 kg/Mg)
10%
0.012 Ib/ton feed
(0.006 kg/Mg)
0%
0%
Monitoring
requirement
No requirement
No requirement
No requirement
Continuous, except when
using wet scrubber
No requirement
Continuous, except when
using wet scrubber
No requirement
Wet scrubber: pressure
loss and liquid supply
pressure
Feed rate to dryer,
calciner, and grinder
-------
Source category
Affected
facility
Pollutant
Emission level
Monitoring
requirement
i
ro
CO
Subpart PP - Ammonium Sulfate
Manufacture
-.
2/4/80 (45 FR 7758)
Promulgated
11/12/80 (45 FR 74846)
Ammonium sulfate dryer
in caprolactam by-
product, synthetic and
coke oven by-product
sectors
Particulate
Opacity
0.30 Ib/ton produced
(0.15 kg/Mg)
15%
No requirement
No requirement
Mass flow rate or weigh
scales for production rate;
total pressure drop across
control system
-------
SECTION III
STANDARDS OF
PERFORMANCE FOR NEW
STATIONARY SOURCES
-------
Title 40—PROTECTION OF
ENVIRONMENT
Chapter I—Environmental Protection
Agency
SUBCHAPTEt C^-AII PtdOIAMS
PART 60—STANDARDS OF PERFORM-
ANCE FOR NEW STATIONARY
SOURCES""139
Subpart A—General Provisions
Sec.
60.1 Applicability.
60.2 Definitions.
60.3 Units and abbreviations.
60.4 Address.
60.5 Determination of construction or
modification.
60.6 Review of plans.
60.7 Notification and record keeping.
60.8 Performance tests.
60.9 Availability of information.
60.10 State authority.
60.11 Compliance with standards and
maintenance requirements.4
60.12 Circumvention.5
60.13 Monitoring requirements.18
60.14 Modification.72
60.15 Reconstruction.
60.16 Priority list.w
Subpart ft—Adoption and Submittal of State
Plan* for Designated Facilities/;
60.20 Applicability.
60.21 Definitions.
60.22 Publication of guideline documents,
emission guidelines, and final compli-
ance times.
60.23 Adoption and submittal of State
plans; public hearings.
60.24 Emission standards and compliance
schedules.
60.25 Emission inventories, source surveil-
lance, reports.
60.26 Legal authority.
60.27 Actions by the Administrator.
60.28 Plan revisions by the State.
60.29 Plan revisions by the Administrator.
Subpart C—Emission Guidelines and
Compliance Times 73
60.30 Scope.
60.31 Definitions.
60.32 Designated facilities.
60.33 Emission guidelines.
60.34 Compliance times.
Subpart D—Standards of Performance for
Fossil-Fuel Fired Steam Generators
for Which Conslnjctlor
After August 17.1S71'
60.40 Applicability and designation of af-
fected facility.
60.41 Definitions.
60.42 Standard for particulate matter.
60.43 Standard for sulfur dioxide.
80.44 Standard for nitrogen oxides.
60.45 Emission and fuel monitoring.
60.46 Test methods and procedures.
60.47 Innovative technology waiver.
Subpart Da—Standards of Performance for
Electric Utility Steam Generating Units for
Which Construction Is Commenced After Sep-
tember I8.197898
60.40a Applicability and designation of af-
fected facility.
60.41a Definitions.
60.42a Standard for particulate matter.
60.43a Standard for sulfur dioxide.
60.44a Standard for nitrogen oxides.
60.45a Commercial demonstration permit.
60.46a Compliance provisions.
60.47a Emission monitoring.
60.48a Compliance determination proce-
dures and methods.
60.49a Reporting requirements.
Subpart E—Standards of Performance for
Incinerators
60.50 Applicability and designation of af-
fected facility.
60.51 Definitions.
60.52 Standard for particulate matter.
60.53 Monitoring of operations.
60.54 Test methods and procedures.
Subpart F—Standards of Performance for
Portland Cement Plants
60.60 Applicability and designation of af-
fected facility.
60.61 Definitions.
60.62 Standard for particulate matter.
60.63 Monitoring of operations.
60.64 Test methods and procedures.
Subpart G—Standards of Performance for
Nitric Acid Plants
60.70 Applicability and designation of af-
fected facility.
60.71 Definitions.
60.72 Standard for nitrogen oxides.
60.73 Emission monitoring.
60.74 Test methods and procedures.
Subpart H—Standards of Performance for
Sulfuric Acid Plants
60.80 Applicability and designation of af-
fected facility.
60.81 Definitions.
60.82 Standard for sulfur dioxide.
60.83 Standard for acid mist.
60.84 Emission monitoring.
60.85 Test methods and procedures.
Subpart I—Standards of Performance for
Asphalt Concrete Plants 3
60.90 Applicability and designation of af-
fected facility.
60.91 Definitions.
60.92 Standard for particulate matter.
60.93 Test methods and procedures.
Subpart J—Standards of Performance for
Petroleum Refineries5
60.100 Applicability and designation of af-
fected facility.
60.101 Definitions.
60.102 Standard for particulate matter.
60.103 Standard for carbon monoxide.
60.104 Standard for sulfur dioxide.
60.105 Emission monitoring.
60.106 Test methods and procedures.
Subpart K—Standards of Performance for
Storage Vessels for Petroleum Liquids
Constructed After June 11, 1173 and Prior to
May 19,197t 5,111
60.110 Applicability and designation of af-
fected facility.
60.111 Definitions.
60.112 Standard for volatile organic
compounds (VOC).111
60.113 Monitoring of operations.
Subpart Ka-£tandards of Performance for
Storage weasels for Petroleum Uoukto
Constructed After May 16,1976 "'
eo.HOa Applicability and designation of
affected facility.
60.111a Definitions.
60.112a Standard for volatile organic
compounds (VOC).
60.113a Testing and procedures.
60.114a Equivalent equipment and
procedures.
60.115a Monitoring of operations.
Subpart I—Standards of Performance for
Secondary Lead Smelters5
60.120 Applicability and designation of al
fected facility.
60.121 Definitions.
60.122 Standard for particulate matter.
60.123 Test methods and procedures.
Subpart M—Standards of Performance for Sot
ondary Brass and Bronze Ingot Produetlo
Plants5
60.130 Applicability and designation of at
fected facility.
60.131 Definitions.
60.132 Standard for particulate matter.
60.133 Test methods and procedures.
Subpart N—Standards of Performance for Irei
and Steel Plants5
60.140 Applicability and designation of al
fected facility.
60.141 Definitions.
60.142 Standard for particulate matter.
60.143 Monitoring of operations.88
60.144 Test methods and procedures.
Subpart O—Standards of Performance for
Sewage Treatment Plants5
60.150 Applicability and designation of al
fected facility.
60.151 Definitions.
60.152 Standard for particulate matter.
60.153 Monitoring of operations.
60.154 Test methods and procedures.
Subpart P—Standards of Performance for
Primary Copper Smelters26
60.160 Applicability and designation of ai
fected facility.
60.161 Definitions.
60.162 Standard for particulate matter.
60.163 Standard for sulfur dioxide.
60.164 Standard for visible emissions.
60.165 Monitoring of operations.
60.166 Test methods and procedures.
III-l
-------
Subpart Q—Standards el Performance for
Primary Zinc Smellers 26
80.170 Applicability and designation of af-
fected facility.
60.171 Definitions.
60.172 Standard for participate matter.
60.173 Standard for sulfur dioxide.
60.174 Standard for visible emissions.
60.175 Monitoring of operations.
60.176 Test methods and procedures.
Subpart R—Standards of Performance for
Primary Lead Smelters
26
60.180 Applicability and designation of af-
fected facility.
60.181 Definitions.
60.182 Standard for paniculate matter.
60.183 Standard for sulfur dioxide.
60.184 Standard for visible emissions.
60.185 Monitoring of operations.
60.186 Test methods and procedures.
Subpart S—Standards of Performance for
Primary Aluminum Reduction Plants27
60.190 Applicability and designation of af- •
fected facility.
60.191 Definitions.
60.192 Standard for fluorides.
60.193 Standard for visible emissions.
60.194 Monitoring of operations.
60.195 Test methods and procedures.
Subpart T—Standards of Performance for the
Phosphate Fertiliier Industry: Wet Process
Phosphoric Acid Plants14
60.200 Applicability and designation of af-
fected facility.
60.201 Definitions.
60.202 Standard for fluorides.
60.203 Monitoring of operations.
60.204 Test methods and procedures.
Subpart U—Standards of Performance for the
Phosphate Fertilizer Industry: Superphos-
phoric Acid Plants "
60.210 Applicability and designation of af-
fected facility.
60.211 Definitions.
60.212 Standard for fluorides.
60.213 Monitoring of operations.
60.214 Test methods and procedures.
Subpart V—Standards of Performance for the
Phosphate Fertilizer Industry: Diammonium
Phosphate Plants14
60.220 Applicability and designation of af-
fected facility.
60.221 Definitions.
60.222 Standard for fluorides.
60.223 Monitoring of operations.
60.224 Test methods and procedures.
Subpart W—Standards of Performance for the
Phosphate Fertilizer Industry: Triple Super-
phosphate Plants14
60.230 Applicability and designation of af-
fected facility.
60.231 Definitions.
60.232 Standard for fluorides.
60.233 Monitoring of operations.
60.234 Test methods and procedures.
Subpart X—Standards of Performance for the
Phosphate Fertilizer Industry: Granular Triple
Superphosphate Storage Facilities14
60.240 Applicability and designation of af-
fected facility.
60.241 Definitions.
60.242 Standard for fluorides.
60.243 Monitoring of operations.
60.244 Test methods and procedures.
Subpart Y—Standards of Performance for Coal
Preparation Plants26
60.250 Applicability and designation of af-
fected facility.
60.251 Definitions.
60.252 Standards for particulate matter.
60.253 Monitoring of operations.
60.254 Test methods and procedures.
Subpart Z—Standards of Performance for
Ferroalloy Production Facilities33
60.260 Applicability and designation of af-
fected facility.
60.261 Definitions.
60.262 Standard for particulate matter.
60.263 Standard for carbon monoxide.
60.264 Emission monitoring.
60.265 Monitoring of operations.
60.266 Test methods and procedures.
Subpart AA—Standards of Performance for
Steel Plants: Electric Arc Furnaces16
60.270 Applicability and designation of af-
fected facility.
60.271 Definitions.
60.272 Standard for particulate matter.
60.273 Emission monitoring.
60.274 Monitoring of operations.
60.275 Test methods and procedures.
Subpart BB—Standards of Performance for
Kraft Pulp Mills82
60.280 Applicability and designation of af-
fected facility.
60.281 Definitions.
60.282 Standard for particulate matter.
60.283 Standard for total reduced sulfur
(TRS).
60.284 Monitoring of emissions and oper-
ations.
60.285 Test methods and procedures.
Subpart CC—Standards of Performance for
Glass Manufacturing Plants ™
60.290 Applicability and designation of
affected facility.
60.291 Definitions.
60.292 Standards for particulate matter.
60.293-60.295 [Reserved)
60.296 Test methods and procedure*.
Subpart DD—Standards of Performance for
Grain Elevators90
60.300 Applicability and designation of af-
fected facility.
60.301 Definitions.
60.302 Standard for particulate matter.
60.302 Test methods and procedures.
60.304 Modification.
Subpart OO—Standards of .Performance for
Stationary Qaa Turbines'° '
60.330 Applicability and designation of
affected facility.
00.331 Definitions.
60.332 Standard for nitrogen oxides.
60.333 Standard for sulfur dioxide.
60.334 Monitoring of operations.
6O335 Test methods and procedures.
Subpart MM—Standards of Performance for
Lime Manufacturing Plants85
60.340 Applicability and designation of af-
fected facility.
60.341 Definitions.
60.342 Standard for particulate matter.
60.343 Monitoring of emissions and oper-
ations.
60.344 Test methods and procedures.
Subpart KK—Standard* of
Performance for Lead-Add Battery
Manufacturing Plant* "5
60.370 Applicability and designation of
affected facility.
60471 Definitions.
60.372 Standards for lead.
60.373 Monitoring of emissions and
operations.
60.374 Test methods and procedures.
Subpart MM—Standards of Performance
for Automobile and Light-Duty Truck
Surface Coaling Operations 'M
60.390 Applicability and designation of
affected facility.
60.391 Definitions.
60.392 Standards for volatile organic
compounds.
60.393 Performance test and compliance
provisions.
60.394 Monitoring of emissions and
operations.
60.395 Reporting and recordkeeping
requirements.
60.396 Reference methods and procedures.
60.397 Modifications.
Subpart NN—Standards of Performance for
Phosphate Rock Plants "6
60.400 Applicability and designation of
affected facility.
60.401 Definitions.
60.402 Standard for particulate matter.
60.403 Monitoring of emissions and
operations.
60.404 Test methods and procedures.
Subpart PP—Standards of Performance for
Ammonium Sulfate Manufacture119
60.420 Applicability and designation of
affected facility.
60.421 Definitions.
60.422 Standards for particulate matter.
60.423 Monitoring of operations.
60.424 Test methods and procedures.
III-2
-------
Appendix A—Reference Methods
Method 1—Sample and velocity traverses
for stationary sources.
Method 2—Determination of stack gas ve-
locity and volumetric flow rate (Type S
pitot tube).
Method 3—Gas analysis for carbon dioxide,
oxygen, excess air, and dry molecular
weight.
Method 4—Determination of moisture con-
tent in stack gases.
1 Method 5—Determination of paniculate
emissions from stationary sources.
Method 6—Determination of sulfur dioxide
emissions from stationary sources.
Method 7—Determination of nitrogen oxide
emissions from stationary sources.
Method 8—Determination of sulfuric acid
mist and sulfur dioxide emissions from
stationary sources.
Method 9—Visual determination of the
opacity of emissions from stationary
sources.
Alternate Method 1-Determinatlon
of the opacity of emissions from
stationary sources remotely by
lidar.131
Method 10—Determination of carbon mon-
oxide emissions from stationary sources.
Method 11—Determination of hydrogen sul-
fide content of fuel gas streams in petro-
leum refineries.79
Method 12—Determination of inor-
ganic lead emissions from stat-
ionary sources.145
Method 13A—Determination of total flu-
oride emissions from stationary
sources—SPADNS Zirconium Lake
Method.14'113
Method 13B—Determination of total flu-
oride emissions from stationary
sources—Specific Ion Electrode Method.
Method 14—Determination of fluoride emis-
sions from potroom roof monitors of pri-
mary aluminum plants.27'"4
Method 15—Determination of hydrogen sul-
fide, carbonyl sulfide, and carbon distil-
fide emissions from stationary sources.86
Method 16—Semicontinuous determination
of sulfur emissions from stationary
sources.82
Method 17—Determination of particulate
emissions from stationary sources (in-
stack filtration method).82
Method 19-Determination of sulfur
dioxide removal efficiency and
particulate, sulfur dioxide and
nitrogen oxides emission rates
from electric utility steam
98
generators.
Method 20-Determination of nitrogen
oxides, sulfur dioxide, and oxy-
gen emissions from stationary gas
turbines.101
Method 24-Determination of volatile
matter content, water content,
density, volume solids, and weight
solids of surface coatings. 117
Method 25-Determination of total
gaseous nonmethane organic
emissions as carbon."7
Appendix B—Performance Specifications'8
Performance Specification 1—Perform-
ance specifications and specification test
procedures for transmissometer systems for
continuous measurement of the opacity of
stack emissions.
Performance Specification 2—Perform-
ance specifications and specification test
procedures for monitors of SO, and NO,
from stationary sources.
Performance Specification 3—Perform-
ance specifications and specification test
procedures for monitors of CO, and O, from
stationary sources.
Appendix C—Determination of Emission
Rate Change22
Appendix D—Required Emission Inventory
Information21
AUTHORITY: Sec. Ill, 301(a) of the CTea
Air Act as amended (42 U.S.C. 741
7601(a», unless otherwise noted.68.83
III-3
-------
Swfaporf A—Oonoral Provisions
f 60.1 Applicability.8'21
Except as provided in Subparts B
and C, the provisions of this part
apply to the owner or operator of any
stationary source which contains an
affected facility, the construction or
modification of which is commenced
after the date of publication in this
part of any standard (or, if earlier, the
date of publication of any proposed
standard) applicable to that facility.
|60.2 Definitions.102
The terms used in this part are
defined in the Act or in this section as
follows:
"Act" means the Clean Air Act (42
U.S.C. 1857 et seq., as amended by Pub.
L 91-604, 84 Stat. 1676).
"Administrator" means the
Administrator of the Environmental
Protection Agency or his authorized
representative.
"Affected facility" means, with
reference to a stationary source, any
apparatus to which a standard is
applicable.
"Alternative method" means any
method of sampling and analyzing for
an air pollutant which is not a reference
or equivalent method but which has
been demonstrated to the
Administrator's satisfaction to, in
specific cases, produce results adequate
for his determination of compliance.5
"Capital expenditure" means an
expenditure for a physical or
operational change to an existing facility
which exceeds the product of the
applicable "annual asset guideline
repair allowance percentage" specified
in the latest edition of Internal Revenue
Service (IRS) Publication 534 and the
existing facility's basis, as defined by
section 1012 of the Internal Revenue
Code. However, the total expenditure
for a physical or operational change to
an existing facility must not be reduced
by any "excluded additions" as defined
in IRS Publication 534, as would be done
for tax purposes.22'109
"Commenced" means, with respect to
the definition of "new source" in section
lll(a)(2) of.the Act, that an owner or
operator has undertaken a continuous
program of construction or modification
or that an owner or operator has entered
into a contractual obligation to
undertake and complete, within a
reasonable time, a continuous program
of construction or modification.5
"Construction" means fabrication.
erection, or installation of an affected
facility.
"Continuous monitoring system"
means the total equipment, required
' under the emission monitoring sections
in applicable subparts, used to sample
and condition (if applicable), to analyze.
and to provide a permanent record of
emissions or process parameters.18
"Equivalent method" means any
method of sampling and analyzing for
ah air pollutant which has been
demonstrated to the Administrator's
satisfaction to have a consistent and
quantitatively known relationship to the
reference method, under specified
conditions.5
"Existing facility" means, with
reference to a stationary source, any
apparatus of the type for which a
standard is promulgated in this part, and
the construction or modification of
which was commenced before the date
of proposal of that standard; or any
apparatus which could be altered in
such a way as to be of that type.22
"Isokinetic sampling" means sampling
in which the linear velocity of the gas
entering the sampling nozzle is equal to
that of the undisturbed gas stream at the
sample point. '
"Malfunction" means any sudden and
unavoidable failure of air pollution
control equipment or process equipment
or of a process to operate in a normal or
usual manner. Failures that are caused
entirely or in part by poor maintenance.
careless operation, or any other
preventable upset condition or
preventable equipment breakdown shall
not be considered malfunctions.4
"Modification" means any physical
change in, or change in the method of
operation of, an existing facility which
increases the amount of any air
pollutant (to which a standard applies)
emitted into the atmosphere by that
facility or which results in the emission
of any air pollutant (to which a standard
applies) into the atmosphere not
previously emitted.72
"Monitoring device" means the total
equipment, required under the
monitoring of operations sections in
applicable subparts, used to measure
and record (if applicable) process
parameters.18
"Nitrogen oxides" means all oxides of
nitrogen except nitrous oxide, as
measured by test methods set forth in
this part.
"One-hour period" means any 60- 4/)8
minute period commencing on the hour.
"Opacity" means the degree to which
emissions reduce the transmission of
light and obscure the view of an object
in the background.
"Owner or operator" means any
person who owns, leases, operates,
controls, or supervises an affected
facility or a stationary source of which
an affected facility is a part.
"Particulate matter" means any fmel;
divided solid or liquid material, other
than uncombined water, as measured b;
the reference methods specified under
each applicable subpart, or-an 5 g 90
equivalent or alternative method. ' '
"Proportional sampling" means
sampling at a rate that produces a
constant ration of sampling rate to staci
gas flow rate.
"Reference method" means any
method of sampling and analyzing for
an air pollutant as described in
Appendix A to this part.5'8
"Run" means the net period of time
during which an emission sample is
collected. Unless otherwise specified, a
run may be either intermittent or
continuous within the limits of good
engineering practice.5
"Shutdown" means the cessation of
operation of an affected facility for any
purpose.4
"Six-minute period" means any one of
the 10 equal parts of a one-hour period.18
"Standard" means a standard of
performance proposed or promulgated
under this part.
"Standard conditions" means a
temperature of 293 K (68°F) and a
pressure of 101.3 kilopascals (29.92 in
Hg).5'84
"Startup" means the setting in
operation of an affected facility for any
purpose.
"Volatile Organic Compound" means
any organic compound which
participates in atmospheric
photochemical reactions; or which is
measured by a reference method, an
equivalent method, an alternative
method, or which is determined by i2<
procedures specified under any subpart.
§ 60.3 Units and abbreviations.5'62
Used in this part are abbreviatioi
and symbols of units of measur
These are defined as follows:
(a) System International (SI) uni
of measure:
A—ampere
g-gram
Hz—hertz
J—joule
K—degree Kelvin
kg—kilogram
m—meter
m '—cubic meter
mg—milligram—10"* gram
mm—millimeter—10'J meter
Mg—megagram—10s gram
mol—mole
N- newton
ng--nanogram—ID' • gram
mil—nanometer—10"' meter
III-4
-------
Pa—pascal
s—second
V—volt
W—watt
n—ohm
jig—microgram—10 " grarr,
65
(b) Other units of measure:
Btu—British thermal unit
°C—degree Celsius (centigrade)
cal—calorie
cfm—cubic feet per minute
cu ft—cubic feet
dcf—dry cubic feet
dcm—dry cubic meter
dscf—dry cubic feet at standard conditions
dscm—dry cubic meter at standard condi-
tions
eq—equivalent
"F—degree Fahrenheit
ft—feet
gal—gallon
gr—grain
g-eq—gram equivalent
hr—hour
in—inch
k—1,000
1—liter
1pm—liter per minute
Ib—pound
meq—milliequivalent
min—minute
ml—milliliter
mol. wt.—molecular weight
ppb—parts per billion
ppm—parts per million
psia—pounds per square inch absolute
psig—pounds per square inch gage
"R—degree Rankine
sci—cubic feet at standard conditions
scfh—cubic feet per hour at standard condi
lions
scm—cubic meter at standard conditions
sec—second
sq ft—square feet
std—at standard conditions
(c) Chemical nomenclature:
CdS—cadmium sulfide
CO—carbon monoxide
COj—carbon dioxide
HC1—hydrochloric acid
Hg—mercury
H,O—water
H,S—hydrogen sulfide
HaSCX—sulfuric acid
N2—nitrogen
NO—nitric oxide
NO,—nitrogen dioxide
NO,—nitrogen oxides
O,—oxygen
SOj—sulfur dioxide
SO,—sulfur trioxide
SO,—sulfur oxides
(d) Miscellaneous:
A.S.T.M.—American Society for Testing and
Materials
(Sees. Ill and 301(a) of the Clean Air Act:
sec. 4(a) of Pub. L. 91-604, 84 Slat. 1683: sec.
2 of Pub. L. 90-148, 81 Stat. 504 (42 U.S.C
1B57C-6. 1857g(a)))
§60.4 Addresj.5'12
(a) All requests, reports, applies
tions, submittals, and other communi
cations to the Administrator pursuant
to this part shall be submitted in du-
plicate and addressed to the appropri
ate Regional Office of the Environ-
mental Protection Agency, to the at-
tention of the Director, Enforcement
Division. The regional offices are as
follows:
Region I (Connecticut, Maine. New Hamp
shire, Massachusetts. Rhode Island. Ver-
mont), John F. Kennedy Federal Building.
Boston. Massachusetts 02203.
Region II (New York, New Jersey, Puerto
Rico, Virgin Islands), Federal Office Build-
ing. 26 Federal Plaza (Foley Square), New-
York. New York 10007.
Region III (Delaware, District of Colum-
bia. Pennsylvania. Maryland, Virginia, West
Virginia), Curtis Building, Sixth and
Walnut Streets, Philadelphia, Pennsylvania
Region IV (Alabama, Florida, Georgia
Mississippi. Kentucky. North Carolina.
South Carolina, Tennessee), Suite 300, 1421
Peachtree Street. Atlanta. Georgia 30309.
Region V (Illinois. Indiana. Minnesota.
Michigan, Ohio, Wisconsin), 230 South
Dearborn Street. Chicago. Illinois 60604.59
Region VI (Arkansas. Louisiana, New
Mexico, Oklahoma, Texas), 1600 Patterson
Street. Dallas. Texas 7520!
Region VII (Iowa. Kansas. Missouri,
Nebraska). 324 East 11th Street, Kansas
City, Missouri 64108.129
Region VIII (Colorado, Montana, No -th
Dakota, South Dakota, Utah, Wyoming).
196 Lincoln Towers. 1860 Lincoln Street.
Denver, Colorado 80203.
Region IX (Arizona, California, Hawaii.
Nevada, Guam, American Samoa), 100 Cali-
fornia Street. San Francisco, California
94111.
Region X (Washington, Oregon, Idaho.
Alaska), 1200 Sixth Avenue. Seattle, Wash-
ington 98101.
(b) Section lll(c) directs the Admin-
istrator to delegate to each State,
when appropriate, the authority to im-
plement and enforce standards of per-
formance for new stationary sources
located in such State. All information
required to be submitted to EPA under
paragraph (a) of this section, must
also be submitted to the appropriate
State Agency of any State to which
this authority has been delegated
(provided, that each specific delega-
tion may except sources from a certain
Federal or State reporting require-
ment). The appropriate mailing ad-
dress for those States whose delega-
tion request has been approved is as
A) ireserveni
(B) State of Alabama, A.ii Pollution Coi
iroi Division, Air Pollution Control Oommiv
v 'n, 645 S. McDonoueh Street, Mon'
E> Ticry, Alabama 36104 *5
(C) (reserved).
(D) Arizona.
Maricopa County Department of Health
Services, Bureau of Air Pollution Control,
1825 East Roosevelt Street, Phoenix. Art'..
85006.
Pima County Health Department, A'r
Quality Control District. 151 West Congres;
Tucson. Ariz. 85701. 51, 89
(E) State of Arkansas. Program
Administrator, Air and Hazardous Materials
Division, Arkansas Department of Pollution
Control and Ecology, 8001 National Drive,
Little Rock. Arkansas 72209.143
(F) California.
Del Norte County Air Pollution Control
District. 909 Highway 101 North, Crescent
City, CA 95531
Fresno County Air Pollution Control District,
P.O. Box 11867,1246 L Street, Fresno, CA
93721
Monterey Bay Unified Air Pollution Control
District. 1270 Natividad Road, Room 105.
Salinas, CA 93906
Northern Sonoma County Air Pollution
Control District, 134 "A" Avenue, Auburn.
CA 95448
Santa Barbara County Air Pollution Control
District, 300 North San Antonio Road,
Santa Barbara, CA 93110
Shasta County Air Pollution Control District,
2850 Hospital Lane, Redding, CA 96001
South Coast Air Quality Management
District, 9150 Flair Drive, El Monte. CA
91731
Stanislaus County Air Pollution Control
District, 1030 Scenic Drive, Modesto. CA
95350
Trinity County Air Pollution Control District.
P.O. Box AK, Weaverville. CA 96093
Ventura County Air Pollution Control
District, 800 South Victoria Avenue.
Ventura, CA 93009
Amador County Air Pollution Control
District. P.O. Box 430,810 Court Street,
Jackson, CA 95642
Butte County Air Pollution Control District
P O. Box 1229, 316 Nelson Avenue,
Oroville.CA 95965
Calaveras County Air Pollution Control
District, Government Center, El Dorado
Road. San Andreas, CA 95249
Cnlusa County Air Pollution Control District
751 Fremont Street. Colusa. CA 95952
Fl Dorado Air Pollution Control District 39f
Fair Lane. Placerville, CA 95667
Glenn County Air Pollution Control District
P.O. Box 351. 720 North Colusa Street,
Willows. CA 96988
Great Basin Unified Air Pollution Control
District, 863 North Main Street, Suite 213.
Bishop. CA 93514
Imperial County Air Pollution Control
District, County Services Building, 939
West Main Street, El Centro. CA 92248
Kings County Air Pollution Control District
330 Campus Drive. Hanford. CA 93230
Lake County Air Potirton Control District,
256 Horth Fortes Strwt Lakeport CA
95454
Lai sen County Air Pollution Control District.
ITS Unwell Avenue. SuMnvilie, CA 96131
MaripoM County Air Pollution Control;
District Box 5. Maripoifl. CA 95339
Merced County Air Pollution Control District
P.O. Box 471. 240 East 15th Street Merced,
CA 95340
Modoc County Air Pollution Control District
202 West 4th Street Altnraa, CA 98101
Nevada County Air Pollution Control District
H.E.W. Complex, Nevada City, CA 96959
Placer County Air Pollution Control District
114*1 "B- Avenin. Auburn. CA 96003
III-5
-------
PhuBM County Air Pollution Control District.
P.O. Box 480, Qulncy. CA 95971
San Bernardino County Air Pollution Control
District 15579-dih. Victorvillft, CA 92392
San Luis Ohispo County Air Pollution Control
District. P.O. Box 637, San Luis Obispo, CA
93406
Sierra County Air Pollution Control District
P.O. Box 200, Downieville. CA 95936
Siakiyon County Air Pollution Control
District, 525 South Foothill Drive. Yreka,
Sutler County Air Pollution Control District.
Suttef County Office Building, 142 Gardea
Highway. Yuba City. CA 95981
Tehams County Air Pollution Control
District. PH Box 38.1780 Walnut Street.
Red Bluff. CA 9608O
Tuian Cam* Air Pollution Control District
County CMe Cantor. Visalia. CA 93277
Tuolumne County Air Pollution Control
District, 9 North Washington Street
Sonora. CA 95370
Yo4o-Solam> Air Pollvttoa Control District
P.O. Box IBM. 323 First Street **,
WoodUndCAl
(PI
(1) This notice lists in tabular form, only
Air Pollution Control Districts that are
affected by this notice. The table lists each
pollutant category by its subpart letter and
pollutant source name. A star (*) or cross(f)
is used to indicate the specific pollutant
category that an Air Pollution Control District
has been delegated authority over and the
date of that delegation. Delegations effective
as of August 30,1979 are indicated by a star
(*) and delegation* effective as of November
19.197« an indicated by a cross (t).
NEW SOURCE PERFORMANCE STANDARDS (NSPS)
POLLUTION
CONTROL
DISTRICT
POLLUTANT
CATEGORY
DEL NORTE
FRESNC
GREAT BASIN
HUMBOLDT
KERN
KINGS
LOS ANGELES
MENDOCINO
MLKCF.D
MODOC
MONTEREY BAY
NORTHERN SONOMA
SAN BERNARDINO
SAN DIFGO
SAN JOAQUIN
TRINITY
TULA RE
VENTURA
YOLO-SOLANO
f*.
f-»
00
•0 iJ
a> to o>
Fossil Fuel Fii
Steam Ceneratoi
Constructed Aft
D
*
„
*
*
*
*
*
*
*
+
00
r*.
B 00
n —
o> -»
4J (f,
V>
fcj
SS CO 01
Electric Utilit
Generating Unit
Constructed Aft
Da
Incinerators
E
*
Portland Cement Plants
F
*
Nitric Acid Plants
G
Sulfuric Acid Plants
H
Asphalt Concrete Plants
1
+
Petroleum Refineries
J
*
*
A
4
*
*
*
*
*
*
Storage Vessals For
Petroleum Liquids
Constructed After
6/11/73 Prior To 5/17/78
K
*
*
*
*
*
*
+
Storage Vessals For
Petroleum Liquids
Constructed After 5/18/78
Ka
Secondary Lead Smelters
L
*
*
Secondary Brass And Bronze
Ingot Production
M
*
*
u
c
«
r-«
o.
*4
01
-------
H
H
H
I
k NEW SOURCE PERFORMANCE STANDARDS (NSPS)
POLLUTION
CONTROL
DISTRICT
POLLUTANT
CATEGORY
DEL NORTE
FRESNO
GREAT BASIN
HUMBOLDT
KERN
KINGS
LOS ANGELES
MENDOCINO '
MKRCED
MODOC
MONTEREY BAY
NORTHERN SONOMA
SAN BERNARDINO
SAN DIEGO
SAN JOAQUIN
TRINITY
TULA RE
VENTURA
YOLO-SOLANO
Phosphate Fertilizer
Industry: Triple
Super Phosphate Plant
W
*
*
*
*
*
*
*
*
*
Phosphate Fertilizer
Industry: Granular
Triple Super Phosphate
Storage Facilities
X
*
*
*
*
*
*
*
*
*
Coal Preparation Plants
Y
*
*
*
*
*
*
*
*
*
*
*
*
Ferralloy Production
Facilities
z
*
*
*
*
*
*
*
*
*
*
*
*
Steel Plants: Electric
Afc Furnaces
AA
*
*
*
*
*
*
*
*
+
u>
1-1
iH
•H
S
a
t-4
PL.
4J
Iw
«
&
BB
*
*
*
*
*
Grain Elevators
DD
*
*
*
*
*
Stationary Gas
Turbines
GG
Lime Manufacturing
Plants
HH
*
*
*
*
*
Ammonium Sulfate
Manufacture
PP
NATIONAL EMISSION
STANDARDS FOR HAZARDOUS
AIR POLLUTANTS (NESHAPS)
Asbestos
B
*
*
*
it
*
*
*
*
*
*
*
*
+
Beryllium
c
*
*
1t
*
*
*
*
*
*
*
Beryllium Rocket Motor
Firing
D
*
*
it
*
*
*
*
*
*
*
Mercury
E
*
*
*
*
*
*
*
*
*
*
+
Vinyl Chloride
f
*
*
*
*
*
*
*
*
* 8/30/79
+ 11/19/76
15,17,36.40,44,48,52,89, «0
-------
(O>—State of Colorado. Colorado Air
Pollution Control Division. 4210 Eas;
lUh Avenue. Denver. Colorado 80220.20
(H) State of Connecticut, Department
of Enviroiunental Protection, State Of-
fice BuUding, Hartford. Connecticut
•6U5. 3I
(I] State of Delaware (for fossil fuel-fired
steam generators; incinerators: nitric acid
plants; asphalt concrete plants; storage
vessels for petroleum liquids; sulfuric acid
plants; sewage treatment plants; electric
utility steam generating units; stationary gat
turbines and petroleum refineries).
Delaware Department of Natural Resources
and Environmental Control, Tatnall
Building. P.O. Box 1401, Dover, Delaware
19901 81.106,127,148
•1MK) [reserved]
(L) State of Georgia, Environmental Pro-
tection Division, Department of Natural Re-
rnurces, 270 Washington Street. S.W.. At-
lanta. Georgia 30334.38
(M) |Reserved]
(N) State of Idaho, Department of Health
and Welfare, Statehouse. Boise, Idaho 83701.13
(O) [Reserved]
iP) State of Indiana, Indiana Air Pollu-
1.1'.n Control Board, 1330 West Michigan
.•5' -.?et. Indianapolis, Indiana 46206.46.135
(Q) State of Iowa, Iowa Department of
Environmental Quality, Henry A. Wallace
Building, 900 East Grand, Des Moines, Iowa
50318. HI 20
(R)- [reserved].
(S) Division of Air Pollution Control, DC
partment for Natural Resources and Envi-
ronmental Prot«^Hon us 127. Frankfort
Ky. 40601.80
(T) State of Louisiana, Program
Administrator, Air Quality Division.
Louisiana Department of Natural
Resources, P.O. Box 44066, Baton Rouge,
Louisiana 70804.143
(U) State of Maine. Department of Envi-
ronmental Protection. State House. Augusta
Maine 04330.24
(V) State of Maryland: Bureau of Air
Quality and Noise Control, Maryland State
Department of Health and Mental Hygiene,
201 West Preston Street, Baltimore, Maryland
21201.105
(W) Massachusetts Department of Ervt
ronmental Quality Engineering. Division >,,
Air Quality Control, 600 Washington Street.
Boston. Massachusetts 02111.34
(X) State of Michigan, Air Pollution
Control Division. Michigan Department of
Natural Resources. Stevens T. M»s
Health and Environmental Services, Cogs* ?..
Building, Helena, Mont. 60601. 7°
(CC) State of Nebraska. Nebraska
Department of Environmental Control,
P.O. Box 94877, State House Station,
Lincoln, Nebraska 68509.'29
(DD) Nevada.
Clark County. County District Health De-
partment, Air Pollution Control Division.
625 Shadow Lane, Las Vegas. Nev. 89106.
Washoe County District Health Depart-
ment, Division of Environmental Protection,
10 Rinnan Avenue, Reno, Nev. 89502. 89
(EE) New Hampshire Air Pollution
Control Agency, D-partment of Health
and Welfare. State Laboratory Building.
Hazen Drive. Concord, New Hampshire
03301.34
(FT)—8Ute of New Jersey: New Jersey De-
partment of Environmental Protection.
John Pitch Plaza. P.O. Box 2807. Trenton
New Jersey 08626. *3
(GG) [reserved].
(HH)—New York: New York State De-
partment of Environmental Conservation, 6fc
Wolf Road. New York 12233, attention: Divi-
sion of Air Resources.'9
(U) North Carolina Environmental Man-
agement Commission. Department of Natural
and Economic Resources, Division of Envi-
ronmental Management. P.O. Box 37687, Rn
leigh. North Carolina 27611. Attention: Ai
«uallty Section. **
(JJ)-State of North Dakota, State Depart-
ment of Health, State Capitol, Bismarck
North Dakota 58501. *7
(KK) Ohio—
Medina, Summit and Portage Counties:
Director, Air Pollution Control. 177 South
Broadway, Akron. Oh:~ «?OS
Stark County; Director, Mr Pollution COL
trol Division, Canton City Health Depart
ment, City Hall, 216 Cleveland Avenue SW
Canton, Ohio. 44702.
Butler, Ctermont. Hamilton and Warren
Counties: Superintendent, Division of Air
Pollution Control. 2400 Beekman Street, Cin-
cinnati. Ohio. 4fi214.
Cuyahoga County; Commissioner, Division
of Air Pollution Control, Department of
Public Health and Welfare, 2736 Broadway
Avenue, Cleveland. Ohio. 44116.
Lorain County; Control Officer. Division of
Air Pollution Control, 200 West Erie Avenue.
7ih Floor, Lorain, Ohio, 44052.
Belmont, Carroll, Columblana, Harrison.
Jefferson, and Monroe Counties; Director.
North Ohio Valley Air Authority (NOVAA).
814 Adams Street. Steubenvllle, Ohio, 43962.
Clark, Darke, Greene. Miami, Montgomery,
and Preble Counties; Supervisor, Regional
Air Pollution Control Agency (RAPCA),
Montgomery County Health Department, 451
West Third Street, Dayton, Ohio, 45402.
Lucas County and the City of Roesford (in
Wood County); Director, Toledo Pollution
Control Agency. 26 Main Street, Toledo, Ohio,
43609.
Adams, Broi'n, Lawrence, and Sooto
Counties; Engineer-Director, Air Division.
Portsmouth City Health Department, 74<
Second Street, Portsmouth, Ohio, 46662.
Allen, Ashland. Auglalze, Crawford, De
fiance, Erie, Fulton, Hancock. Hardln, Henr
Huron, Knox, Marlon, Mercer, Morrcv
Ottawa, Pauldlng, Putnam. Rlchland, San-
6usky, Seneca. Van Wen, Wllllar ,-
"•'jod (except City of Rosaford), and Wy»n-
dot Counties: Ohio Environmental Protec-
tion Agency, Northwest District Office, 11:
West Washington Street, Bowling Oreen.
Ohio. 43402.
Ashtabula. Geauga, Lake, Mahoning.
Trumbull, and Wayne Counties; Ohio Envi-
ronmental Protection Agency. Northeast Dis-
trict Office. 2110 East Aurora Road, Twim-
burg, Ohio, 44087.
Athens, Ooshocton, Oallla, Guernsey. Hlgl
land, Hocking. Holmes. Jackson, Melg-
Morgan, Uuakingum, Noble, Perry, Plk-
Ross, Tusc&rawas, Vlnton, and WashingUi.
Counties; Ohio Environmental Protectic-
Agency. Southeast District Office, Route 3.
Box 603, Logan, Ohio, 43138.
Champaign. Clinton, Logan, and Shell.v
Counties; Ohio Environmental Proteru-•
Agency, Southwest District Office. 7 I a<-
»*urth Street. Dayton. Ohio. 46402
Delaware, Pmlrftsld. PayetU, Frank: t"
I .Irk Ing, Madison, Pick»way, and Dnlor
Counties; ObJo Environment*! Protection
Afir^y. Ontra! District Office. 369 Eas-.
Broad Street. Columbus. Ohio. 43215.53.l35
(LL) State of Oklahoma, Oklahoma State
Department of Health, Air Quality
Service, P.O. Box 53551, Oklahoma City,
Oklahoma 73152.H7
,MM)—State of Oregon, Department
ol Environmental Quality. 1234 SW?
Viarrison Street, Portland. Oregon 97205.-
(NN)(a) City of Philadelphia: Philadelphia
Department of Public Health. Air Mar-
agement Services. 601 Arch Street, Phllr
delphla. Pennsylvania 19107. "
(NN) (b) Commonwealth of Pennsylvania.
Department of Environmental Resources. Post
Office Box 20b3, Harrisburg, Pennsylvania
17120.'08'"6
(OO) State of Rhode Island. Department of
Environmental Management. 83 Park Street.
Providence, Rhode Island 02908 92-116
(PP) State of South Carolina, Office or
Environmental Quality Control. Department
of Health and Environmental Control, j8OQ
Bull Street. Columbia, South Carolina 2920!?6
«QQ> State of South Dakota, De)>aw-
ment of Environmental Protection, Jo«-
Fu. - BiitidiJifc. Fieur, South Da! -
57- 3?
(RR) Division of Air Pollution Control.
Tennessee Department of Public Health,
256 Capitol Hill Building, Nashville,
Tennessee 37219 128
(SS) State of Texas, Texa/3 Air Con
trol Board, 8520 Shoal Creek Booic
• n-d, Austin, Texas 78758.95
TT)—State of Utah, Utah Air Cor.
-• -ation Committee, State Dlvlslo: o.
nealth, 44 Medical Drive, Salt Lake City
* 84113.37Jj7
(U.' I —state of Vermont. Agency of Envlioi. -
mental Protection. Box 489, Montpe Iti
V- y.irtt. 06602."
W) Commonwealth of Virginia. Vi.
v 111-1 State Air Pollution Control Boar.i
Rt-om 1106, Ninth Street Office Builcinit
Oi hmond. Virginia 23219.30
( VW) (1) Washington: State of Washing
. Department of Ecology, Olympla. Wa*^
ton 985O«.
(li) Northwest Air Pollution Authority, 207
Pioneer Building, Second and Pine Streets.
Mount Vernon, Washington 98273.
(:il) Puget Sound Air Pollution IXra'rr i
Af
-------
Authority. North 811 Jefferson, Spokane.
Washington 90201.
IT; Southwest Air Pollution Control Au-
Uiartty,-Suite 7001 H, NE HazelDe.ll Aveuue,
Vancouver.. Washington 08086. I2.z8
(vi) Olympic Air Pollution Control
Authority, 120 East State Avenue.
Olympia. WA 98501 97
(viii) Benton-Franklin-Walla Walla
Counties Air Pollution Control
Authority. 650 George Washington Way,
Richland. Washington 99352: m
XX) (reserved).
(TT) Wtoconaln—
WKcondn Department of Natural Resources.
P.O. Boi 7931.'Uadlaon. Wisconsin 687073
-------
(&D.5
of
(a) When requested to do so by an
owner or operator, the Administrator
will make a determination of whether
action taken or intended to be taken by
such owner or operator constitutes con-
struction (including reconstruction) or
modification or the commencement
thereof within the meaning of this part.
(b) The Administrator will respond to
any request for a determination under
paragraph (a) of this section within 30
days of receipt of such request.
(e) When requested to do so by ®a
owner or operator, the Administrator will
review plans for construction or modifi-
cation for the purpose of providing
technical advice to the owner or operator.
(b) (1) A separate request shall be sub-
mitted for each construction or modifi-
cation project. 5
(2) Each request shall identify the lo-
cation of such project, and be accom-
panied by technical information describ-
ing the proposed nature, size, design, and
method of operation of each affected fa-
cility involved in such project, including
Information on any requipment to be
used for measurement or control of emis-
sions. 5
(c) Neither a request for plans review
Bor advice furnished by the Administra-
tor in response to such request snail (1)
relieve an owner or operator of legel
responsibility for compliance with aay
provision of this part or of any applics&l®
Stata or local requirement, or (2) preraxfe
the Administrator from implementing csr
enforcing any provision of this part or
taking any other action authorized by fehe
Act.
amsj n-ewsird!
(a) Any owner or operator subject to
the provisions of this part shall furnish
fcfea Administrator written nottflce&ca eo
(1) A notification of the date construc-
tion (or reconstruction as denned under
§ 60.15) of an affected facility is com-
menced postmarked no later than 30
days after such date. This requirement
shall not apply in the case of mass-pro-
duced facilities which are purchased in
completed form.22
(2) A notification of the anticipated
date of initial startup of an affected
facility postmarked not more than 60
days nor less than 30 days prior to such
date. 22
(3) A notification of the actual date
of initial startup of an affected facility
postmarked within 15 days after such
date. 22
(4) A notification of any physical or
operational change to an existing facil-
ity'which may increase the emission rate
of any air pollutant to which a stand-
ard applies, unless that change is spe-
cifically exempted under an applicable
subpart or in i 60.MieM09
This notice shall be postmarked 60 days
or as soon as practicable before the
change is commenced and shall include
information describing the precise na-
ture of the change, present and proposed
emission control systems, productive
capacity of the facility before and after
the change, and the expected comple-
tion date of the change. The Administra-
tor may request additional relevant in-
formation subsequent to this notice. "
(5) A notification of the date upon
which demonstration of the continuous
monitoring system performance com-
mences in accordance with § 60.13(c).
Notification shall be postmarked not less
than 30 days prior to such date.'8
(b) Any owner or operator subject to
the provisions of this part shall main-
tain records of the occurrence and dura-
tion of any startup, shutdown, or mal-
function in the operation of an affected
facility; any malfunction of the air pol-
lution control equipment; or any periods
during which a continuous monitoring
system or monitoring device is inopera-
tive. 18
(c) Each owner or operator required
to install a continuous monitoring sys-
tem shall submit a written report of
excess emissions (as defined in applicable
subparts) to the Administrator for every
calendar quarter. All quarterly reports
shall be postmarked by the 30th day fol-
lowing the-end of each calendar quarter
and shall include the following informa-
tion: 18
.(1) The magnitude of excess emissions
computed in accordance with § 60.13(h),
any conversion factor (s) used, and the
date and time of commencement and
completion of each time period of excess
emissions.18
(2) Specific identification of each
period of excess emissions that occurs
during startups, shutdowns, and mal-
functions of the affected facility. The
nature and cause of any malfunction (if
known), the corrective action taken or
preventative measures adopted.'8
(3) The date and time identifying each
period during which the continuous
monitoring system was inoperative ex-
cept for zero and span checks and the
nature of the system repairs or adjust-
ments. 18
(4) When no excess emissions have
occurred or the continuous monitoring
system (s) have not been inoperative, re-
paired, or adjusted, such information
shall be stated in the report.4. '8
(d) Any owner or operator subject to
the provisions of this part shall maintain
a file of all measurements, including con-
tinuous monitoring system, monitoring
device, and performance testing meas-
urements; all continuous monitoring sys-
tem performance evaluations: all con-
tinuous monitoring system or monitoring
device calibration checks; adjustments
and maintenance performed on these
systems or devices; and all other infor-
mation required by this part recorded in
a permanent form suitable for inspec-
tion. The file shall he retained for at Ipfl^t
two years following the <1at<> of snrh
measurements, maintenance, reports, and
records. 5, 18
'.e> If notification substantially similar
to that in paragraph (a) of this section
is required by any other State or loca
agency, sending the Administrator i,
copy of that notification will satisfy the
requirements of paragraph (a) of this
section.22
ct ta omended (42
tr
•
§ 60.8 Performance tests.
(a) Within 60 days after achieving tin
maximum production rate at which th
affected facility will be operated, but no
later than 180 days after initial startu;
of such facility and at such other time
as may be required by the Administrate)
under section 114 of the Act, the owne
or operator of such facility shall conduc
performance test(s) and furnish the Ad
siinistrator a written report of the result
of such performance test(s).
(b) Performance tests shall be con
ducted and data reduced in accordanc
with the test methods and procedure
contained in each applicable subpar
unless the Administrator (1) specific
or approves, in specific cases, the use o
a reference method with minor change
in methodology, (2) approves the us
of an equivalent method, (3) approve
the use of an alternative method the re
suits of which he has determined to b
adequate for indicating whether a spe
cific source is hi compliance, or
waives the requirement for performani
tests because the owner or operator ,
a source has demonstrated by oth'<
means to the Administrator's satisfac
tlon that the affected facility is in, com
pliance with the standard. Nothing ii
this paragraph shall be construed b
abrogate the Administrator's authorit;
to require testing under section 114 o:
the Act.5
(c) Performance tests shall be con-
ducted under such conditions as the Ad-
ministrator shall specify to the planl
operator based on representative per-
formance of the affected facility. Tht
owner or operator shall make available
to the Administrator such records as maj
be necessary to determine the conditions
of the performance tests. Operations
during periods of startup, shutdown, anc
malfunction shall not constitute repre-
sentative conditions for the purpose of a
performance test nor shall emissions Ir
excess of the level of the applicable emis-
sion limit during periods of 'startup
shutdown, and malfunction be con-
sidered a violation of the applicable
emission limit unless otherwise specified
in the applicable standard.4-74
(d) The owner or operator of an
affected facility shall provide the
Administrator at least 30 days prior
notice of any performance test, except
as specified under other subparts, to
afford the Administrator the opportunity
to have an observer present.5'98 £
(e) The owner or operator of
affected facility shall provide, or causi
111-10
-------
provided, performance
as follows:
testing £&cil=
(1) Sampling ports adequate for test
methods applicable to such facility.
<2> Safe sampling platform (s).
(3) Safe access to sampling plat-
form (s).
(4) Utilities for sampling and testing
equipment.
(f) Unless otherwise specified in the
applicable subpart, each performance
test shall consist of three separate runs
using the applicable test method. Each
run shall be conducted for the time and
under the conditions specified in the
applicable standard. For the purpose of
determining compliance with an
applicable standard, the arithmetic
means of results of the three runs shall
apply. In the event that a sample is
accidentally lost or conditions occur in
which one of the three runs must be
discontinued because of forced
shutdown, failure of an irreplaceable
portion of the sample train, extreme
meteorological conditions, or other
circumstances, beyond the owner or
operator's control, compliance may,
upon the Administrator's approval, be
determined using the arithmetic mean of
She results of the two other runs.5'98
(Sec. 110. Clean AH- Act \a amended (42
U.S.C. 7014)). 68,33
§ 60.9 Availability of information.
The availabality to the public of in-
formation provided to, or otherwise ob-
tained by, the Administrator under this
Part shall be governed by Part 2 of this
chapter. (Information submitted volun-
tarily to the Administrator for the pur-
poses of §§ 60.5 and 60.6 is governed by
§ 2.201 through § 2.213 of this chapter
and not by § 2.301 of this chapter.)
(Sec. 114. Oeon Air Act to amended (43
U.S.C. 7414)).68'83
§ 60.1® State authority.
The provisions of this part shall not
be construed in any manner to preclude
any State or political subdivision thereof
from:
(a) Adopting and enforcing any emis-
sion standard or limitation applicable to
an affected facility, provided that such
emission standard or limitation is not
less stringent than the standard appli-
cable to such facility.
(b) Requiring the owner or operator
of an affected facility to obtain permits,
licenses, or approvals prior to initiating
construction, modification, or operation
of such facility.
I (Sec. 116 of the Clean Air Act as amended
(42U.S.C. 7416)). 68,83
§ 60.11 Complianco with otendarcSo and
maintenance requlrementa
(a) Compliance with standards in this
part, other than opacity standards, shall
be determined only by performance
tests established by § 60.8, unless
otherwise specified in the applicable
standard.1"
(b) Compliance with opacity stand-
ards in this part shall be determined by
conducting observations in accordance
with Reference Method 9 in Appendix A
of this part or any alternative method
that is approved by the Administrator.
Opacity readings of portions of plumes
which contain condensed, uncombined
water vapor shall not be used for pur-
poses of determining compliance with
opacity standards. The results of con-
tinuous monitoring by transmissometer
which indicate that the opacity at the
time visual observations were made was
not in excess of the standard are proba-
tive but not conclusive evidence of the
actual opacity of an emission, provided
that the source shall meet the burden of
proving that the instrument used meets
(at the time of the alleged violation)
Performance Specification 1 in Appendix
B of this part, has been properly main-
tained and (at the time of the alleged
violation) calibrated, and that the
resulting data have not been tampered
with in any way.ia60
(c) The opacity standards set forth In
this part shall apply at all times except
during periods of startup, shutdown, mal-
function, and as otherwise provided in
the applicable standard.
(d) At all times, including periods of
startup, shutdown, and malfunction,
owners and operators shall, to the extent
practicable, maintain and operate any
affected facility Including associated air
pollution control equipment in a manner
consistent with good air pollution control
practice for minimizing emissions. De-
termination of whether acceptable oper-
ating and maintenance procedures are
being used will be based on Information
available to the Administrator which may
Include, but is not limited to, monitoring
results, opacity observations, review of
operating and maintenance procedures,
and inspection of the source.
(e) (1) An owner or operator of an af-
fected facility may request the Admin-
istrator to determine opacity of emis-
sions from the affected facility during
the initial performance tests required by
§ 60.8.10
(2) Upon receipt from such owner or
operator of the written report of the re-
sults of the performance tests required
by § 60.8, the Administrator will make
a finding concerning compliance with
opacity and other applicable standards.
If the Administrator finds that an af-
fected facility is in compliance with all
applicable standards for which perform-
ance tests are conducted in accordance
with § 60.8 of this part but during the
time such performance tests are being
conducted fails to meet any applicable
opacity standard, he shall notify the
owner or operator and advise him that he
may petition the Administrator within
10 days of receipt of notification to make
appropriate adjustment to the opacity
standard for the affected facility.10
(3) The Administrator will grant such
a petition upon a demonstration by the
owner or operator that the affected fa-
cility and associated air pollution con-
trol equipment was operated and main-
tained in a manner to minimize the
opacity of emissions during the perform-
ance tests; that the performance tests
were performed under the conditions es-
tablished by the Administrator; and that
the affected facility and associated air
pollution, control equipment were In-
capable of being adjusted or operated to
meet the applicable opacity standard.10
(4) The Administrator will establish
an opacity standard for the affected
facility meeting the above requirements
at a level at which the source will be
able, as Indicated by the performance
and opacity tests, to meet the opacity
standard at all times during which the
source is meeting the mass or concentra-
tion emission standard. The Adminis-
trator will promulgate the new opacity"
standard in the FEDERAL REGISTER.10
(Sec. 114. Clean Air Act Is emended (42
U.S.C. 7414)). 68, 83
§ 60.12 Circumvention.
No owner or operator subject to the
provisions of this part shall build, erect,
Install, or use any article, machine,
equipment or process, the use of which
conceals an emission which would other-
wise constitute a violation of an applica-
ble standard. Such concealment In-
cludes, but Is not limited to, the use of
gaseous diluents to achieve compliance
with an opacity standard or with a
standard which is based on the concen-
tration of a pollutant in the gases dis-
charged to the atmosphere.
10
§60.13 Monitoring requirements.
(a) For the purposes of this section,
all continuous monitoring systems re-
quired under applicable subparts shall
be subject to the provisions of this sec-
tion upon promulgation of perfor-
mance specifications for continuous
monitoring system under Appendix B
to this part, unless:82
(1) The continuous monitoring
system fs subject to the provisions of
paragraphs (c)(2) and (c)(3) of this
' section, or82
(2) otherwise specified in an applica-
ble subpart or by the Administrator.82
(b) All continuous monitoring systems
and monitoring devices shall be installed
and operational prior to conducting per-
formance tests under § 60.8. Verification
of operational status shall, as a mini-
mum, consist of the following:
III-ll
-------
(1) For continuous monitoring sys-
tems referenced in paragraph (c) (1) of
this section, completion of the condi-
tioning/period, specified by applicable
requirements in Appendix B.
(2) For continuous "monitoring sys-
tems referenced in paragraph (c) (2) of
this section, completion of seven days of
operation.
(3) For monitoring devices referenced
in applicable subparts, completion of the
manufacturer's written requirements or
recommendations for checking the op-
eration, or calibration of the device.
(c) During any performance tests
required under § 60.8 or within 30 days
thereafter and at such other times as
may be required by the Administrator
under section 114 of the Act, the owner
or operator of any affected- facility shall
conduct continuous monitoring system
performance evaluations and furnish the
Administrator within 60 days thereof two
or, upon request, more copies of a written
report of the results of such tests. These
continuous monitoring system perform-
ance evaluations shall be conducted in
accordance with the following specifica-
tions and procedures:
(1) Continuous monitoring systems
listed within this paragraph except as
provided in paragraph (c) (2) of this sec-
tion shall be evaluated in accordance
with the requirements and procedures
contained in the applicable perform-
ance specification of Appendix B as
follows:
(i) Continuous monitoring systems for
measuring opacity of emissions shall
comply with Performance Specification 1.
(ii) Continuous monitoring systems for
measuring nitrogen oxides emissions
shall comply with Performance Specifi-
cation 2.
(ill) Continuous monitoring systems for
measuring sulfur dioxide emissions shall
comply with Performance Specification 2.
(iv) Continuous monitoring systems for
measuring the oxygen content or carbon
dioxide content of effluent gases shall
comply with Performance Specification
3.
(2) AJI owner or operator who, prior
to September 11, 1974, entered Into a
binding contractual obligation to pur-
chase specific, continuous monitoring
system components except as referenced
by paragraph (c) (2) (iii) of this section
shall comply with the following require-
ments:
(i) Continupus monitoring systems for
measuring opacity of.emissions shall be
capable of measuring emission levels
within ±20 percent with a confidence
level of 95 percent. The Calibration Error
Test and associated calculation proce-
dures set forth in Performance Specifi-
cation 1 of Appendix B shall be used for
demonstrating compliance with this
specification.
(ii) Continuous monitoring systems
for measurement of nitrogen oxides or
sulfur dioxide shairbe capable of meas-
uring emission levels within ±20 percent
with a confidence level of 95 percent. The
Calibration Error Test, the Field Test
for Accuracy (Relative), and associated
operating and calculation procedures set
forth in Performance Specification 2 of
Appendix B shall be used for demon-
strating compliance with this specifica-
tion.
(ill) Owners or operators of all con-
tinuous monitoring systems installed on
an affected facility prior to October 6,
1975 are not required to conduct
tests under paragraphs (c) (2) (i) and/or
(ii) of this section unless requested by
the Administrator.23
(3) All continuous monitoring systems
referenced by paragraph (c) (2) of this
section shall be upgraded or replaced (if
necessary) with new continuous moni-
toring systems, and the new or improved
systems shall be demonstrated to com-
ply with applicable performance speci-
fications under paragraph (c) (1) of this
section on or before September 11, 1979.
(d) Owners or operators of all con-
tinuous monitoring systems Installed in
accordance with the provisions of this
part shall check the zero and span drift
at least once daily in accordance with
the method prescribed by the manufac-
turer of such systems unless the manu-
facturer recommends adjustments at
shorter intervals, in which case such
recommendations shall be followed. The
zero and span shall, as a minimum, be
adjusted whenever the 24-hour zero drift
or 24-hour calibration drift limits of the
applicable performance specifications in
Appendix B are exceeded. For continuous
monitoring systems measuring opacity of
emissions, the optical surfaces exposed
to the effluent gases shall be cleaned prior
to performing the zero or span drift ad-
justments except that for systems using
automatic zero adjustments, the optical
surfaces shall be cleaned when the cum-
ulative automatic zero compensation ex-
ceeds four percent opacity. Unless other-
wise approved by the Administrator, the
following procedures, as applicable, shall
be followed:
(1) For extractive continuous moni-
toring systems measuring gases, mini-
mum procedures shall include introduc-
ing applicable zero and span gas mixtures
into the measurement system as near the
probe as is practical. Span and zero gases
certified by their manufacturer to bs
traceable to National Bureau of Stand-
ards reference gases shall be used when-
ever these reference gases are available.
The span and zero gas mixtures shall be
the same composition as specified in Ap-
pendix B of this part. Every six months
from date of manufacture, span and zero
gases shall be reanalyzed by conducting
triplicate analyses with Reference Meth-
ods 6 for SO«, 7 for NO,, and 3 for O,
and CO», respectively. The gases may ba
eaaSyzed at less frequent intervals itf
longer shelf lives are guaranteed by the
manufacturer.
(2) For non-extractive continuous
monitoring systems measuring gases,
minimum procedures shall include up-
scale check(s) using a certified calibra-
tion gas cell or test cell which is func-
tionally equivalent to a known gas con-
centration. The zero check may be per-
formed by computing the zero value from
upscale measurements or by mechani-
cally producing a zero condition.
(3) For continuous monitoring systems
measuring opacity of emissions, mini-
mum procedures shall include a method
for producing a simulated zero opacity
condition and an upscale (span) opacity
condition using a certified neutral den-
sity filter or other related technique to
produce a known obscuration of the light
beam. Such procedures shall provide a
system check of the analyzer internal
optical surfaces and all electronic cir-
cuitry including the lamp and photode-
tector assembly.
(e) Except for system breakdowns, re-
pairs, calibration checks, and zero and
span adjustments required under para-
graph (d) of this section, all continuous
monitoring systems shall be in contin-
uous operation and shall meet minimum
frequency of operation requirements as
follows:
(1) All continuous monitoring sys-
tems referenced by parafjraphs (c)(l)
and (c) (2) of this section for measuring
opacity of emissions shall complete a
minimum of one cycle of sampling and
analyzing for each successive ten-second
period and one cycle of data recording
for each successive six-minute period.5'
(2) All continuous monitoring systems
referenced by paragraph (c) (1) of this
section for measuring oxides of nitrogen,
sulfur dioxide, carbon dioxide, or oxyge:
shall complete a minimum of one cycl<
of operation (sampling, analyzing, and
data recording) for each successive 15-
minute period.
(3) All continuous monitoring systems
referenced by paragraph (c) (2) of this
section, except opacity, shall complete a
minimum of one cycle of operation (sam-
pling, analyzing, and data recording)
for each successive one-hour period.
(f) All continuous monitoring systems
or monitoring devices shall be Installed
such that representative measurements
of emissions or process parameters from
the affected facility are obtained. Addi-
tional procedures for location of contin-
uous monitoring systems contained in
the applicable Performance Specifica-
tions of Appendix B of this part shall be
used.
(g) When the effluents from a single
affected facility or two or more affected
facilities subject to the same emission
standards are combined before being re-
leased to the atmosphere, the owner or
operator may install applicable contin-
uous monitoring systems on each effluent
or on the combined effluent. When the af-
fected facilities are not subject to the
same emission standards, separate con-
tinuous monitoring systems shall be in-
stalled on each effluent. When the efflu-
ent from one affected facility is released
to the atmosphere through more than
one point, the owner or operator sha:
install applicable continuous monitor!:
systems on each separate effluent unli
111-12
-------
the installation of fewer systems is ap- •
proved by the Administrator.
(h) Owners or operators of all con-
tinuous monitoring systems for measure-
ment of opacity shall reduce all data to
six-minute averages and for systems
other than opacity to one-hour averages
for time periods under § 60.2 (x) and (r)
respectively. Six-minute opacity averages
sha'l be calculated from 24 or more data
points equally spaced over each six-
minute period. For systems other than
opacity, one-hour averages shall be com-
puted from four or more data points
equally spaced over each one-hour pe-
riod. Data recorded during periods of sys-
tem breakdowns, repairs, calibration
checks, and zero and span adjustments
shall not be Included in the data averages
computed under this paragraph. An
arithmetic or integrated average of all
data may be used. The data output of all
continuous monitoring systems may be
recorded in reduced or nonreduced form
(e.g. ppm pollutant and percent CX or
lb/million Btu of pollutant). All excess
emissions shall be converted into units
of the standard using the applicable con-
version procedures specified in subparts.
After conversion into units of the stand-
ard, the data may be rounded to the same
number of significant digits used in sub-
parts to specify the applicable standard
(e.g., rounded to the nearest one percent
opacity).
(1) After receipt and consideration of
written application, the Administrator
may approve alternatives to any moni-
toring procedures or requirements of this
part including, but not limited to QIQ
following:42
(1) Alternative monitoring require-
ments when installation of a continuous
monitoring system or monitoring device
specified by this part would not provide
accurate measurements due to liquid wa-
ter or other interferences caused by sub-
stances with the effluent gases.
(2) Alternative monitoring require-
ments when the affected facility is infre-
quently operated.
(3) Alternative monitoring require-
ments to accommodate continuous moni-
toring systems that require additional
measurements to correct for stack mois-
ture conditions.
(4) Alternative locations for installing
continuous monitoring systems or moni-
toring devices when the owner or opera-
tor can demonstrate that installation at
alternate locations will enable accurate
and representative measurements.
(5) Alternative methods of converting
pollutant concentration measurements to
units of the standards.
(6) Alternative procedures for per-
forming daily checks of zero and span
drift that do not involve use of span gases
or test cells.
(7) Alternatives to the A.S.T.M. test
methods or sampling procedures specified
by any subpart.
(8) Alternative continuous monitor-
ing systems that do not meet the design
or performance requirements in Perform-
ance Specification 1, Appendix B, but
adequately demonstrate a definite and
consistent relationship between its meas-
urements and the measurements of
opacity by a system complying with the
requirements in Performance Specifica-
tion 1. The Administrator may require
that such demonstration be performed
for each affected facility.
(9) Alternative monitoring require-
ments when the effluent from a single
affected facility or the combined effluent
from two or more affected facilities are
released to the atmosphere through more
than one point.
(Sec. 11<3, Clean Air Act la caneaded (42
U.S.C. 7<11<1)).68, 83
§ 80.14 Modification.22
(a) Except as provided under
paragraphs (e) and (f) of this section,
any physical or operational change to an
existing facility which results in an
increase in the emission rate to the
atmosphere of any pollutant to which a
standard applies shall be considered a
modification within the meaning of
oection 111 of the Act. Upon modification,
an existing facility shall become an af-
fected facility for each pollutant to
which a standard applies and for which
there is an increase in the emission rate
to the atmosphere.109
(b) Emission rate shall be expressed as
kg/hr of any pollutant discharged into
the atmosphere for which a standard is
applicable. The Administrator shall use
the following to determine emission rate:
(1) Emission factors as specified in
the latest issue of "Compilation of Air
Pollutant Emission Factors," EPA Pub-
lication No. AP-42, or other emission
factors determined by the Administrator
to be superior to AP-42 emission factors,
in cases where utilization of emission
factors demonstrate tuat the emission
level resulting from the physical or op-
erational change will cither clearly in-
crease or clearly not increase.
(2) Material balances, continuous
monitor data, or manual emission tests
in cases where utilization of emission
factors as referenced in paragraph (b)
(1) of this section does not demonstrate
to the Administrator's satisfaction
whether the emission level resulting from
the physical or operational change will
either clearly increase or clearly not in-
crease, or where an owner or operator
demonstrates to the Administrator's
satisfaction that there are reasonable
grounds to dispute the result obtained by
the Administrator utilizing emission fac-
tors as referenced in paragraph (b)(l)
of this section. When the emission rate
is based on results from manual emission
tests or continuous monitoring systems,
the procedures specified in Appendix C
of this part shall be used to determine
whether an increase in emission rate has
occurred. Tests shall be conducted under
such conditions as the Administrator
shall specify to the owner or operator
based on representative performance of
the facility. At least three valid test
runs must be conducted before and at
least three after the physical or opera-
tional change. All operating parameters
which may affect emissions must be held
constant to the maximum feasible degree
for all test runs.
(c) The addition of an affected facility
to a stationary source as an expansion
to that source or as a replacement for
an existing facility shall not by itself
bring within the applicability of this
part any other facility within that
source.
(d) [Reserved] '°9
(e) The following shall not, by them-
selves, be considered modifications under
this part:
(1) Maintenance, repair, and replace-
ment which the Administrator deter-
mines to be routine for a source category,
subject to the provisions of paragraph
(c) of this section and % 60.15.
(2) An increase in production rate of
an existing facility, if that increase can
be accomplished without a capital ex-
penditure on that facility. 9°
(3) An increase in the hours of opera-
tion.
(4) Use of an alternative fuel or raw
material if, prior to the date any stand-
ard under tills part becomes applicable
to that source type, as provided by § 60.1,
the existing facility was designed to ac-
commodate that alternative use. A
facility shall be considered to be designed
to accommodate an alternative fuel or
raw material if that use could be accom-
plished under the facility's construction
specifications as amended prior to the
change. Conversion to coal required
for energy considerations, as specified
in section lll(a)(8) of the Act, shall not
be considered a modification.'09
(5) The addition or use of any system
or device whose primary function is the
reduction of air pollutants, except when
an emission control system is removed
or is replaced by a system which the Ad-
ministrator determines to be less en-
vironmentally beneficial.
(6) The relocation or change In
ownership of an existing facility.
{f) Special provisions set forth under
an applicable subpart of this part shall
siapsrsede any conflicting provisions of
this section.
(g) Within 180 days of the completion
of any physical or operational change
subject to the control measures specified
in paragraph (a) of this section,
compliance with all applicable
standards must be achieved.109
111-13
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§ 60.15 Reconstruction.22
(a) An existing facility, upon recon-
struction, becomes an affected facility,
Irrespective of any change in emission
rate.
(b) "Reconstruction" means the re-
placement of components of an existing
facility to such an extent that:
(1) The fixed capital cost of the new
components exceeds 50 percent of the
fixed capital cost that would be required
to construct a comparable entirely new
facility, and
(2) It is technologically and econom-
ically feasible to meet the applicable
standards set forth in this part.
(c) "Fixed capital cost" means the
capital needed to provide all the de-
preciable components.
(d) If an owner or operator of an
existing facility proposes to replace com-
ponents, and the fixed capital cost of the
new components exceeds 50 percent of
the fixed capital cost that would be re-
quired to construct a comparable en-
tirely new facility, he shall notify the
Administrator of the proposed replace-
ments. The notice must be postmarked
60 days (or as soon as practicable) be-
fore construction of the replacements is
commenced and must include the fol-
lowing information:
(1) Name and address of the owner
or operator.
(2) The location of the existing facil-
ity.
(3) A brief description of the existing
facility and the components which are to
be replaced.
(4) A description of the existing air
pollution control equipment and the
proposed air pollution control equip-
ment.
(5) An estimate of the fixed capital
cost of the replacements and of con-
structing a comparable entirely new
facility.
(6) The estimated life of the existing
facility after the replacements.
(7) A discussion of any economic or
technical limitations the facility may
have in complying with the applicable
standards of performance after the pro-
posed replacements.
(e) The Administrator will deter-
mine, within 30 days of the receipt of the
notice required by paragraph (d) of this
section and any additional information
he may reasonably require, whether the
proposed replacement constitutes re-
construction.
(f) The Administrator's determination
under paragraph (e) shall be based on:
(1) The fixed capital cost of the re-
placements in comparison to the fixed
capital cost that would be required to
construct a comparable entirely new
facility;
(2) The estimated life of the facility
after the replacements compared to the
life of a comparable entirely new facility;
(3) The extent to which the compo-
nents being replaced cause or contribute
to the emissions from the facility; and
(4) Any economic or technical limita-
tions on compliance with applicable
standards of performance which are in-
herent in the proposed replacements.
(g) Individual subparts of this part
may include specific provisions which
refine and delimit the concept of recon-
struction set forth in this section.
560.16 Priority Hst."'M°
Prioritized Major Source Categories
Priority Number'
Source Category
1. Synthetic Organic Chemical Manufacturing
(a) Unit processes
(b) Storage and handling equipment
(c) Fugitive emissions sources
(d) Secondary sources
2. Industrial Surface Coating: Cane
3. Petroleum Refineries: Fugitive Sources
4. Industrial Surface Coating: Paper
5. Dry Cleaning
(a) Perchloroethylene
(b) Petroleum solvent
6. Graphic Arts
7. Polymers and Resins: Acrylic Resins
8. Mineral Wool (Deleted)
9. Stationary Internal Combustion Engines
10. Industrial Surface Coating: Fabric
11. Fossil-Fuel-Flred Steam Generators:
Industrial Boilers
12. Incineration: Non-Municipal [Deleted)
13. Non-Metallic Mineral Processing
14. Metallic Mineral Processing
IS. Secondary Copper (Deleted)
16. Phosphate Rock Preparation
17. foundries: Steel and Gray Iron
18. Polymers and Resins: Polyethylene
19. Charcoal Production
20. Synthetic Rubber
(H) Tire manufacture
(b) SBR production
21. Vegetable Oil
22. Industrial Surface Coating: Metal Coil
23. Petroleum Transportation and Marketing
24. By-Product Coke Ovens
25. Synthetic Fibers
26. Plywood Manufacture
27. Industrial Surface Coating: Automobile*
28. Industrial Surface Coating: Large
Appliances
29. Crude Oil and Natural Gas Production
30. Secondary Aluminum
31. Potash (Deleted)
32. Lightweight Aggregate Industry: Clay,
Shale, and Slate *
33. Glass
34. Gypsum
35. Sodium Carbonate
36. Secondary Zinc (Deleted)
37. Polymers and Resins: Phenolic
38. Polymers and Resins: Urea-Melamine
39. Ammonia (Deleted)
40. Polymers and Resins: Polystyrene
41. Polymers and Resins: ABS-SAN Resins
42. Fiberglass
43. Polymers and Resins: Polypropylene
44. Textile Processing
45. Asphalt Roofing Plants
46. Brick and Related Clay Products
47. Ceramic Clay Manufacturing (Deleted)
48. Ammonium Nitrate Fertilizer
49. Castable Refractories (Deleted)
50. Borax and Boric Acid (Deleted)
51. Polymers and Resins: Polyester Resins
52. Ammonium Sulfate
53. Starch
54. Perlite
55. Phosphoric Acid: Thermal Process
(Deleted)
56. Uranium Refining
57. Animal Feed Defluorination (Deleted)
58. Urea (for fertilizer and polymers)
59. Detergent (Deleted)
Other Source Categories
Lead acid battery manufacture "
Organic solvent cleaning 3
Industrial surface coating: metal furniture '
Stationary gas turbines '
(Section 111. 301(a), Clean Air Act as
amended (42 U.S.C. 7411. 7001))
1 Low numbers have highest priority, e.g., No. 1 is
high priority. No. 59 is low priority.
-Formerly tilled "Sintering: Clay and Fly Ash".
3 Minor source category, but included on list since
an NSPS is being developed for that source
category.
' Not prioritized, since an NSPS for this major
source category has already been proumlgated.
111-14
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Subpart B—Adoption and Submlttal of
State Plans for Designated Facilities21
g 60.20 Applicability.
The provisions of this subpart apply
to States upon publication of a final
guideline document under f 60.22(a).
g 60.21 Definitions.
Terms used but not defined In this
subpart shall have the meaning given
them In the Act and in subpart A:
(a) "Designated pollutant" means any
sir pollutant, emissions of which are
subject to a standard of performance for
new stationary sources but for which air
quality criteria have not been issued,
and which is not Included on t list pub-
lished under section 108(a) or section
112 (1HA) of the Act.
(b) "Designated facility" means any
existing facility (see 560.2(aa)) which
emits a designated pollutant and which
would be subject to a standard of per-
formance for that pollutant If the exist-
ing facility were an affected facility (see
J60.2(e)>.
(c) "Plan" means a plan under sec-
tion llKd) of the Act which establishes
emission standards for designated pol-
lutants from ^designated facilities and
provides for "the Implementation and
enforcement of such emission standards.
(d) "Applicable plan" means the plan,
or most recent revision thereof, which
has been approved under § 60.27 (b) or
promulgated under 5 60.27(d).
(e) "Emission guideline" means a
guideline set forth in subpart C of this
part, or in a final guideline document
published under §60.22(a>, which re-
flects the degree of emission reduction
achievable through the application of the
best system of emission reduction which
(taking into account the cost of such
reduction) the Administrator has de-
termined has been adequately demon-
strated for designated facilities.
(f) "Emission standard" means a
legally enforceable regulation setting
forth an allowable rate of emissions into
the atmosphere, or prescribing equip-
ment specifications for control of air pol-
lution emissions.
(g) "Compliance schedule" means a
legally enforceable schedule specifying
a date or dates by which a source or cate-
gory or sources must comply with specific
emission standards contained In a plan
or with any increments of progress to
achieve such compliance.
(h) "Increments of progress" means
steps to achieve compliance which must
be taken by an owner or operator of a
designated facility, Including:
(1) Submittal of a final control plan
for the designated facility to the appro-
priate air pollution control agency;
(2) Awarding of contracts for emis-
sion control systems or for process modi-
fications, or issuance of orders for the
purchase of component parts to accom-
plish emission control or process modi-
fication.
(3) Initiation of on-site construction
or Installation of emission control equip-
ment or process change:
(4) Completion of on-slte construc-
tion or installation of emission control
equipment or process change; and
(5) Final compliance.
(i) "Region" means an air quality con-
trol region designated under section 107
of the Act and described in Part 81 of
this chapter.
(j) "Local agency" means any local
governmental agency.
§ 60.22 Publication of guideline docu-
ments, emission guidelines, and final
compliance times.
(a) After promulgation of a standard
of performance for the control of a des-
ignated pollutant from affected facilities.
the Administrator will publish a draft
guideline document containing Informa-
tion pertinent to control of the desig-
nated pollutant from designated facil-
ities. Notice of the availability of the
draft guideline document will be pub-
lished In the FEDERAL REGISTER, and pub-
lic comments on Its contents will be In-
vited. After consideration of public com-
ments, a final guideline document will be
published and notice of its availability
will be published In the FEDERAL REGISTER.
(b) Guideline documents published
under this section will provide informa-
tion for the development of State plans,
such as:
(1) Information concerning known or
suspected endangerment of public health
or welfare caused, or contributed to, by
the designated pollutant.
(2) A description of systems of emis-
sion reduction which, In the judgment
of the Administrator, have been ade-
quately demonstrated.
(3) Information on the degree of emis-
sion reduction which Is achievable with
each system, together with information
on the costs and environmental effects of
applying each system to designated fa-
cilities.
(4) Incremental periods, of time nor-
mally expected to be necessary for the
design, installation, and startup of iden-
tified control systems.
(5) An emission guideline that reflects
the application of the best system of
emission reduction (considering the cost
of such reduction) that has been ade-
quately demonstrated for designated fa-
cilities, and the time within which com-
pliance with emission standards of equiv-
alent stringency can be achieved. The
Administrator will specify different emis-
sion guidelines or compliance times or
both for different sizes, types, and classes
of designated facilities when costs of
control, physical limitations, geographi-
cal location, or similar factors make sub-
categorization appropriate.
(6) Such other available Information
as the Administrator determines may
contribute to the formulation of State
plans.
(c) Except as provided In paragraph
(d) (1) of this section, the emission guide-
lines and compliance 'times referred to
In paragraph (b) (5) of this section win
be proposed for comment upon publica-
tion of the draft guideline document,
and after consideration of comments will
be promulgated in Subpart C of this part
with such modifications as may be ap-
propriate.
(d) (1) If the Administrator determines
that a designated pollutant may cause
or contribute to endangerment of public
welfare, but that adverse effects on pub-
lic health have not been demonstrated,
he will include the determination In the
draft guideline document and in the FED-
ERAL REGISTER notice of its availability.
Except as provided in paragraph (d) (2)
o' this section, paragraph (c) of this
section shall be Inapplicable in such
cases.
(2) If the Administrator determines at
any time on the basis of new information
that a prior determination under para-
graph (d) (1) «f this section is incorrect
or no longer correct, he will publish
notice of the determination In the FED-
ERAL REGISTER, revise the guideline docu-
ment as necessary under paragraph (a)
of this section, and propose and promul-
gate emission guidelines and compliance
times under paragraph (e) of thia
section.
§ 60.23 Adoption and subinitml of State
plans; public hearings.
(a)U> Within nine months after no-
tice of the availability of a final guide-
line document is published under | 60.22
(a), each State shall adopt and submit
to the Administrator, in accordance with
§ 60.4, a plan for the control of the desig-
nated pollutant to which the guideline
document applies.
(2) Within nine months after notice of
the availability of a final revised guide-
line document Is published as provided
in ? 60.22(d)(2), each State shall adopt
and submit to the Administrator any
plan revision necessary to meet the re-
quirements of this subpart.
(b) If no designated facility is located
within a State, the State shall submit
a letter of certification to that effect to
the Administrator within the time spe-
cified in paragraph (a) of this section.
Such certification shall exempt the State
from the requirements of this subpart
for that designated pollutant.
(c)U) Except as provided In para-
graphs (c) (2) and (c) (3) of this section,
the State shall, prior to the adoption of
any plan or revision thereof, conduct
one or more public hearings within the
State on such plan or plan revision.
(2) No hearing shall be required for
any change to an Increment of progress
In an approved compliance schedule un-
less the change Is likely to cause the
facility to be unable to comply with the
final compliance date In the schedule.
(3) No hearing shall be required on
an emission standard in effect prior to
the effective date of this subpart If It was
adopted after a public hearing and is
at least as stringent as the corresponding
emission guideline specified in the appli-
cable guideline document published
under 5 60.22(a).
(d) Any hearing required by para-
graph (c) of this section shall be held
only after reasonable notice. Notice shall
be given at least 30 days prior to the
date of such hearing and shall include:
(1) Notification to the public by
prominently advertising the date, time.
and place of such hearing In each region
affected;
(2) Availability, at the time of public
announcement, of each proposed plan or
111-15
-------
revision thereof for public Inspection In
at least one location in each region to
which it will apply;
(3) Notification to fee Administrator;
(4) Notification to each local air pol-
lution control agency in each region to
which the plan or revision will apply; and
(5) In the case of an interstate re-
gion, notification to any other State in-
cluded in the region.
(e) The State shall prepare and retain,
for a minimum of 2 years, a record of
each hearing for inspection by any Inter-
ested party. The record shall contain, as
a minimum, a list of witnesses together
with the text of each presentation.
(f) The State shall submit with the
plan or revision:
(1) Certification that each hearing re-
quired by paragraph (c) of this section
was held in accordance with the notice
required by paragraph (d) of this sec-
tion; and
(2) A list of witnesses and their orga-
nizational affiliations, if any, appearing
at the hearing and a brief written sum-
mary of each presentation or written
submission.
(g) Upon written application by a
State agency (through the appropriate
Regional Office), the Administrator may
approve State procedures designed to in-
sure public participation in the matters
for which hearings are required and pub-
lic notification of the opportunity to par-
ticipate if, in the judgment of the Ad-
ministrator, the procedures, although
different from the requirements of this
subpart, in fact provide for adequate
notice to and participation of fee public.
The Administrator may impose such con-
ditions on his approval as he deems
necessary. Procedures approved under
this section shall be deemed to satisfy the
requirements of this subpart regarding
procedures for public hearings.
§ 60.24 Emission standards and compli-
ance schedules.
(a) Each plan shall Include emission
standards and compliance schedules.
-------
standard or compliance schedule of the
plan.
(2) Identification of the achievement
of any increment of progress required by
the applicable plan during the reporting
period.
(3) Identification of designated facili-
ties that have ceased operation during
the reporting period.
(4) Submission of emission inventory
data as described in paragraph (a) of
this section for designated facilities that
were not in operation at the time of plan
development but began operation during
the reporting period.
- (5) Submission of additional data as
necessary to update the information sub-
mitted under paragraph (a) of this sec-
tion or in previous progress reports.
(6) Submission of copies of technical
reports on all performance testing on
designated facilities conducted under
paragraph (b) (2) of this section, com-
plete with concurrently recorded process
data.
§ 60.26 Legal authority.
(a) Each plan shall show that the
State has legal authority to carry out
the plan, including authority to:
(1) Adopt emission standards and
compliance schedules applicable to des-
ignated facilities.
(2) Enforce applicable laws, regula-
tions, standards, and compliance sched-
ules, and seek injunctive relief.
(3) Obtain information necessary to
determine whether designated facilities
are in compliance with applicable laws,
regulations, standards, and compliance
schedules, including authority to require
recordkeeping and to make inspections
and conduct tests of designated facilities.
(4) Require owners or operators of
designated facilities to install, maintain,
and use emission monitoring devices and
to make periodic reports to the State on
the nature and amounts of emissions
from such facilities; also authority for
the State to make such data available to
the public as reported and as correlated
with applicable emission standards.
(b) The provisions of law or regula-
tions which the State determines provide
the authorities required by this section
shall be specifically identified. Copies of
such laws or regulations shall be sub-
mitted with the plan unless:
(1) They have been approved as por-
tions of a preceding plan submitted
under this subpart or as portions of an
implementation plan submitted under
section 110 of the Act, and
(2) The State demonstrates that the
laws or regulations are applicable to the
designated pollutant(s) for which the
plan is submitted.
(c) The plan shall show that the legal
authorities specified in this section are
available to the State at the time of sub-
mission of the plan. Legal authority ade-
quate to meet the requirements of para-
graphs (a) (3) and (4) of this section
may be delegated to the State under sec-
tion 114 of the Act.
(d) A State governmental agency
other than the State air pollution con-
trol agency may be assigned responsibil-
ity for jarrying out a portion of a plan
if the plan demonstrates to the Admin-
istrator's satisfaction that the State gov-
ernmental agency has the legal authority
necessary to carry out that portion of the
plan.
(e) The State may authorize a local
agency to carry out a plan, or portion
thereof, within the local agency's juris-
diction if the plan demonstrates to the
Administrator's satisfaction that the
local agency has the legal authority nec-
essary to implement the plan or portion
thereof, and that the authorization does
not relieve the State of responsibility
under the Act for carrying out the plan
or portion thereof.
§ 60.27 Actions by the Administrator.
(a) The Administrator may, whenever
be determines necessary, extend the pe-
riod for submission of any plan or plan
revision or portion thereof.
(b) After receipt of a plan or plan re-
vision, the Administrator will propose the
plan or revision for approval or dis-
approval. The Administrator will, within
four months after the date required for
submission of a plan or plan revision,
approve or disapprove such plan or revi-
sion or each portion thereof.
(c) The Administrator will, after con-
sideration of any State hearing record,
promptly prepare and publish proposed
regulations setting forth a plan, or por-
tion thereof, for a State if:
(1) The State fails to submit a plan
within the time prescribed;
(2) The State fails to submit a plan
revision required by § 60.23(a> (2) within
the time prescribed; or
(3) The Administrator disapproves the
State plan or plan revision or any por-
tion thereof, as unsatisfactory because
the requirements of this subpart have not
been met.
(d) The Administrator will, within six
months after the date required for sub-
mission of a plan or plan revision,
promulgate the regulations proposed un-
der paragraph (c) of this section with
such modifications as may be appropriate
unless, prior to such promulgation, the
State has adopted and submitted a plan
or plan revision which the Administra-
tor determines to be approvable.
(e) (1) Except as provided in para-
graph (e) (2) of this section, regulations
proposed and promulgated by the Admin-
istrator under this section will prescribe
emission standards of the same strin-
gency as the corresponding emission
guideline(s) specified in the final guide-
line document published under § 60.22(a^
and will require final compliance with
such standards as expeditiously as prac-
ticable but no later than the times speci-
fied in the guideline document.
(2) Upon application by the owner or
operator of a designated facility to which
regulations proposed and promulgated
under this section will apply, the Ad-
ministrator may provide for the appli-
cation of less stringent emission stand-
ards or longer compliance schedules than
those otherwise required by this section
in accordance with the criteria specified
in§60.24(f).
(f) If a State failed to hold a public
hearing.as required by § 60.23(c), the
Administrator will provide opportunity
for a hearing within the State prior to
promulgation of a plan under paragraph
(d) of this section.
g 60.28 Plan revisions by the State.
(a) Plan revisions which have the
effect of delaying compliance with ap-
plicable emission standards or incre-
ments of progress or of establishing less
stringent emission standards shall be
submitted to the Administrator within
60 days after adoption in accordance with
the procedures and requirements appli-
cable to development and submission of
the original plan.
(b) More stringent emission standards,
or orders which have the effect of ac-
celerating compliance, may be submitted
to the Administrator as plan revisions
in accordance with the procedures and
requirements applicable to development
and submission of the original plan.
(c) A revision of a plan, or any portion
thereof, shall not be considered part of
an applicable plan until approved by the
Administrator in accordance with this
subpart.
§ 60.29 Plan revisions by the Adminis-
trator.
After notice and opportunity for pub-
lic hearing in each affected State, the
Administrator may revise any provision
of an applicable plan if:
(a) The provision was promulgated by
the Administrator, and
(b) The plan, as revised, will be con-
sistent with the Act and with the require-
ments of this subpart.
111-17
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Subpart C—Emission Guidelines and
Compliance Times73
§ 60.30 Scope.
This subpart contains emission guide-
lines and compliance times for the con-
trol of certain designated pollutants from
certain designated facilities in accord-
ance with section lll(d) of the Act and
Subpart B.
§ 60.31 Definitions.
Terms used but not defined in this
subpart have the meaning given them
in the Act and in Subparts A and B of
this part.
§ 60.32 Designated facilities.
(a) Sulfuric acid production units.
The designated facility to which |{ 60.33
(a) and 60.34(a) apply is each existing
"sulfuric acid production unit" as de-
fined in { 60.81 (a) of Subpart H.
§ 60.33 Emission guidelines.
(a) Sulfuric acid production units.
The emission guideline for designated
facilities is 0.25 gram sulfuric acid mist
(as measured by Reference Method 8, of
Appendix A) per kilogram of sulfuric
acid produced (0.5 Ib/ton), the produt-
tton being expressed as 100 percent
HJSO.
S 60.34 Compliance times.
(a) Sulfuric acid production units.
Planning, awarding of contracts, and
Installation of equipment capable of
attaining the level of the emission guide-
line established under { 60.33 (a) can be
accomplished within 17 months after the
effective date of a State emission stand-
ard for sulfuric acid mist.
111-18
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©—:
OlnXSO fef P©OS50=I
Do
98,110
Aftteir
IF,
§ 60.40 Applicability end designation of
effected facility.8'49-64'94
(a) The affected facilities to which
the provisions of this subpart apply
are:
(1) Each fossil-fuel-fired steam gen-
erating unit of more than 73
megawatts heat input rate (250 million
Btu per hour).
(2) Each fossil-fuel and wood-resi-
due-fired steam generating unit capa-
ble of firing fossil fuel at a heat input
rate of more than 73 megawatts (250
million Btu per hour).
(b) Any change to an existing fossil-
fuel-fired steam generating unit to ac-
commodate the use of combustible ma-
terials, other than fossil fuels as de-
fined in this subpart, shall not bring
that unit under the applicability of
this subpart.
(c) Except as provided in paragraph
(d) of this section, any facility under
paragraph (a) of this section that com-
menced construction or modification
after August 17, 1971, is subject to the
requirements of this subpart.84
(d) The requirements of
§§ 60.44(a)(4), (a)(5), (b) and (d), and
80.45(f)(4)(vi) are applicable to lignite-
fired steam generating units that com-
menced construction or modification
after December 22,1976.84
(e) Any facility covered under Sub-
part Da is not covered under this Sub-
part.98
§ 60.41 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act, and in Subpart
A of this part.
(a) "Fossil-fuel fired steam generat-
ing unit" means a furnace or boiler
used in the process of burning fossil
fuel for the purpose of producing
steam by heat transfer.
(b) "Fossil fuel" means natural gas,
petroleum, coal, and any form of solid.
liquid, or gaseous fuel derived from
such materials for the purpose of cre-
ating useful heat.
(c) "Coal refuse" means waste-prod-
ucts of coal mining, cleaning, and coal
preparation operations (e.g. culm, gob,
etc.) containing coal, matrix material,
clay, and,other organic and inorganic
material."
11
(d) "Fossil fuel and wood residue-
fired steam generating unit" means a
furnace or boiler used in the process
of burning fossil fuel and wood residue
for the purpose of producing steam by
heat transfer.49
(e) "Wood residue" means bark, saw-
dust, slabs, chips, shavings, mill trim,
and other wood products derived from
wood processing and forest' manage-
ment operations.49
(f) "Coal" means all solid fuels clas-
sified as anthracite, bituminous, subbi-
tuminous, or lignite by the American
Society for Testing Material. Designa-
tion D 38S-86.84
§ 60.42 Standard for particulate matter.3
(a) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere from
any affected facility any gases \vhich:
(1) Contain particulate matter in
excess of 43 nanograms per joule heat
input (0.10 Ib per million Btu) derived
from fossil fuel or fossil fuel and wood
residue.49
(2) Exhibit greater than 20 percent
opacity except for one six-minute
period per hour of not more than 27
percent opacity.18'76
(b)(l) On and after (the date of
publication of this amendment), no
owner or operator shall cause to be
discharged into the atmosphere from the
Southwestern Public Service Company's
Harrington Station Unit #1, in Amarillo,
Texas, any gases which exhibit greater
than 35% opacity, except that a
maximum of 42% opacity shall be
permitted for not more than 6 minutes in
any hour.107
(2) Interstate Power Company shall
not cause to be discharged into the
atmosphere from its Lansing Station
Unit No. 4 in Lansing, Iowa, any gases
which exhibit greater than 32% opacity,
except that a maximum of 39% opacity
shall be permitted for not more than six
minutes in any hour."2'"5
(3) Omaha Public Power District shall
not cause to be discharged into the
atmosphere from its Nebraska City
Power Station in Nebraska City.
Nebraska, any gases which exhibit
greater than 30% opacity, except that a
maximum of 37% opacity shall be
permitted for not more than six minutes
in any hour.133
§ 60.43 Standard for sulfur dioxide.2-8
(a) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere from
any affected facility any gases which
contain sulfur dioxide in excess of:
(1) 340 nanograms per joule heat
input (0.80 Ib per million Btu) derived •
from liquid fossil fuel or liquid fossil
fuel and wood residue.49
(2) 520 nanograms per joule heat
input (1.2 Ib per million Btu) derived
from solid fossil fuel or solid fossil fuel
and wood residue.49
(b) When different fossil fuels are
burned simultaneously in any combi-
nation, the applicable standard (in ng/
J) shall be determined by proration
using the following formula:
PS,., = ly (340) + z (520)]/!/ + 2
where:
PS*,, is the prorated standard for sulfur
dioxide when burning different fuels si-
multaneously. in nanograms per joule
heat input derived from all fossil fuels
fired or from all fossil fuels and wood
residue fired,
y is the percentage of total heat input de-
rived from liquid fossil fuel, and
z is the percentage of total heat input de-
rived from solid fossil fuel.49
(c) Compliance shall be based on the
total heat input from all fossil fuels
burned, including gaseous fuels.
§ 60.44 Standard for nitrogen oxides.3
(a) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere from
any affected facility any gases which
contain nitrogen oxides, expressed as
NO, in excess of:
(1) 86 nanograms per joule heat
input (0.20 Ib per million Btu) derived
from gaseous fossil fuel or gaseous
fossil fuel and wood residue.49
(2) 130 nanograms per joule heat
input (0.30 Ib per million Btu) derived
from liquid fossil fuel or liquid fossil
fuel and wood residue.49
(3) 300 nanograms per joule heat
input (0.70 Ib per million Btu) derived
from solid fossil fuel or solid fossil fuel
and wood residue (except lignite or a
solid fossil fuel containing 25 percent.
by weight, or more of coal refuse). '-49
(4) 260 nanograms per joule heat
input (0.60 Ib per million Btu) derived
from lignite or lignite and wood resi-
due (except as provided under para-
graph (a)(5) of this section).84
(5) 340 nanograms per joule heat
input (0.80 Ib per million Btu) derived
from lignite which is mined in North
Dakota, South Dakota, or Montana
and which is burned in a cyclone-fired
unit.84
(b) Except as provided under para-
graphs (c) and (d) of this section,
when different fossil fuels are burned
simultaneously in any combination,
the applicable standard (in ng/J) is de-
termined by proration using the fol-
lowing formula:
w+x+y+z
111-19
-------
where:
PSHo* = is the prorated standard for nitro-
gen oxides when burning different
fuels simultaneously, in nanograms
per joule heat input derived from all
fossil fuels fired or from all fossil fuels
and wood residue fired;
u> = is the percentage of total heat input
derived from lignite;
x=is the percentage of total heat input
derived from gaseous fossil fuel;
t/=is the percentage of total heat input
derived from liquid fossil fuel; and
z=is the percentage of total heat input de-
rived from solid fossil fuel (except lig-
nite). 11/9,84
(c) When a fossil fuel containing at
least 25 percent, by weight, of coal
refuse is burned in combination with
gaseous, liquid, or other solid fossil
fuel or wood residue, the standard for
nitrogen oxides does not apply.34
(d) Cyclone-fired units which burn
fuels containing at least 25 percent of
lignite that is mined in North Dakota,
South Dakota, or Montana remain
subject to paragraph (a)(5) of this sec-
tion regardless of the types of fuel
combusted in combination with that
lignite.84
§ 60.45 Emission and fuel monitoring1.
1,18
(a) Each owner or operator shall in-
stall, calibrate, maintain, and operate
continuous monitoring systems for
measuring the opacity of emissions,
sulfur dioxide emissions, nitrogen
oxides emissions, and either oxygen or
carbon dioxide except as provided in
paragraph (b) of this section.57
(b) Certain of the continuous moni-
toring system requirements under
paragraph (a) of this section do not
apply to owners or operators under
the following conditions:57
(1) For a fossil fuel-fired steam gen-
erator that burns only gaseous fossil
fuel, continuous monitoring systems
for measuring the opacity of emissions
and sulfur dioxide emissions are not
required.57
(2) For a fossil fuel-fired steam gen-
erator that does not use a flue gas de-
sulfurization device, a continuous
monitoring system for measuring
sulfur dioxide emissions is not re-
quired if the owner or operator moni-
tors sulfur dioxide emissions by fuel
sampling and analysis under para-
graph (d) of this section.57
(3) Notwithstanding § 60.13(b), in-
stallation of a continuous monitoring
system for nitrogen oxides may be de-
layed until after the initial perform-
ance tests under § 60.8 have been con-
ducted. If the owner or operator dem-
onstrates during the performance test
that emissions of nitrogen oxides are
less than 70 percent of the applicable
standards in § 60.44, a continuous mon-
itoring system for measuring nitrogen
oxides emissions is not required. If the
initial performance test results show
that nitrogen oxide emissions are
greater than 70 percent of the applica-
ble standard, the owner or operator
shall install a continuous monitoring
system for nitrogen oxides within one
year after the date of the initial per-
formance tests under § 60.8 and
comply with all other applicable moni-
toring requirements under this part.57
(4) If an owner or operator does not
install any continuous monitoring sys-
tems for sulfur oxides and nitrogen
oxides, as provided under paragraphs
cbXl) and (b)(3) or paragraphs (b)(2>
and (b)(3) of this section a continuous
monitoring system for measuring
either oxygen or carbon dioxide is not
required.57
(c) For performance evaluations
under I 60.13(c) and calibration checks
under §60.13(d), the following proce-
dures shall be used:57
(1) Reference Methods 6 or 7, as ap-
plicable, shall be used for conducting
performance evaluations of sulfur
dioxide and nitrogen oxides continu-
ous monitoring systems.57
(2) Sulfur dioxide or nitric oxide, as
applicable, shall be used for preparing
calibration gas mixtures under Per-
formance Specification 2 of Appendix
B to this part.57
(3) For affected facilities burning
fossil fuel(s), the span value for a con-
tinuous monitoring system measuring
the opacity of emissions shall be 80,
90, or 100 percent and for a continuous
monitoring system measuring sulfur
oxides or nitrogen oxides the span
value shall be determined as follows:
[In parts per million]
Fossil fuel Span value for Span value for
sulfur dioxide nitrogen oxides
Gas (')
Liquid 1,000
Solid 1 500
Combinations 1.000y-t 1,5007 500(x
500
500
500
'Not applicable.
where:
x = the fraction of total heat input derived
from gaseous fossil fuel, and
y = the fraction of total heat input derived
from liquid fossil fuel, and
z=the fraction of total heat input derived
from solid fossil fuel. 57
(4) All span values computed under
paragraph (c)(3) of this section for
burning combinations of fossil fuels
shall be rounded to the nearest 500
ppm.
(5) For a fossil fuel-fired steam gen-
erator that simultaneously burns fossil
fuel and nonfossil fuel, the span value
of all continuous monitoring systems
shall be subject to the Administrator's
approval.57
(d) [Reserved]
(e) For any continuous monitoring
system installed under paragraph (a)
ol this section, the lonowmg conver-
sion procedures shall be used to con-
vert the continuous monitoring data
i 57
into units of the applicable standards
(ng/J, Ib/million Btu):49-57
(1) When a continuous monitoring
system for measuring oxygen is select-J
ed, the measurement of the pollutant
concentration and oxygen concentra-
tion shall each be on a consistent basis
(wet or dry). Alternative procedures
approved by the Administrator shall
be used when measurements are on a
wet basis. When measurements are on
a dry basis, the following conversion
procedure shall be used:
E-rr f 20-9 1
i_20.9-percent Q8J
where:
E, C, P, and %O, are determined under
paragraph (f) of this section.57
(2) When a continuous monitoring
system for measuring carbon dioxide is
selected, the measurement of the pol-
lutant concentration and carbon diox-
ide concentration shall each be on a
consistent basis (wet or dry) and the
following conversion procedure shall
be used:
E-CF f 10° 1
c-c'< [percent COJ
where:
E, C, Pc and %CO, are determined under
paragraph (f) of this section.57
(f) The values used in the equations
under paragraphs (e) (1) and (2) of
this section are derived as follows:
(1) E=pollutant emissions, ng/J (lb/
million Btu).
(2) C= pollutant concentration, ng/
dscm (Ib/dscf), determined by multi-
plying the average concentration
(ppm) for each one-hour period by
4.15xl04 M ng/dscm per ppm
(2.59x10-' M Ib/dscf per ppm) where
M= pollutant molecular weight, g/g-
mole (Ib/lb-mole). M= 64.07 for sulfur
dioxide and 46.01 for nitrogen oxides.49
(3) %O2, %COZ=oxygen or carbon
dioxide volume (expressed as percent),
determined with equipment specified
under paragraph (d) of this section.
(4) F, Fc=a factor representing a
ratio of the volume of dry flue gases
generated to the calorific value of the
fuel combusted (F), and a factor repre-
senting a ratio of the volume of
carbon dioxide generated to the calo-
rific value of the fuel combusted (Fc),
respectively. Values of F and Fc are
given as follows:
(i) For anthracite coal as classified
according to A.S.T.M. D 388-66, F=
2.723x10' ' dscm/J (10,140 dscf/mil-
lion Btu) and Fc=0.532xlO~ ' scm
CO,/J (1,980 scf COj/million Btu).49
(ii) For subbituminous and bitumi-
nous coal as classified according to
A.S.T.M. D 388-66, F= 2.637x10-'
dscm/J (9,820 dscf/million Btu) and
^C=0.486xl0-7 scm CO,/J (1,810 scf
CCVmillion Btu).49
(iii) For liquid fossil fuels including i
crude, residual, and distillate oils,
F= 2.476x10-' dscm/J (9,220 dscf/mil-
111-20
-------
lion Btu) and Fc = 0.384 x 10'' scm CO,/
J (1,430 scf CO,/million Btu).49-67
(iv) For gaseous fossil fuels, F= 2.347
xlfl-' dscm/J (8,740 dscf/million Btu).
For natural gas, propane, and butane
fuels, Fc = 0.279x10-' scm CO,// (1,040
scf CO./million Btu) for natural gas,
0.322x10-' scm CO,// (1,200 scf CO,/
million Btu) for propane, and
0.338x10-' scm CO,/J (1,260 scf CO,/
million Btu) for butane.49,67
(v) For bark F=2.589xlO-' dscm/J
(8,640 dscf/million Btu) and Fc=0.500
xlO-' scm CO,/J (1,880 scf CO,/ mil-
lion Btu). For wood residue other than
bark F=2.492xlfl-' dscm/J (9,280
dscf/million Btu) and Fc=0.494xlO-'
scm CO,/J (1,840 scf CO,/ million
Btu).49-67
(vi) For lignite coal as classified ac-
cording to A.S.T.M. D 388-66,
F=2.659xlO-' dscm/J (9900 dscf/mil-
lion Btu) and Fc=0.518xlO-'scm CO,/
J (1920 scf CO,/million Btu). ^
(5) The owner or operator may use
the following equation to determine
an F factor (dscm/J or dscf/million
Btu) on a dry basis (if it is desired to
calculate F on a wet basis, consult the
Administrator) or Fc factor (scm CO,/
J, or scf COj/million Btu) on either
basis in lieu of the F or Fc factors spec-
ified in paragraph (f)(4) of this sec-
tion:49
(8) For effected facilities firing com-
binations of fossil fuels or fossil fuels
and wood residue, the F or F, factors
determined by paragraphs (f)(4) or
(f )(5) of this section shall be prorated
in accordance with the applicable for-
mula as follows:
F =
where:
Xi=the fraction of total heat Input de-
rived from each type of fuel (e.g. natu-
ral gas, bituminous coal, wood residue.
etc.)
Ft or (F,)i=the applicable F or F, factor
for each fuel type determined in ac-
cordance with paragraphs (f)(4) and
(f K5) of this section.
a=the number of fuels being burned in
combination.49
(g) For the purpose of reports re-
quired under B80.7(c), periods of
excess emissions that shall be reported
are defined as follows:
(1) Opacity. Excess emissions are de-
fined as any six-minute period during
which the average opacity of emissions
exceeds 20 percent opacity, except
that one six-minute average per hour
P =10-o'
_n[227.2 (pet. H)+95.5 (pet. Q + 35.6 (pc>. .S)+H.7 (pet. N) -28.7J_pct. O)l
GCV
(SI units)
10s[3.64(%/0-H.53(%C)+0.57(%S)+0.1
-------
consist of at least four grab sampk.-,
taken at approximately 15-minute in-
tervals. The arithmetic mean of the
samples shall constitute the run value.
(f) For each run using the methods
specified by paragraphs (a)(3), (a)(4).
and (a)(5) of this section, the emis-
sions expressed in ng/J (Ib/million
Btu) shall be determined by the fol-
lowing procedure:
£=Cf(20.9/20.9-percent O2>
where:
(1) E = pollutant emission ng/J (lb/
million Btu).
(2) C = pollutant concentration, ng/
dscm (Ib/dscf), determined by method
5, 6, or 7.
(3) Percent O,=oxygen content by
volume (expressed as percent), dry
basis. Percent oxygen shall be deter-
mined by using the integrated or grab
sampling and analysis procedures of
Method 3 as applicable.
The sample shall be obtained as fol-
lows:
(1) For determination of sulfur diox-
ide and nitrogen oxides emissions, the
oxygen sample shall be obtained si-
multaneously at the same point in the
duct as used to obtain the samples for
Methods 6 and 7 determinations, re-
spectively [§ 60.46(c)]. For Method 7.
the oxygen sample shall be obtained
using the grab sampling and analysis
procedures of Method 3.
(ii) For determination of particulate
emissions, the oxygen sample shall be
obtained simultaneously by traversing
the duct at the same sampling location
used for each run of Method 5 under
paragraph (b) of this section. Method
1 shall be used for selection of the
number of traverse points except that
no more than 12 sample points are re-
quired.
(4) F=a factor as determined in
paragraphs (f) <4), (5) or (6) of § 60.45.
(g) When combinations of fossil
fuels or fossil fuel and wood residue
are fired, the heat input, expressed in
watts (Btu/hr), is determined during
each testing period by multiplying the
gross, calorific value of each fuel fired
(in J/kg or Btu/lb) by the rate of each
fuel burned (in kg/sec or Ib/hr). Gross
calorific values are determined in ac-
< ordance with A.S.T.M. methods D
2015-66(72) (solid fuels), D 240-64(73)
(liquid fuels), or D 1826-64(7) (gaseous
fuels) as applicable. The method used
to determine calorific value of wood
residue must be approved by the Ad-
ministrator. The owner or operator
shall determine the rate of fuels
burned during each testing period by
suitable methods and shall confirm
the rate by a material balance over the
steam generation system.49
Sec. 114. Clean All Act
J.SC. 7414)). 68-83
ti amended <4'<
§ 60.47 Innovative technology waiver*
waiver of sulfur dioxide standards of
performance for new stationary sources
for Homer City Unit No. 3 under section
1110) of the Clean Air Act for Multi-Steam
Coal Cleaning System.132
(a) Pursuant to section lll(j) of the
Clean Air Act, 42 U.S.C. 7411(j).
commencing on November 13,1981
Pennsylvania Electric Company and
New York State Electric & Gas
Corporation shall comply with the
following terms and conditions for
electric generating Units Nos. 1. 2, and 3
at the Homer City Steam Electric
Generating Station, Center Township,
Indiana County, Pennsylvania.
(b) The foregoing terms and
conditions shall remain effective
through November 30,1981, and
pursuant to section lll(j)(B), shall be
Federally promulgated standards of
performance. As such, it shall be
unlawful for Pennsylvania Electric
Company and New York State Electric &
Gas Corporation to operate Units Nos. 1,
2, and 3 in violation of the standards of
performance established in this waiver.
Violations of the terms and conditions
of this waiver shall subject
Pennsylvania Electric Company and
New York State Electric & Gas
Corporation to Federal enforcement
under sections 113 (b) and (c). 42 U.S.C.
7413 (b) and (c), and 120.42 U.S.C. 7420,
of the Act as well as possible citizen
enforcement under section 304 of the
Act, 42 U.S.C. 7604. Pursuant to section
lll(c)(l) of the Act. 42 U.S.C. 7411(c)(l).
at 45 FR 3109, January 16,1980, the
Administrator delegated to the
Commonwealth of Pennsylvania
authority to implement and enforce the
Federal Standards of Performance for
New Stationary Sources of 1.2 lb SO,/
10s Btu applicable to Homer City Unit
No. 3. The SO* emission limitations
specified in this waiver for Unit No. 3
are new Federally promulgated
Standards of Performance for New
Stationary Sources for a limited time
period. Thus, during the period this
waiver is effective, the delegated
authority of the Commonwealth of
Pennsylvania to enforce the Federal
Standards of Performance for New
Stationary Sources of 1.2 lb SO,/106 Btu
applicable to Homer City Unit No. 3 is
superseded and enforcement of the
terms and conditions of this waiver shall
be the responsibility of the
Administrator of EPA. The
Commonwealth of Pennsylvania may,
and is encouraged to. seek delegation of
authority, pursuant to section lll(c)(l).
to enforce the temporary Federal
Standards of Performance for New
Stationary Sources specified in this
waiver. Should such authority be
delegated to the State, the terms and
conditions of this waiver shall be
enforceable by the Administrator of
EPA and the Commonwealth of
Pennsylvania, concurrently. Nothing in
this waiver shall affect the rights of the
Commonwealth of Pennsylvania under
the Decree filed in the Pennsylvania
Commonwealth Court on January 28.
1981, at Docket No. 161 C.D. 1981.
(c) On December 1,1981, and
continuing thereafter, at no time shall
emissions of SO* from Unit No. 3 exceed
1.2 lb/10" Btu of heat input, as specified
in 40 CFR 60.43(a}(2) (July 1.1979).
(d) On January 15,1982, Pennsylvania
Electric Company and New York State
Electric & Gas Corporation shall
demonstrate compliance at Homer City
Unit No. 3 with 40 CFR 60.43(a)(2) {July
1,1979) in accordance with the test
methods and procedures set forth in 40
CFR 60.8 (b). (c), (d), (e) and (f) (July 1.
1979).
(e) Emission limitations. (1)
Commencing on November 13,1981 and
continuing until November 30,1981:
(i) At no time shall emissions of SO*
from Units Nos. 1,2, and 3, combined,1
exceed: 2.87 lb SO./106 Btu of heat input
in a rolling 30-day period (starting with
the 60th day after the effective date of
the waiver); 3.6 lb SO,/108 Btu of heat
input in any day;1 and 3.1 lb SO,/10S Btu
of heat input on more than 4 days in any
rolling 30-day period.
(ii) At no time shall emissions of SO>
from Units Nos. 1, 2, and 3, combined.2
exceed 695 tons in any day.
(iii) At no time shall emissions of SO*
from Units Nos. 1, 2, and 3, combined,1
exceed 91 tons in any discrete ' 3-hour
period.
(iv) At no time shall emissions of SOi
from Units Nos. 1 and 2, combined,
exceed 463 tons in any day.
(v) At no time shall emissions of SO,
from Units Nos. 1 and 2, combined,
exceed 61 tons in any discrete ' 3-hour
period.
(f) Installation Schedule. (1)
Pennsylvania Electric and New York
State Electric & Gas have selected
engineering designs for necessary
modifications to the Multi-Stream Coal
Cleaning System (MCCS) 93B Circuit.
(2) Pennsylvania Electric and New
York State Electric & Gas have placed
1A "day" (a 24-hour period) and a "discrete 3-
hour period" Is defined in section (g)(7)(iv).
'The procedures used for calculating combined
SO, emissions are given in paragraph (g)(5) of this
section.
111-22
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purchase orders for all major equipment
necessary to complete necessary
modifications to the MCCS S3B circuit.
(3) Pennsylvania Electric and New
York State Electric & Gas have
completed design engineering of (he
modifications tCLthe MCCS 93B circuit.
(4) Oh or before September IS, 1981.
Pennsylvania Ejgctric and New York
State Electric & Gas shall complete
construction of ihe MCCS 93B circuit.
(5) On or before October 15,1981,
Pennsylvania Electric and New York
State Electric & Gas shall start-up the
MCCS 93B circuit.
(g) Monitoring and Reporting.
Throughout the waiver period the
Company shall acquire sufficient
quantities of emission monitoring and
fuel analysis data to continuously
demonstrate compliance with the
combined emission limitations. The
Company shall acquire heat input and
emission data (sufficient to demonstrate
compliance) from each boiler during all
operating periods (i.e., whenever fuel is
being fired), including periods of process
start-up, shutdown, and malfunction.
This requirement shall be met through
the use of continuous emission
monitoring systems (CEMS) [or as
supplemented by continuous bubbler
(CB) systems], heating value as
determined by as-fired fuel analysis.
and coal mass feed-rate measurements.
(1) Continuous Emission Monitoring
System (CEMS): Primary Compliance
Monitoring Method:
(i) The Company shall install, test,
operate, and maintain all CEMS as the
primary compliance monitoring method
in such a manner as to result in the
acquisition of validated data which are
representative of each boiler's 3-hour,
24-hour, and 30-day emission rates. (See
paragraph (g)(7) of this section.)
(ii) The validity of the emission data
obtained with CEMS shall be
determined initially by conducting a
performance specification test (PST).
Subsequent CEMS data validations shall
be performed in accordance with
paragraphs (g)(6) and (g)(7) of this
section. All PSTs of CEMS shall include
at least: (A) All of the specifications and
test procedures contained in the January
26,1981 proposed Performance
Specifications 2 and 3 (Ref. 1). 46 FR
8352; and (B) the calibration error and
response time specifications and test
procedures contained in the October 10.
1979 proposed Performance
Specifications 2 and 3 (Ref. 2), 44 FR
58602. The calibration error, response
time, and all drift tests shall be
conducted using calibration gases which
conform to the requirements of
paragraph (g)(6)(iii) of this section.
(2) Continuous Bubbler Syotena (CB):
Secondary Compliance Teot Method:
(i) The Company shall use the CB
system ao & secondary compliance
monitoring method to supplement CEMS
data whenever a CEMS io out of service
or is otherwise providing data of
insufficient quality or quantity. The CB
technique shall also be used to
periodically assess the validity of CEMS
data (See paragraph (g)(6)(i)(C) of this
section).
(ii) The CB technique for
quantitatively assessing SOo emissions
(in Ib/10° Btu) is delineated in Appendix
I of this waiver. This technique 8s based
upon combining the basic wet-chemical
technique of EPA's Reference Method 6
at 40 CFR Part 60, Appendix I. July 1.
1979, (for determining SOa
concentrations) with the gravimetric
method (absorption of COo onto
ascarite) for determining COa
concentrations. Using reduced How
rates and increased reagent volumes
and concentrations, the CB system may
be run for much longer periods of time
than Reference Method 6 at 40 CFR Part
60, Appendix I (July 1.1879). The
Company may make the following
modifications to the CB method as long
as they periodically demonstrate that
their modified CB method meets the
performance criteria of paragraph
(g)(6)(ii) of this section:
(A) Use a heated sample probe
(B) Use an in-stack filter (up stream of
the impingers) to remove particulate
matter
(C) Eliminate the isopropanol (initial)
impingers
(D) Use a diaphragm pump with flow
regulators in place of the peristaltic
pump
(iii) The Company shall initially
demonstrate its proficiency in acquiring
SOj/COa data with the CB method by
comparing the results obtained using the
CB method with those obtained using
Reference Methods 3 and 6 (See Ref. 3
and paragraph (g)(6)(ii)(B) of this
section). The CB data shall be deemed
initially acceptable if the results of this
test are within the Limits prescribed in
paragraph (gX9)(") (A) and (B) of this
section. Subsequently, the CB data shall
be periodically ^validated as per the
QA requirements of paragraph (g)(6)(ii)
(A) and (B) of this section.
(3) Requirements for Obtaining 3-hour
and 24-hour Emission Data from
Individual Boilers: Using the methods
set forth in this waiver, the Company
shall obtain the following quantities of
3-hour and 24-hour emission data.
Failure to acquire the specified quantity
or quality of data shall constitute a
violation of the terms and conditions of
this waiver.
(i) Data end calculation requirements
for continuous emission monitoring
system (CEMS). During normal
operation of a CEMS (primary
compliance method) to obtain emission
data from one or more of Units Nos. 1,2.
and 3, the Company shaU obtain the
following data from each CEMS:
(A) 3-hour discrete averaging times
using CEMS.—For each boiler,
continuously measure and calculate
eight discrete 3-hour averages each day,
using the three consecutive (exclusive of
exemptions below) 1-hour emission
averages (each consisting of four equally
spaced data points per 1-hour period).
The only periods when CEMS
measurements are exempted are periods
of routine maintenance (as specified in
the Lear Siegler Operator's Manual) and
as required for daily zero/span checks
and calibrations. Such exemptions
notwithstanding, at no time shall less
than six discrete 3-hour averages per
day be obtained. Note that in
calculations each 3-hour average one
only uses the data available from that
specific discrete average.
(B) 24-hour averaging times using
CEMS. For each boiler, continuously
measure and calculate one discrete 24-
hour average per day, using the
available (18-24) 1-hour emission
averages obtained during that specific
day. The only periods when CEMS
measurements are exempted are periods
of routine maintenance (as specified in
the Lear Siegler Operator's Manual) and
as required for daily zero/span checks
and calibrations. Such exemptions
notwithstanding, and except for the
instances when a boiler operated for
only part of the day, at no time shall a
calculated 24-hour average consist of
less than a total of eighteen 1-hour
averages.
(ii) Data requirements when switching
from CEMS to CB system. If it becomes
necessary to take a CEMS out of service
(because of CEMS inoperability or
failure to meet the performance
requirements (paragraph (g)(6)(i) of the
section), the Company shall immediately
initiate the activities necessary to begin
sampling with the secondary (CB)
compliance test method. However, EPA
recognizes that some reasonable amount
of time will be necessary to diagnose a
CEMS problem, to determine whether
minor maintenance will be sufficient to
resolve the problem, or to determine if
the monitoring system must be taken out
of service. Additionally, CEMS
downtime could occur during the night
time shifts or other times when
immediate corrective action cannot
reasonably be made. Therefore, the
waiver requires that at no time shall
111-23
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•more than six hours elapse between
acceptable operation of the CEMS and
the start of CB sampling. All data which
are obtained during any interrupted
averaging period(s) shall be used to
calculate the reported average(s), and
the Company shall clearly indicate this
data "shortfall" (e.g., acquisition of only
2 hours of data for a 3-hour averaging
period) in the subsequent report (See
paragraph (g)(8) of this section).
(A) 3-hour averaging times during
CEMS-to-CB transition.—During any
day in which a transition (from the
CEMS) to the secondary compliance
method is made, at least four (4) 3-hour
average rates of the affected boiler's
emissions shall be obtained.
Note.—At least six (6) 3-hour emission
averages are required when a planned CB-to-
CEMS transition is performed.
(B) 24-hour averaging times that
include a CEMS-to-CB transition. During
any day in which a transition (from the
CEMS) to the secondary compliance
method is made, a 24-hour average rate
of the affected boiler's emissions shall
be obtained, using the combination of all
available 1-hour CEMS emission
averages and 3-hour CB emission
averages. Such a calculation shall
weight (e.g., one CB average is
equivalent to three 1-hour CEMS
average values) the CB data
appropriately.
(iii) Data and calculation requirements
for continuous bubbler (CB) monitoring
systems. During all periods when a
CEMS is out of service and a CB system
is in use at one or more of Units Nos. 1,
2, or 3, the Company shall obtain the
following data from each CB:
(A) 3-hour averaging times using CB
systems. For each boiler being
monitored by a CB system, measure and
calculate at least six discrete 3-hour
emission rates each day.
(B) 24-hour averaging times using CB
systems. For each boiler being
monitored by the CB method, calculate
one 24-hour average emission rate each
day. Each average shall be based upon a
continuous 24-hour sample.
(4) Requirements for Measuring and
Calculating Heat Input Rates:
(i) The Company shall determine the
coal feed rate, for each boiler that is
being fired, for each 24-hour period in
accordance with the Company's
standard procedures for weighing coal
being fed to the boilers.
(ii) The Company shall determine the
heat content (gross calorific value) of
the coal, for each boiler being fired and
for each 24-hour period, in accordance
with the Company's established
procedures for as-fired, 24-hour fuel
sampling (15-minute sample intervals)
and composite automated analysis.
(iii) The Company shall calculate the
average heat input rate for each boiler
for each 24-hour period (10* Btu/24-
hours). For each boiler, multiply the
average heat content of the coal (Btu/lb)
by the coal feed rate as determined for
the same 24-hour averaging period.
(iv) The Company shall estimate the
average 3-hour heat input rate (106Btu/
3-hours) for each boiler from the
previously determined 24-hour values.
To estimate a 3-hour heat input rate
multiply the corresponding 24-hour
value (106Bru/24-hours) by the ratio of
the respective 3-hour to the 24-hour
megawatt outputs.
(5) Requirements for Calculating
Combined SOi Emissions:
(i) 3-hour averaging period: The
combined emission rates from the
operating boilers are equal to the sum of
the products of the individual heat input
rates (10s Btu/3-hours) and the SO»
emission rates (lb/10'Btu as determined
for the 3-hour period). This quantity,
when divided by 2000 Ib/ton, equals the
combined tons of 3-hour SOa emissions
(see Equation 1).
determined for the 24-hour period)
divided by the sum of the combined heat
inputs (see Equation 2).
Equation 2
—V"*
2-
Equation 1
Where:
Mj=combined (e.g., Units Nos. 1 and 2 or
Units Nos. 1, 2, and 3) emission rates for
the operating units in tons SO., for the jth
averaging period (3-hour or 24-hour).
ED=average emission rates from the "ith"
unit in Ib SO* for the jth average period
where )=3-hour or 24-hour.
HU=average heat input rates for the "ith"
unit in 10'Btu per "jth" averaging period
where j=3-hour or 24-hour.
n=number of operating units.
Note.—Equation 1 is to be used for
calculating: (1) combined tons of SO,
emissions from Units Nos. 1 and 2 and (2)
combined tons of SO. emissions from Units
Nos. 1, 2, and 3. Equation 1 is applicable to
both 3-hour and 24-hour averaging periods.
Furthermore, if a unit is not combusting fuel,
"HD" will be zero.
(ii) 24-hour aver
(A) The combined emissions from the
operating boilers is equal to the sum of
the products of the individual heat
inputs (108 Btu/24-hour) and the SOt
emissions (lb/10*Btu as determined for
the 24-hour period). This quantity, when
divided by 2000 Ib/ton, equals the
combined tons of 24-hour SOt emissions
(see Equation 1).
(B) The combined emissions from the
operating boilers, in the units lb/10'Btu,
is equal to the sum of the products of the
individual heat inputs (10s Btu/24-hour)
and the SO« emissions (lb/108 Btu as
H,
Where:
E=combined emission rates for the operating
units in Ib SO,/106Btu, for the 24-hour
averaging period.
E|=24-hour average emission rates from the
"ith" unit in Ib SO,/108Btu.
H(=24-hour average heat input rates for the
"ith" unit in 10« Btu/24-hour.
n=number of operating units.
Note.—If a unit is not combusting fuel, "H,"
will be zero.
(iii) 30-day rolling average: Once
every day, calculate combined 30-
calendar day emission average rates
(beginning 60 days after the effective
date of this waiver), using all available
combined 24-hour emission rate
averages [paragraph (g)(5)(ii)(B) of this
section], for the most recent 30
consecutive calendar days. To make the
two calculations for the combined (Units
Nos. 1,2, and 3; Units Nos. 1 and 2)
emission rates, add the 30 consecutive
daily combined average emission rates
(Ib SOi/lO'Btu) and divide the sum by
30 days.
(6) Quality Assurance (QA)
Requirements: The Company shall
validate the required emission data by
performing at least the quality
assurance procedures specified herein.
These QA requirements are considered
the minimum necessary to ensure that
the sampling methods employed
produce valid data. The performance
criteria that are established in this
section and that are restated in Table 1
are considered both necessary and
reasonably achievable. If, for any
reason, a CEMS system fails to achieve
the required specifications, the CEMS
shall be immediately taken out of
service and sampling with a CB system
shall be initiated. If, for any reason, a
CB (which is being used while a CEMS
is out of service) fails to meet the
required specifications, the Company
shall notify the Director of the Division
of Stationary Source Enforcement
(Washington, D.C.) within 72 hours, as
per paragraph (g)(8)(iv) of this section.
The Company is encouraged to
supplement these procedures to improve
the quality of the emission data
obtained.
(i) QA requirements, calculation
procedures, and specification limits for
CEMS: At a minimum, the Company
shall conduct the following initial, daily,
weekly, and quarterly QA evaluations of
111-24
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each boiler's OEMS data. Where including those for relative accuracy, of
designated, the response time and the January 26,1981 proposed
calibration error test procedures Performance Specifications 2 and 3 (Ref.
contained in Reference 2 and the 1) shall be used.
remaining performance test procedures,
(A) Daily zero and calibration checks of the GEMS. Conduct the following zero
and calibration drift checks of each GEMS at approximately 24-hour intervals, and
use the equations provided here to determine if the CEMS meets the designated
drift specifications. All monitors that have exhibited drift during the previous 24-
hour period must be adjusted immediately after the drift checks have been per-
formed and the results have been recorded.
(1) 24-hour zero drift of the SO, monitor (this test is to be performed using low
range (2-5%) span gas):
Specification limits: 8.0% of span in any 24-hour period; 2.0% of span for any three
consecutive 24-hour periods.
24-hour SOj stern drift = !CEMS'~G'| xlOO Equation 3
; CEMS; |
where:
CEMS.=monitor zero value (ppm)
G,=zero gas value (ppm)
CEMS.=monitor span value (ppm)
(2) 24-hour zero drift of the O> monitor:
Specification limits: 2.0% Cs in any 24-hour period; 0.5% O, for any three consecutive 24-
hour periods.
24-hour Oi zero drift= | CEMS,-G,|xlOO Equation 4
where:
CEMS,=monitor zero value (%OJ)
G,=zero gas value (%O>)
(3) 24-hour calibration drift of the SO» monitor (this test is to be performed
using 85-95% span gas):
Specification limits: 10.0% of span in any one 24-hour period: 2.5% of span for any three
consecutive 24-hour periods.
24-hour SO, calibration drift =
CEMS.-GV
XlOO Equation 5
GEM.
where:
CEMS,=monitor reading (ppm)
G, = calibration gas value (ppm)
CEMS.=monitor span value (ppm)
(4) 24-hour calibration drift of the O» monitor
Specification limits: 2.0% O> in any one 24-hour period; 0.5% O, for any three consecutive
24-hour periods.
24-hour O« calibration drift= | CEMS,-GV| xlOO Equation 6
where:
CEMS,=monitor reading (%Oj)
G.=calbration gas value (%OS)
(B) Daily mid-range checks of the CEMS.—Conduct the following mid-range
calibration checks of each CEMS after performing the zero and calibration drift
checks. The purpose for requiring mid-range calibration checks is to verify CEMS
linearity between the zero and calibration values. The mid-range calibration
checks shall be conducted at approximately 24-hour intervals (or more frequently),
and the equations provided shall be used to determine if the CEMS meets the
designated specification limits:
111-25
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24-hour mid-range drift check of the SO, and the Oi monitors (this test is to be performed
using 45-55% span gas): Specification limits (same for SOt and O, monitors): 10% of
mid-range gas in any one 24-hour period and 5.0% of mid-range gas in any three
consecutive 24-hour periods.
SOi and Oj mid-range drift =
CEMS,
-1
X100 Equation 7
where:
CEMSr=monitor reading (ppm SO, or %O,)
Gv = mid-range gas value (ppm SO* or %OJ
(C) Initial and weekly checks of the GEMS.—Initially and once each week.
conduct at least one 24-hour modified relative accuracy teat of each GEMS (com-
bined SO? and O> channels in units of SO, lb/106 Btu) using the CB method. If the
difference between the GEMS and CB exceeds the designated specification limit,
the 24-hour test must be repeated, within the next 24-hour period. If the GEMS
again fails to meet the specification limit, remove the monitor from service.
Specification limit: ±20% (maximum percent difference between CEMS and CB)
24-hour percent difference (CEM vs. CB) IcEMS' _t x 100 Equation 8
ICB I
where:
CEMS=SO,/O, monitor system reading (SO, lb/108 Btu)
CB = CB measurement results (SO, lb/108 Btu)
(D) Initial and quarterly performance specification tests of CEMS. Initially and
once each three months, conduct at least one 3-hour relative accuracy test (com-
bined SO9 and O» channels as per Reference 1), and a response time and calibra-
tion error test, (as per Reference 2). The calculation procedures provided in Refer-
ences 1 and 2 shall also be used.
Specification limits: • Relative Accuracy=±20% (maximum percent difference between
the CEMS and the RM data in units of Ib SO2/109 Btu)
• Response Time=15 minutes
• Calibration Error=5.0% (SO, and O, channels separately)
(E) Unscheduled performance specification tests of the CEMS.—If for any
reason (other than routine maintenance as specified in the Lear Siegler operating
manual) the GEMS is taken out of service or its performance is not within the
specification limits of paragraph (g)(6) of this section, the Company shall conduct a
complete Performance Specification Test (PST) of the CEMS, according to the
combined requirements of References 1 and 2, as per paragraph (g](6](i}(D) of this
section. Whenever a CEMS is taken out of service and a supplementary CB system
is being used, the CEMS shall not replace the CB system until such time that the
Company has demonstrated that the performance of the CEMS is within all of the
performance limits established by paragraphs (g)(6)(i)(A), (B), (C), and (D) of this
section.
(ii) QA requirements, calculation procedures, and specification limits for CB
systems: At a minimum, the Company shall conduct the following initial, weekly.
and quarterly QA evaluations of all CB systems that are being used: (1) For any
quality assurance evaluations of a CEMS; and (2) as the secondary compliance
method when a CEMS is out of service. If a CB system does not meet these
specifications, then: (1) The CB must immediately be taken out of service; (2) the
Company must notify the Director, Division of Stationary Source Enforcement
(Washington, D.C.) within 72 hours after this determination is made; and (3) the
Company will be considered in violation of the provisions of the waiver until an
acceptable monitoring method is initiated (see paragraph (g)(8)(iii) of this section).
(A) Initial and weekly mid-range calibration checks of the CB system.—Cali-
bration checks of the CB system, using mixed SOi/COs mid-range calibration gas,
shall be performed initially and at least once each week thereafter. The calibration
gas shall be sampled by the CB system for no less than 2 hours at a flow rate
approximately the same as used during emission sampling. The following equation
111-26
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shall be used to determine if the CB meets the designated mid-range calibration
specification limit.
Specification limit: 10.0% (maximum percent difference between CB value and mid-range
gas value).
CB
Percent difference fCB vs. calibration gas) =
G.
xioo
Equiilion 9
where:
CB=bubbler value (SO, lb/10* Btu)
Gv=mixed SO,/CO, mid-range calibration gas value (SO* lb/106 Btu)
(B) Initial and quarterly relative accuracy tests of the CB systems. Operate at
least one of the CB systems used during the quarter for a 3-hour period. During the
same three hour period, collect at least one paired set of Reference Method 3 and 6
samplesf Each paired set shall consist of at least three to six 20-60 minute
consecutive ("back-to-back") runs. The following equation shall be used to deter-
mine if the CB meets the designated relative accuracy specifications limit.
CB Specification limit: 10.0% (maximum percent difference between CB value and and
RM value).
Percent difference (CB vs. RM)
CB
RM
xioo
Equation 10
I
where:
CB=bubbler value (SO, lb/106 Btu)
RM = average value of the paired Reference Method 3 and 6 runs (SO, lb/106 Btu)
(iii) QA requirements and specification limit for calibration gases: All calibra-
tion gases used for daily, weekly, or quarterly calibration drift checks, CB calibra-
tion checks and performance specification tests shall be analyzed following EPA
Traceability Protocol No. 1 (see reference 4) or with Method 3 or 6. If Method 3 or
6 is used, do the following. Within two weeks prior to its use on a CEMS, perform
triplicate analyses of the cylinder gas with the applicable reference method until
the results of three consecutive individual runs agree within 10 percent of the
average. Then use this average for the cylinder gas concentration.
(iv) Quality assuance checks for laboratory analysis: Each day that the Compa-
ny conducts Reference Method 6 or CB laboratory analyses, at least two SOi audit
samples shall be analyzed concurrently, by the same personnel, and in the same
manner as the Company uses when analyzing its daily emission samples. Audit
samples must be obtained from EPA. The following equation shall be used to
calculate the designated specification limit to determine if the Company's labora-
tory analysis procedures are adequate.
Analysis specification limit (for each of two audit samples): 5°i, (maximum percent
difference between laboratory value and the average of the actual value of the audit
samples).
Percent difference (laboratory vs. actual) =
SLY
SAV
-1
X100
Equation 11
where:
SLV=laboratory value (mg/DSCM) of the audit sample
SA\=actuol value (mg/DSCM) of the audit sample
(v) QA requirements, calculation procedures, and specification limits for 24-
hour fuel sampling and analysis: At a minimum, the Company shall conduct the
following bi-weekly QA evaluations of each boiler's fuel sampling and analysis
data.
111-27
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(A) Initially and at least bi-weekly the Company (or its own contractor labora-
tory) shall prepare and split a 60 mesh (250 micron) sample of coal (24-hour
composite) with an independent laboratory. The Company shall compare the inde-
pendent laboratory's heat content values to those of the Company's respective
analyses. Use the following equation to determine if the Company's coal analysis
procedures are adequate.
Specification limit: 500 Btu/lb (maximum difference between the two laboratories' results)
Inter-laboratory difference= CFA —IFA Equation 12
where:
CFA = Company's fuel analysis (Btu/lb)
IFA = Independent laboratory anlysis (Btu/lb)
(B) Analysis of reference coal.—At a minimum, the Company shall initially
(and thereafter bi-weekly), but on alternating weeks from above (g)(6)(v)(A) of this
section analysis, analyze the heat content of at least one reference coal sample.
Reference coal samples must be obtained from EPA. Use the following equation to
determine if the Company's fuel analysis procedures are adequate.
Specification limit: 500 Btu/lb (maximum difference between the Company laboratory's
value and the heat content of the reference coal).
Difference between Company's laboratory and reference = FAV —FLV Equation 13
where:
FLV = laboratory value (Btu/lb)
FAV = reference value (Btu/lb)
(vi) The use of more than the
minimum quantities of data to calculate
the QA specifications: Whenever the
Company supplements, expands, or
otherwise obtains more than the
minimum amount of QA data required
by paragraph (g)(6) of this section for the
QA evaluations, the Company shall use
all available data in assessing
achievement of the QA specifications.
All of the equations delineated above
may be expanded algebraically to
accommodate increased data, sample
runs, or test repetitions.
(7) Compliance Provisions:
(i) Compliance with all of the
provisions of this waiver requires:
(A) Documentation that the combined
emission levels (of Units Nos. 1, 2, and 3
or 1 and 2, as appropriate) did not
exceed the emission limitations
specified in paragraph (e) of this section.
(B) Documentation that the Company
acquired at least the minimum quantity
and quality of valid emission data
specified in paragraph (g](3) of this
section.
(C) Documentation that the Company
performed at least the minimum quality
assurance checks specified in paragraph
(g)(6) of this waiver; and
(D) Timely and adequate reporting of
all data specified in paragraph (g)(8) of
this section.
Failure to meet any of these
requirements constitutes a violation of
this waiver.
(ii) SOj emissions rate data from
individual boilers shall be obtained by
the primary compliance test method
(CEMS), by the secondary compliance
test method (CB), or other methods
approved by the Administrator. Data for
the heat input determination shall be
obtained by 24-hour as-fired fuel
analysis and 24-hour coal feed rate
measurements, or other methods
approved by the Administrator.
Compliance with all SO3 emission
limitations shall be determined in
accordance with the calculation
procedures set forth in paragraph (g)(5)
of this section or other procedures
approved by the Administrator. The
Company must demonstrate compliance
with all 3-hour, 24-hour, and 30-day SOa
emission limitations during all periods
of fuel combustion in one or more
boilers (beginning with the effective
date of the waiver), and including all
periods of process start-nip, shutdown,
and malfunction.
(iii) If the minimum quantity or quality
of emission data (required by paragraph
(g) of this section) were not obtained,
compliance of the affected facility with
the emission requirements specified in
this waiver may be determined by the
Administrator using all available data
which is deemed relevant.
(iv) For the purpose of demonstrating
compliance with the emission
limitations and data requirements of this
waiver:
(A) "A day" (24-hour period) begins at
12:01 p.m. and ends at 12:00 noon the
following day. The Company may select
an alternate designation for the
beginning and end of the 24-hour day.
However, the Agency must be notified
of any alternate designation of a "day"
and must be maintained throughout the
waiver period. Also, for the purpose of
reporting, each day shall be designated
by the calendar date corresponding with
the beginning of the 24-hour period;
(B) Where concurrent 24-hour data
averages are required (i.e., coal feed
rate, fuel sampling/analysis, SOa tons/
24 hours, and SO, lb/106 Btu), the
designated 24-hour period comprising a
day shall be consistent for all such
averages and measurement data; and
(C) There are eight discrete 3-hour
averaging periods during each day. .
(8) Notification and Reporting
Requirements.
(i) Notification: The Company shall
provide at least 30 days notice to the
Director, Division of Stationary Source
Enforcement (Washington, D.C.) of any
forthcoming quarterly CEMS
Performance Specification Tests and CB
accuracy tests.
(ii) Quarterly Compliance and
Monitoring Assessment Report
requirements: The Company shall
submit to the Director, Division of
Stationary Source Enforcement
(Washington, D.C.) "hard copy"
quarterly reports that present
compliance data and relevant
monitoring and process data (e.g.,
process output rate, heat input rate,
monitoring performance, and quality
assurance) acquired during the reporting
period. Quarterly reports shall be
postmarked no later than 30 days after
the completion of every (whole or
partial) calendar quarter during which
the waiver is in effect.
Note.—These requirements do not replace
or preclude the "Unscheduled Reporting
Requirements" contained in paragraph
(g)(8)(iii) of this section.
The following specific information shall
be furnished for every calendar day:
(A) General Information:
(7) Calendar date;
[2] The method(s), including
description, used to determine the 24-
hour heat input to each boiler (in units
ofBtu/hour);
(3)i The "F" factor(s) used for all
applicable calculations, the method of
111-28
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determination, and the type of fuel
rned;
I) Emission Data:
'l] Combined (Units Nos. 1, 2, and 3)
•hour average SOa emission rate (in
its of Ib/MMBtu);
2} Combined (Units Nos. 1,2 and 3)
ling 30-day average SOa emission rate
units of Ib/M&iBtu):
[3) Combined (Units Nos. 1, 2, and 3)
lour average emission rates (in units
tons SO3);
[4) Combined (Units Nos. 1. 2. and 3)
•hour average emission rates (in units
tons SOa);
[5] Combined (Units Nos. 1 and 2) 3-
ur average emission rates (in units of
ns SO3); and
(6) Combined (Units Nos. 1 and 2) 24-
ur average emission rates (in units of
ns SO,).
(C) Quality Assurance Check Data:
(J) The date and summary of results
>m all (initial and repetitions) of the
lality assurance checks performed
iring the quarter. This includes all
lalytical results on EPA's SO: and coal
idit samples.
(2) Description(s) of any
odification(s) made to the GEMS or CB
hich could affect the ability of those
stems to comply with the performance
lecifications in References 1 and 2, or
e CB performance specifications
jtablished by Section (g) of this waiver.
(D) Atypical Operations;
(1) Identification of specific periods
iring the calendar quarter when each
)iler was not combusting fuel;
[2] Periods of time when 3-hour, 24-
>ur, and/or 30-day averages were
stained using continuous bubbler data;
(3) All emission averages which have
jen calculated using a composite of
\>o or more different sampling methods
e.. periods when both CEMS and CB
/stems have been used) must be
lentified by designating all duration(s)
id cause(s) of data loss during such
;riods:
(4) For each instance when a CEMS
is been out of service, the Company
lall designate:
{/) Time, date, duration;
(if) Reason for such downtime;
(Hi) Corrective action taken;
(iv) Duration before CB sampling
began:
(v) Time, date, and performance
specification test (summary) results
acquired before CEMS returned to
service; and
(vi) Time and date when CEMS
actually returned to service, relative to
terminating CB sampling.
(5) Where only a portion of
continuouo data from any averaging
period(s) was obtained, the duration per
averaging period(s) when data were
acquired and were used to calculate the
emission average(s) must be identified;
(0) If the required quantity or quality
of emission data (as per paragraph (g) of
this section) were not obtained for any
averaging period(s), the following
information must also be reported for
each affected boiler. (See also
Unscheduled Reporting Requirements.
paragraph (g)(7)(iv) of this section:
(/) Reason for failure to acquire
sufficient data;
(//) Corrective action taken;
(iv] Characteristics (percent sulfur.
ash content, heating value, and
moisture) of the fuel burned;
(v) Fuel feed rates and steam
production rates;
(vi) All emission and quality
assurance data available from this
quarter; and
(w7) Statement (signed by a
responsible Company official) indicating
if any changes were made in the
operation of the boiler or any
measurement change (±20 percent)
from the previous averaging period) in
the type of fuel or firing rate during such
period.
(E) Company Certifications: The
Company shall submit a statement
(signed by a responsible Company
official) indicating:
(1} Whether or not the QA
requirements of this waiver for the
CEMs, CB, and fuel sampling/analysis
methods, or other periodic audits, have
been performed in accordance with the
provisions of this waiver;
(2) Whether or not the data used to
determine compliance was obtained in
accordance with the method and
procedures required by this waiver,
including the results of the quality
assurance checks;
(3) Whether or not the data
requirements have been met or, if the
minimum data requirements have not
been met due to errors that were
unavoidable (attach explanation);
[4] Whether or not compliance with
all of the emission standards
established by this waiver have been
achieved during the reporting period.
(iii) Unscheduled Reporting
Requirements. The Company shall
submit to the Director, Division of
Stationary Source Enforcement
(Washington, D.C.).
(A) Complete results of all CEMS
performance specification tests within
45 days after the initiation of such tests:
(B) The Company shall report, within
72 hours, each instance of:
(1] Failure to maintain the combined
(Units Nos. 1, 2, and 3 and Units Nos. 1
and 2, respectively) SOa emission rates
below the emission limitations
prescribed in Section (e) of this waiver;
(2) Failure to acquire the specified
minimum quantity of valid emission
data; and
(3) Failure of the Company's CB(s) to
meet the quality assurance checks.
References
1. Standards of Performance for New
Stationary Sources; Revisions to General
Provisions and Additions to Appendix A, and
Reproposal of Revisions to Appendix B, 46 FR
8352 (January 26.1981).
2. Proposed Standards of Performance for
New Stationary Sources: Continuous
Monitoring Performance Specifications 44 KR
58602 (October 10,1979).
3. 40 CFR Part 60. Appendix A (July 1,
1979).
4. Quality Assurance Handbook for Air
Pollution Measurement Systems, Volume III.
Stationary Source Specific Methods. EPA-
600/4-77-027b. August 1977.
TTT-OQ
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TABLE 1.—REQUIRED PERFORMANCE CRITERIA FOR QIMUTY ASSURANCE (QA) EVALUATIONS
Sampling method
OEMS
CEMS
CEMS
CEMS
CEMS
CEMS
CEMS
CEMS
CEMS
CEMS
CEMS1
CEMS
CEMS
CEMS
CEMS
CB
CB
Fuel S&A
Fuel S&A
Minimum frequency '
Dailv
Daily
Daily
Dailv
Daily
Dailv
Daily
Daily
Daily
Daily . .
Weekly1
Initial and weekly
Initial and quarterly
Initial and bi-weekly
Initial and bi-weekly
Daily
OA check
24-hour zero drift SO,
24-hour zero drift Sd
24-hour calibration drift SOi
24-hour zero drift Cs
24-hour zero drift Cs
24-hour calibration drift d
24-hour calibration drift d
24-hour mid-range check (SOiO&i)
24-hour mid-range check (SO.O4.) _
Relative accuracy (SO./O, combined) _
Calibration error.....
24-hour calibration drift (SO. and Oj or COi)
Mid-range check (SO./CO,) .
Specification Nmit
20 0 percent difference '
50.0 percent calibration gas value
500 Btu/hr difference
500 Btu/hr difference
Duration
24 hours
24 hours
24 hours
24 hours
24 hours
24 hours '
9-12 hours. . .
(N/A)
(N/A)
(N/A)
3 hours
(N/A)
(N/A)
(N/A)
Calculation
procedures
Equation 11
H
H
U)
O
' Failure to meet this specification requires the test to be repeated one time. H this test documents a second failure to CEMS must be taken out of service.
-------
Appendix I—Determination of Sulfur Dioxide
Emissions From Fossil Fuel Fired Combustion
Sources (Continuous Bubbler Method)132
(Note.—The Company may use the method
or its modifications which it requested and
which are restated in Section (g)(2)(ii)(A)
during the waiver period.]
1. Applicability and Principle.
1.1 Applicability. This method applies to
the determination of sulfur dioxide (SO,)
emissions from combustion sources in terms
of emission rate ng/J (Ib/MMBtu).
1.2. Principle. A gas sample is extracted
from the sampling point (in the emission
exhaust duct or stack) over a 24-hour or other
specified time period. The SO, and CO,
contained in the sampled exhaust gases are
separated and collected in the sampling train.
The SO, fraction is measured by the barium-
thorium titration method and CO, is
determined gravimetrically.
2. Apparatus.
2.1 Sampling. The sampling train is shown
in Figure 1; the equipment required is the
same as for Method 6, except as specified
below:
2.1.1 Impingers. Three 150 ml. Mae West
impingcrs with a 1-mm restricted tip.
2.1.2 Absorption Tubes. Two 51 mm x 178
mm glass tubes with matching one-hole
stoppers.
2.2 Sample Recovery and Analysis. The
equipment needed for sample recovery and
analysis is the same as required for Method
6. In addition, a balance to measure (within
O.OSg) is needed for analysis.
3. Reagents.
Unless otherwise indicated, all reagents
must conform to the specifications
established by the Committee on Analytical
Reagents of the American Chemical Society.
Where such specifications are not available,
use the best available grade.
3.1. Sampling. The reagents required for
sampling are the same as specified in Method
6. except that 10 percent hydrogen peroxide
is used. In addition, the following reagents
are required:
3.1.1 Drierite. Anhydrous calcium sulfate
(CaSOJ dessicanl, 8 mesh.
3.1.2 Ascarite. Sodium hydroxide coated
asbestos for absorption of CO,, 8 to 20 mesh.
3.2 Sample Recovery and Analysis. The
reagents needed for sample recovery and
analysis are the same as for Method 6,
Sections 3.2 and 3.3, respectively.
4. Preparation of Collection Train. Measure
75 ml. of 80 percent IPA into the first impinger
and 75 ml. of 10 percent hydrogen peroxide
into each of the remaining impingers. Into one
of the absorption tubes place a one-hole
stopper and glass wool plug in the end and
add 150 to 200 grams of drierite to the tube.
As the drierite is added shake the tube to
evenly pack the absorbent. Cap the tube with
another plug of glass wool and a one-hold
stopper (use this end as the inlet for even
flow). The ascarite tube is filled in a similar
manner, using 150-175 grams of ascarite.
Clean and dry the outside of the ascarite tube
and weigh (at room temperatue, 20 degrees C)
to the nearest 0.1 gram. Record this initial
mass as M^. Assemble the train as shown in
Figure 1. Adjust the probe heater to a
temperature sufficient to prevent water
condensation.
4.1.1 Sampling. The bubbler shalfbe
operated continuously at a sampling rate
sufficient to collect 70-80 liters of source
effluent during the desired sampling period.
For example, a sampling rate of 0.05 liter/
min. is sufficient for a 24-hour average and
0.40 liter per minute for a 3-hour average. The
sampling rate shall not, however, exceed 1.0
liter/min.
4.2 Sample Recovery.
4.2.1 Peroxide Solution. Pour the contents
of the second and third impingers into a leak-
free polyethylene bottle for storage or
shipping. Rinse the two impingers and
connecting tubing with deionized distilled
water, and add the washings to the same
storage container.
4.2.2 Ascarile Tube. Allow the ascarite
tube to equilibrate with room temperature
(about 10 minutes), clean and dry the outside,
and weigh to the nearest O.lg in the same
manner as in Section 4.1.1. Record this final
mass (M.i) and discard the used ascarite.
4.3 Sample Analysis. The sample analysis
procedure for SO, is the same as specified in
Method 6. Section 4.3.
5. Calculations.
5.1 SO, mass collected.
MSM=32.03 (V,-VJ N VMlnV. Equation Al-1
Where:
Mjm=mass of SO, collected, mg
V,=volume of barium perchlorate titrant
used for the sample, ml (average of
replicate titrations).
Vu, = volume of barium perchlorate titrant
used for the blank, ml.
N=normality of barium perchlorate titrant.
milliequivalents/ml.
V.oin = total volume of solution in which the
sulfur dioxide sample is contained, ml.
V, = volume of sample aliquot titrated, ml. 5.2
Sulfur dioxide emission rate
Eso,=Fe (K,) MSO, Equation Al-2
(M.,-M.V)
Where:
M., = initial mass of ascarite, grams.
M^=final mass of ascarite. grams.
ESM=Emission rate of SO,, ng/J (Ib/MMBtu).
Fe=Carbon F factor for the fuel burned. M3/J.
from Method 19 (Ref. 2)
K2= 1.829X10'
Proposed/effective
36 FR 15704, 8/17/71
Promulgated
36 FR 24876, 12/23/71
(1)
Revised
37 FR 14877,
38 FR 28564,
39 FR 20790,
40 FR 2803,
40 FR 46250,
40 FR 59204,
41 FR 51397,
42 FR 5936,
42 FR 37936,
42 FR 41122,
42 FR 41424,
42 FR 61537,
43 FR 8800,
43 FR 9276,
44 FR 3491,
44 FR 33580,
44 FR 76786,
45 FR 8211,
45 FR 36077,
45 FR 47146,
46 FR 55975,
46 FR 57497,
47 FR 2314,
7/26/72 (2)
10/15/73 (4)
6/14/74 (8)
1/16/75 (11)
10/6/75 (18)
12/22/75 (23)
11/22/76 (49)
1/31/77 (57)
7/25/77 (64)
8/15/77 (67)
8/17/77 (68)
12/5/77 (76)
3/3/78 (83)
3/7/78 (84)
1/17/79 (94)
6/11/79 (98)
12/28/79 (107)
2/6/80 (110)
5/29/80 (112)
7/14/80 (115)
11/13/81 (132)
11/24/81 (133)
1/15/82 (141)
111-31
-------
FIGURE 1
CONTINOUOUS BUBBLER (S02/C02) SAMPLING TRAIN
[NOTE: See Section (g)(2)(ii) for acceptable modifications of the
CB train during the waiver period.)
80%
2-PROPANOL
(OPTIONAL)
OPTIONAL:
HEATED
PROBE AND
IN-STACK
FILTER
CONSTANT
RATE
PUMP
|FR Doc. 81-32510 Filed 11-12-tt: 8:45 am|
111-32
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Subpart Da—Standard* of
Performance for Electric Utility Steam
Generating Units for Which
Construction Is Commenced After
September IS, 1978 93<"°
$60.40a Appflcabfltty and designation of
affected facility.
(a) The affected facility to which this
subpart applies is each electric utility
steam generating unit:
(1) That is capable of combusting
more than 73 megawatts (250 million
Btu/hour) heat input of fossil fuel (either
alone or in combination with any other
fuel); and
(2) For which construction or
modification is commenced after
September 18,1978.
(b) This subpart applies to electric
utility combined cycle gas turbines that
are capable of combusting more than 73
megawatts (250 million Btu/hour} heat
input of fossil fuel in the eteam
generator. Only emissions resulting from
combustion of fuels in the steam
generating unit are subject to this
subpart. (The gas turbine emissions are
subject to Subpart CG.)
(c) Any change to an existing fossil-
fuel-fired steam generating unit to
accommodate the use of combustible
materials, other than fossil fuels, shall
not bring that unit under the
applicability of this subpart
(d) Any change to an existing steam
generating unit originally designed to
fire gaseous or liquid fossil fuels, to
accommodate the use of any other fuel
(fossil or nonfossil) shall not bring that
unit under the applicability of this
subpart.
J 60.41s Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
"Steam generating unit" means any
furnace, boiler, or other device need for
combusting fuel for the purpose of
producing steam (including fossil-fuel-
fired steam generators associated with
combined cycle gas turbines; nuclear
steam generators are not included).
"Electric utility steam generating unit"
means any steam electric generating
unit that is constructed for the purpose
of supplying more than one-third of its
potential electric output capacity and
more than 25 MW electrical output to
any utility power distribution system for
sale. Any steam supplied to a steam
distribution system for the purpose of
providing steam to a steam-electric
generator that would produce electrical
energy for sale is also considered in
determining the electrical energy output
capacity of the affected facility.
"Fossil fuel" means natural gas,
petroleum, coal, and any form of solid,
liquid, or gaseous fuel derived from such
material for the purpose of creating
useful heat.
"Sabbiruminoas coal" means coal that
is classified as subbitaminoos A, B, or C
according to the American Society of
Testing and Materials' (ASTM)
Standard Specification for Classification
of Coals by Rank D388-66.
"Lignite" means coal that is classified
as lignite A or B according to the
American Society of Testing and
Materials' (ASTM) Standard
Specification for Classification of Coals
by Rank D388-66.
"Coal refuse" means waste products
of coal mining, physical coal cleaning,
and coal preparation operations (e.g.
culm, gob, etc.) containing coal, matrix
material, clay, and other organic and
inorganic material.
"Potential combustion concentration"
means the theoretical emissions (ng/J,
Ib/million Btu heat input) that would
result from combustion of a fuel in an
uncieaned state 9without emission
control systems) anch
(a) For particulate matter is:
(1) 3AX) ng/J (7O Ib/million Btu) heat
input for solid fuel; and
(2) 75 ng/J (0.17 Ib/million Btu) heat
input for liquid fuels.
(b) For sulfur dioxide is determined
under § 60.48a(b).
(c) For nitrogen oxides is:
(1) 290 ng/J (0.67 Ib/million Btu) heat
input for gaseous fuels;
(2) 310 ng/J (0.72 Ib/million Btn) heat
input for liquid fuels; and
(3) 990 ng/J (2.30 Ib/million Btn) heat
input for solid fuels.
"Combined cycle gas turbine" means
a stationary turbine combustion system
where heat from the turbine exhaust
gases is recovered by a steam
generating unit
"Interconnected" means that two or
more electric generating units are
electrically tied together by a network of
power transmission lines, and other
power transmission equipment
"Electric utility company" means the
largest interconnected organization,
business, or governmental entity that
generates electric power for sale (e-g-, a
holding company with operating
subsidiary companies).
"Principal company" means the
electric utility company or companies
which own the affected facility.
"Neighboring company" means any
one of those electric utility companies
with one or more electric power
interconnections to the principal
company and which have
geographically adjoining service areas.
"Net system capacity" means the sum
of the net electric generating capability
(not necessarily equal to rated capacity)
of all electric generating equipment
owned by an electric utility company
(including steam generating units,
internal combustion engines, gas
turbines, nuclear units, hydroelectric
units, and all other electric generating
equipment) plus firm contractual
purchases that are interconnected to the
affected facility that has the
malfunctioning flue gas desulfurization
system. The electric generating
capability of equipment under multiple
ownership is prorated based on
ownership unless the proportional
entitlement to electric output is
otherwise established by contractual
arrangement
"System load" means the entire
electric demand of an electric utility
company's service area interconnected
with the affected facility that has the
malfunctioning flue gas desulfurization
system plus firm contractual sales to
other electric utility companies. Sales to
other electric utility companies (e.g.,
emergency power) not on a firm
contractual basis may also be included
in the system load when no available
system capacity exists in the electric
utility company to which the power is
supplied for sale.
"System emergency reserves" means
an amount of electric generating
capacity equivalent to the rated
capacity of the single largest electric
generating unit in the electric utility
company (including steam generating
units, internal combustion engines, gas
turbines, nuclear units, hydroelectric
units, and all other electric generating
equipment) which is interconnected with
the affected facility that has the
malfunctioning flue gas desulfurization
system. The electric generating
capability of equipment under multiple
ownership is prorated based on
ownership unless the proportional
entitlement to electric output is
otherwise established by contractual
arrangement.
"Available system capacity" means
the capacity determined by subtracting
the system load and the system .
emergency reserves from the net system
capacity.
"Spinning reserve" means the sum of
the unutilized net generating capability
of all units of the electric utility
company that are synchronized to the
power distribution system and that are
capable of immediately accepting
111-33
-------
additional load. The electric generating
capability of equipment under multiple
ownership is prorated based on
ownership unless the proportional
entitlement to electric output is
otherwise established by contractual
arrangement.
"Available purchase power" means
the lesser of the following:
(a) The sum of available system
capacity in all neighboring companies.
(b) The sum of the rated capacities of
the power interconnection devices
between the principal company and all
neighboring companies, minus the sum
of the electric power load on these
interconnections.
(c) The rated capacity, of the power
transmission lines between the power
interconnection devices and the electric
generating units (the unit in the principal
company that has the malfunctioning
flue gas desulfurization system and the
unit(s) in the neighboring company
supplying replacement electrical power)
(ess the electric power load on these
transmission lines.
"Spare flue gas desulfurization system
module" means a separate system of
sulfur dioxide emission control
equipment capable of treating an /
amount of flue gas equal to the total
amount of flue gas generated by an
affected facility when operated at
maximum capacity divided by the total
number of nonspare flue gas
desulfurization modules in the system.
"Emergency condition" means that
period of time when:
(a) The electric generation output of
an affected facility with a
malfunctioning flue gas desulfurization
system cannot be reduced or electrical
output must be increased because:
(1) All available system capacity in
the principal company interconnected
with the affected facility is being
operated, and
(2) All available purchase power
interconnected with the affected facility
is being obtained, or
(b) The electric generation demand is
being shifted as quickly as possible from
an affected facility with a
malfunctioning flue gas desulfurization
system to one or more electrical
generating units held in reserve by the
principal company or by a neighboring
company, or
(c) An affected facility with a
malfunctioning flue gas desulfurization •
system becomes the only available unit
to maintain a part or all of the principal
company's system emergency reserves
and the unit is operated in spinning
reserve at the lowest practical electric
generation load consistent with not
causing significant physical damage to
the unit. If the unit is operated at a
higher load to meet load demand, an
emergency condition would not exist
unless the conditions under (a) of this
definition apply.
"Electric utility combined cycle gas
turbine" means any combined cycle gas
turbine used for electric generation that
is constructed for the purpose of
supplying more than one-third of its
potential electric output capacity and
more than 25 MW electrical output to
any utility power distribution system for
sale. Any steam distribution system that
is constructed for the purpose of
providing steam to a steam electric
generator that would produce electrical
power for sale is also considered in
determining the electrical energy output
capacity of the affected facility.
"Potential electrical output capacity"
is defined as 33 percent of the maximum
design heat input capacity of the steam
generating unit (e.g., a steam generating
unit with a 100-MW (340 million Btu/hr)
fossil-fuel heat input capacity would
have a 33-MW potential electrical
output capacity). For electric utility
combined cycle gas turbines the
potential electrical output capacity is
determined on the basis of the fossil-fuel
firing capacity of the steam generator
exclusive of the heat input and electrical
power contribution by the gas turbine.
"Anthracite" means coal that is
classified as anthracite according to the
American Society of Testing and
Materials' (ASTM) Standard
Specification for Classification of Coals
by Rank D388-66.
"Solid-derived fuel" means any solid,
liquid, or gaseous fuel derived from solid
fuel for the purpose of creating useful -
heat and includes, but is not limited to,
solvent refined coal, liquified coal, and
gasified coal.
"24-hour period" means the period of
time between 12:01 a.m. and 12:00
midnight.
"Resource recovery unit" means a
facility that combusts more than 75
percent non-fossil fuel on a quarterly
(calendar) heat input basis.
"Noncontinental area" means the
State of Hawaii, the Virgin Islands,
Guam, American Samoa, the
Commonwealth of Puerto Rico, or the
Northern Mariana Islands.
"Boiler operating day" means a 24-
hour period during which fossil fuel is
combusted in a steam generating unit for
the entire 24 hours.
§ 60.42s Standard for participate matter.
(a) On and after the date on which the
performance test required to be
conducted under § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere from
any affected facility any gases which
contain particulate matter in excess of:
(1) 13 ng/J (0.03 Ib/million Btu) heat
input derived from the combustion of
solid, liquid, or gaseous fuel;
(2) 1 percent of the potential
combustion concentration (99 percent
reduction) when combusting solid fuel;
and
(3) 30 percent of potential combustion
concentration (70 percent reduction)
when combusting liquid hie).
(b) On and after the date the
particulate matter performance test
required to be conducted under § 60.8 is
completed, no owner or operator subject
to the provisions of this subpart shall
cause to be discharged into the
atmosphere from any affected facility
any gases which exhibit greater than 20
percent opacity (6-minute average),
except for one 6-minute period per hour
of not more than 27 percent opacity.
{60.43a Standard for sulfur dioxide.
(a) On and after the date on which the
initial performance test required to be
conducted under § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere from
any affected facility which combusts
solid fuel or solid-derived fuel, except as,
provided under paragraphs (c), (d), (f) 01
(h) of this section, any gases which
contain sulfur dioxide in excess of:
(1) 520 ng/J (1.20 Ib/million Btu) heat
input and 10 percent of the potential
combustion concentration (90 percent
reduction), or
(2) 30 percent of the potential
combustion concentration (70 percent
reduction), when emissions are less than
260 ng/J (0.60 Ib/million Btu) heat input.
(b) On and after the date on which the
initial performance test required to be
conducted under § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere from
any affected facility which combusts
liquid or gaseous fuels (except for liquid
or gaseous fuels derived from solid fuels
and as provided under paragraphs (e) or
(h) of this section), any gases which
contain sulfur dioxide in excess of:
(1) 340 ng/J (0.80 Ib/million Btu) heat
input and 10 percent of the potential
combustion concentration (90 percent
reduction), or
(2) 100 percent of the potential
combustion concentration (zero percent
reduction) when emissions are less than
86 ng/J (0.20 Ib/million Btu) heat input.
(c) On and after the date on which the
initial performance test required to be
111-34
-------
conducted under § 60.8 is complete, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere from
any affected facility which combusts
solid solvent refined coal (SRC-I) any
gases which contain sulfur dioxide in
excess of 520 ng/J (1.20 Ib/million Btu)
heat input and 15 percent of the
potential combustion concentration (85
percent reduction) except as provided
under paragraph (f) of this section;
compliance with the emission limitation
is determined on a 30-day rolling
average basis and compliance with the
percent reduction requirement is
determined on a 24-hour basis.
(d) Sulfur dioxide emissions are
limited to 520 ng/J (1.20 Ib/million Btu)
heat input from any affected facility
which:
(1) Combusts 100 percent anthracite,
(2) Is classified as a resource recovery
facility, or
(3) Is located in a noncontinental area
and combusts solid fuel or solid-derived
fuel.
(e) Sulfur dixoide emissions are
limited to 340 ng/J (0.80 Ib/million Btu)
heat input from any affected facility
which is located in a noncontinental
area and combusts liquid or gaseous
fuels (excluding solid-derived fuels).
(f) The emission reduction
requirements under this section do not
apply to any affected facility that is
operated under an SO* commercial
demonstration permit issued by the
Administrator in accordance with the
provisions of $ 60.45a.
(g) Compliance with the emission
limitation and percent reduction
requirements under this section are both
determined on a 30-day rolling average
basis except as provided under
paragraph (c) of this section.
(h) When different fuels are
combusted simultaneously, the
applicable standard is determined by
proration using the following formula:
(1) If emissions of sulfur dioxide to the
atmosphere are greater than 260 ng/J
(0.60 Ib/million Btu) heat input
EM, = [340 x + 520 y]/100 and
Pgo, = 10 percent
(2) It emissions of sulfur dioxide to the
atmosphere are equal to or less than 260
ng/J (0.60 Ib/million Btu) heat input:
En, = [340 x + 520 y]/100 and
Pfo. = [90 x + 70 y]/100
where:
EM, is the prorated sulfur dioxide emission
limit (ng/J heat input),
Pio, is the percentage of potential sulfur
dioxide emission allowed (percent
reduction required = 100-Pn|).
x is the percentage of total heat input derived
from the combustion of liquid or gaseous
fuels (excluding solid-derived fuels)
y is the percentage of total heat input derived
from the combustion of solid fuel
(including solid-derived fuels]
{ 60.44a Standard for nitrogen oxides,
(a) On and after the date on which the
initial performance test required to be
conducted under § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere from
any affected facility, except as provided
under paragraph (b) of this section, any
gases which contain nitrogen oxides in
excess of the following emission limits,
based on a 30-day rolling average.
(1) NO, Emission Limits—
Fuel type
Gaseous Fuels:
Cod-derived fuels _____
An otNK |w>|ff
Uquid Fuels:
Coal-derived fuels .,.-, ....,-..,• .,.,,
ShaK>o emissions to 15 percent of
the potential combustion concentration
(85 percent reduction) on a 30-day
rolling average basis and to less than
520 ng/J (1.20 Ib/million Btu) heat input
on a 30-day rolling average basis.
(d) The owner or operator of an
affected facility that combusts coal-
derived liquid fuel and who is issued a
commercial demonstration permit by the
Administrator is not subject to the
applicable NO, emission limitation and
percent reduction under § 60.44a(a) but
must, as a minimum, reduce emissions
to less than 300 ng/J (0.70 Ib/million Btu)
111-35
-------
heat input on a 30-day rolling average
basis.
(e) Commercial demonstration permits
may not exceed the following equivalent
MW electrical generation capacity for
any one technology category, and the
,total equivalent MW electrical
generation capacity for all commercial
demonstration plants may not exceed
15,000 MW.
Technology
Equivalent
•Metrical
Pollutant capacity
(MW electrical
ampul)
Sokd solvent raOned coal
(SRCO ............. -
Fludizod bed vmifcustion
(etinosplNN &*)•••—•— .....
SO, 6,000-10,000
SO. 400-WOO
Cotf kquMcatton
SO,
NO.
technologies...
400-1.200
75O-10.000
15,000
160.46a Compliance provision*.
(a) Compliance with the particulate
matter emission limitation under
§ 60.42a(a)(l) constitutes compliance
with the percent reduction requirements
for particulate matter under
S 60.42a(a)(2) and (3).
(b) Compliance with the nitrogen
oxides emission limitation under
§ 60.44a(a) constitutes compliance with
the percent reduction requirements
under } 60.44a(a)(2).
(c) The particulate matter emission
standards under 5 60.42a and the
nitrogen oxides emission standards
under 5 60.44a apply at all times except
during periods of startup, shutdown, or
malfunction. The sulfur dioxide emission
standards under § 60.43a apply at all
times except during periods of startup,
shutdown, or when both emergency
conditions exist and the procedures
under paragraph (d) of this section are
implemented.
(d) During emergency conditions in
the principal company, an affected
facility with a malfunctioning flue gas
desulfurization system may be operated
if sulfur dioxide emissions are
minimized by:
(1) Operating all operable flue gas
desulfurization system modules, and
bringing back into operation any
malfunctioned module as soon as
repairs are completed.
(2) Bypassing flue gases around only
those flue gas desulfurization system
modules that have been taken out of
operation because they were incapable
of any sulfur dioxide emission reduction
or which would have suffered significant
physical damage if they had remained in
operation, and
(3) Designing, constructing, and
operating a spare flue gas
desulfurization system module for an
affected facility larger than 365 MW
(1,250 million Btu/hr) heat input
(approximately 125 MW electrical
output capacity). The Administrator
may at his discretion require the owner
or operator within BO days of
notification to demonstrate spare
module capability. To demonstrate this
capability, the owner or operator must
demonstrate compliance with the
appropriate requirements under
paragraph (a), (b). (d), (e), and (i) under
S 60.43a for any period of operation
lasting from 24 hours to 30 days when:
(i) Any one flue gas desulfurization
module is not operated,
(ii) The affected facility is operating at
the maximum heat input rate,
(iii) The fuel fired during the 24-hour
to 30-day period is representative of the
type and average sulfur content of fuel
used over a typical 30-day period, and
(iv) The owner or operator has given
the Administrator at least 30 days notice
of the date and period of time over
which the demonstration will be
performed.
(e) After the initial performance test
required under § 60.8, compliance with
the sulfur dioxide- emission limitations
and percentage reduction requirements
under { 60.43a and the nitrogen oxides
emission limitations under f 60.44a is
based on the average emission rate for
30 successive boiler operating days. A
separate performance test is completed
at the end of each boiler operating day
after the initial performance test, and d
new 30 day average emission rate for
both sulfur dioxide and nitrogen oxides
and a new percent reduction for sulfur
dioxide are calculated to show
compliance with the standards.
(f) For the initial performance test
required under S 60.8, compliance with
the sulfur dioxide emission limitations
and percent reduction requirements
under § 60.43a and the nitrogen oxides
emission limitation under { 60.44a is
based on the average emission rates for
sulfur dioxide, nitrogen oxides, and
percent reduction for sulfur dioxide for
the first 30 successive boiler operating
days. The initial performance test is the
only test in which at least 30 days prior
notice is required unless otherwise
specified by the Administrator. The
initial performance test is to be
scheduled so that the first boiler
operating day of the 30 successive boiler
operating days is completed within 60
days after achieving the maximum
production rate at which the affected
facility will be operated, but not later
than 180 days after initial startup of the
facility.
(g) Compliance is determined by
calculating the arithmetic average of all
hourly emission rates for SO, and NO,
for the 30 successive boiler operating
days, except for data obtained during
startup, shutdown, malfunction (NO,
only), or emergency conditions (SO,
only). Compliance with the percentage
reduction requirement for SO, is
determined based on the average inlet
and average outlet SO* emission rates
for the 30 successive boiler operating
days.
(h) If an owner or operator has not
obtained the minimum quantity of
emission data as required under S 60.47a
of this subpart compliance of the
affected facility with the emission
requirements under § § 60.43a and 60.44a
of this subpart for the day on which the
30-day period ends may be determined
by the Administrator by following the
applicable procedures in sections 6.0
and 7.0 of Reference Method 19
(Appendix A).
§ 60.47a Emission monitoring.
(a) The owner or operator of an
affected facility shall install, calibrate.
maintain, and operate a continuous
monitoring system, and record the
output of the system, for measuring the
opacity of emissions discharged to the
atmosphere, except where gaseous fuel
is the only fuel combusted. If opacity
interference due to water droplets exists
in the stack (for example, from the use
of an FGD system), the opacity is
monitored upstream of the interference
(at the inlet to the FCD system). If
opacity interference is experienced at
all locations (both at the inlet and outlet
of the sulfur dioxide control system),
alternate parameters indicative of the
particulate matter control system's
performance are monitored (subject to
the approval of the Administrator).
(b) The owner or operator of an
affected facility shall install, calibrate,
maintain, and operate a continuous
monitoring system, and record the •
output of the system, for measuring
sulfur dioxide emissions, except where
natural gas is the only fuel combusted,
as follows:
(1) Sulfur dioxide emissions are
monitored at both the inlet and outlet of
the sulfur dioxide control device.
(2) For a facility which qualifies under
the provisions of § 60.43a(d), sulfur
dioxide emissions are only monitored as
discharged to the atmosphere.
(3) An "as fired" fuel monitoring
system (upstream of coal pulverizers)
meeting the requirements of Method 19
(Appendix A) may be used to determine
111-36
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potential oulfur dioxide emissions in
place of a continuous sulfur dioxide
emission monitor at the inlet to the
sulfur dioxide control device as required
under paragraph (b)(l) of thi. section.
(c) The owner or operator of an
affected facility shall install, calibrate,
maintain, and operate a continuous
monitoring system, and record the
output of the system, for measuring
nitrogen oxides emissions discharged to
the atmosphere.
(d) The owner or operator of an
affected facility shall install, calibrate,
maintain, and operate a continuous
monitoring system, and record the
output of the system, for measuring the
oxygen or carbon dioxide content of the
flue gases at each location where sulfur
dioxide or nitrogen oxides emissions are
monitored.
(e) The continuous monitoring
systems under paragraphs (b), (c), and
(d) of this section are operated and data
recorded during all periods of operation
of the affected facility including periods
of startup, shutdown, malfunction or
emergency conditions, except for
continuous monitoring system
breakdowns, repairs, calibration checks,
and zero and span adjustments.
(f) When emission data are not
obtained because of continuous
monitoring system breakdowns, repairs,
calibration checks and zero and span
adjustments, emission data will be
obtained by using other monitoring
systems as approved by the
Administrator or the reference methods
as described in paragraph (h) of this
section to provide emission data for a
minimum of 18 hours in at least 22 out of
30 successive boiler operating days.
(g) The 1-hour averages required
under paragraph § 60.13(h) are
expressed in ng/J (Ibs/million Btu) heat
input and used to calculate the average
emission rates under § 60.48a. The 1-
hour averages are calculated using the
data points required under § 60.13(b). At
least two data points must be used to
calculate the 1-hour averages.
(h) Reference methods used to
supplement continuous monitoring
system data to meet the minimum data
requirements in paragraph i 60.47a(f)
will be used as specified below or
otherwise approved by the
Administrator.
(1) Reference Methods 3,6, and 7, as
applicable, are used. The sampling
location(s) are the same as those used
for the continuous monitoring system.
(2) For Method 6, the minimum
campling time is 20 minutes and the
minimum sampling volume is 0.02 dscm
(0.71 dscf] for each sample. Samples are
intervals. Each sample represents a 1-
hour average.
(3) For Method 7, samples are taken at
approximately 30-minute intervals. The
arithmetic average of these two
consective samples represent a 1-hour
average.
(4) For Method 3, the oxygen or
carbon dioxide sample is to be taken for
each hour when continuous SO3 and
NOj data are taken or when Methods 6
and 7 are required. Each sample shall be
taken for a minimum of 30 minutes in
each hour using the integrated bag
method specified in Method 3. Each
sample represents a 1-hour average.
(5) For each 1-hour average, the
emissions expressed in ng/J (Ib/million
Btu) heat input are determined and used
as needed to achieve the minimum data
requirements of paragraph (f) of this
section.
(i) The following procedures are used
to conduct monitoring system
performance evaluations under
i 60.13{c) and calibration checks under
§ 60.13(d).
(1) Reference method 8 or 7, as
applicable, is used for conducting
performance evaluations of sulfur
dioxide and nitrogen oxides continuous
monitoring systems.
(2) Sulfur dioxide or nitrogen oxides,
as applicable, is used for preparing
calibration gas mixtures under
performance specification 2 of appendix
B (9 this part.
(3) For affected facilities burning only
fossil fuel, the span value for a
continuous monitoring system for
measuring opacity is between 60 and 80
percent and for a continuous monitoring
system measuring nitrogen oxides is
determined as follows:
Fossil fusl
Span valuator
nitrogen oxzdas (ppm)
Liquid
600
SCO
1,000
600 (x+y)-I-1,0002
where:
it is the fraction of total heat input derived
from gaseous fossil fuel,
y is the fraction of total heat input derived
from liquid fossil fuel, and
s is the fraction of total heat input derived
from solid fossil fuel.
(4) All span values computed under
paragraph (b)(3) of this section for
burning combinations of fossil fuels are
rounded to the nearest 500 ppm.
(5) For affected facilities burning fossil
fuel, alone or in combination with non-
fossil fuel, the span value of the sulfur
dioxide continuous monitoring system at
fche inlet to the sulfur dioxide control
device is 125 percent of the maximum
estimated hourly potential emissions of
the fuel fired, and the outlet of the sulfur
dioxide control device is 50 percent of
maximum estimated hourly potential
emissions of the fuel fired.
(Sec. 114, Clean Air Act as amended (42
U.S.C. 7414).)
g S0.40Q Compliance determination
procedures and methods.
(a) The following procedures and
reference methods are used to determine
compliance with the standards for
particulate matter under § 60.42a.
(1) Method 3 is used for gas analysis
when applying method 5 or method 17.
(2) Method 5 is used for determining
particulate matter emissions and
associated moisture content. Method 17
may be used for stack gas temperatures
less than 160 C (320 F).
(3) For Methods 5 or 17, Method 1 is
used to select the sampling site and the
number of traverse sampling points. The
sampling time for each run is at least 120
minutes and the minimum sampling
volume is 1.7 dscm (60 dscf) except that
smaller sampling times or volumes,
when necessitated by process variables
or other factors, may be approved by the
Administrator.
(4) For Method 5, the probe and filter
holder heating system in the sampling
train is set to provide a gas temperature
no greater than 160°C (32°F).
(5) For determination of particulate
emissions, the oxygen or carbon-dioxide
sample is obtained simultaneously with
each run of Methods 5 or 17 by
traversing the duct at the same sampling
location. Method 1 is used for selection
of the number of traverse points except
that no more than 12 sample points are
required.
(6) For each run using Methods 5 or 17,
the emission rate expressed in ng/J heat
input is determined using the oxygen or
carbon-dioxide measurements and
•particulate matter measurements
obtained under this section, the dry
basis Fc-factor and the dry basis
emission rate calculation procedure
contained in Method 19 (Appendix A).
(7) Prior to the Administrator's
issuance of a particulate matter
reference method that does not
experience sulfuric acid mist
interference problems, particulate
matter emissions may be sampled prior
to a wet flue gas desulfurization system.
(b) The following procedures and
methods are used to determine
compliance with the sulfur dioxide
standards under § 60.43a.
(1) Determine the percent of potential
combustion concentration (percent PCC)
emitted to the atmosphere as follows:
111-37
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(i) Fuel Pretreatment (% Rf):
Determine the percent reduction
achieved by any fuel pretreatment using
the procedures in Method 19 (Appendix
A). Calculate the average percent
reduction for fuel pretreatment on a
quarterly basis using fuel analysis data.
The determination of percent Rf to
calculate the percent of potential
combustion concentration emitted to the
atmosphere is optional. For purposes of
determining compliance with any
percent reduction requirements under
§ 60.43a, any reduction in potential SOj
emissions resulting from the following
processes may be credited:
(A) Fuel pretreatment (physical coal
cleaning, hydrodesulfurization of fuel
oil, etc.),
(B) Coal pulverizers, and
(C) Bottom and flyash interactions.
(ii) Sulfur Dioxide Control System (%
Re): Determine the percent sulfur
dioxide reduction achieved by any
sulfur dioxide control system using
' emission rates measured before and
after the control system, following the
procedures in Method 19 (Appendix A);
or, a combination of an "as fired" fuel
monitor and emission rates measured
after the control system, following the
procedures in Method 19 (Appendix A).
When the "as fired" fuel monitor is
used, the percent reduction is calculated
using the average emission rate from the
sulfur dioxide control device and the
average SO» input rate from the "as
fired" fuel analysis for 30 successive
boiler operating days.
(iii) Overall percent reduction (% Ha):
Determine the overall percent reduction
using the results obtained in paragraphs
(b)(l) (i) and (ii) of this section following
the procedures in Method 19 (Appendix
A). Results are calculated for each 30-
day period using the quarterly average
percent sulfur reduction determined for
fuel pretreatment from the previous
quarter and the sulfur dioxide reduction
achieved by a sulfur dioxide control
system for each 30-day period in the
current quarter.
(iv) Percent emitted (% PCC):
Calculate the percent of potential
combustion concentration emitted to the
atmosphere using the following
equation: Percent PCC = 100-Percent R,
(2) Determine the sulfur dioxide
emission rates following the procedures
in Method 19 (Appendix A).
(c) The procedures and methods
outlined in Method 19 (Appendix A) are
used in conjunction with the 30-day
nitrogen-oxides emission data collected
under § 60.47a to determine compliance
with the applicable nitrogen oxides
standard under § 60.44.
(d) Electric utility combined cycle gas
turbines are performance tested for
particulate matter, sulfur dioxide, and
nitrogen oxides using the procedures of
Method 19 (Appendix A). The sulfur
dioxide and nitrogen oxides emission
rates from the gas turbine used in
Method 19 (Appendix A) calculations
are determined when the gas turbine is
performance tested under subpart GG.
The potential uncontrolled particulate
matter emission rate from a gas turbine
is defined as 17 ng/J (0.04 Ib/miliion Btu)
heat input.
§ 60.49a Reporting requirements.
(a) For sulfur dioxide, nitrogen oxides,
and particulate matter emissions, the
performance test data from the initial
performance test and from the
performance evaluation of the
continuous monitors (including the
transmissometer) are submitted to the
Administrator.
(b) For sulfur dioxide and nitrogen
oxides the following information- is
reported to the Administrator for each
24-hour period.
(1) Calendar date.
(2) The average sulfur dioxide and
nitrogen oxide emission rates (ng/J or
Ib/million Btu) for each 30 successive
boiler operating days, ending with the
last 30-day period in the quarter;
reasons for non-compliance with the
emission standards; and, description of
corrective actions taken.
(3) Percent reduction of the potential
combustion concentration of sulfur
dioxide for each 30 successive boiler
operating days, ending with the last 30-
day period in the quarter; reasons for
non-compliance with the standard; and,
description of corrective actions taken.
(4) Identification of the boiler
operating days for which pollutant or
dilutent data have not been obtained by
an approved method for at least 18
hours of operation of the facility;
justification for not obtaining sufficient
data; and description of corrective
actions taken.
(5) Identification of the times when
emissions data have been excluded from
the calculation of average emission
rates because of startup, shutdown,
malfunction (NO, only), emergency
conditions (SO. only), or other reasons,
and justification for excluding data for
reasons other than startup, shutdown,
malfunction, or emergency conditions.
(6) Identification of "F" factor used for
calculations, method of determination,
and type of fuel combusted.
(7) Identification of times when hourly
averages have been obtained based on
manual sampling methods.
(8) Identification of the times when
the pollutant concentration exceeded
full span of the continuous monitoring
system.
(9) Description of any modifications to
the continuous monitoring system which
could affect the ability of the continuous
monitoring system to comply with
Performance Specifications 2 or 3.
(c) If the minimum quantity of
emission data as required by § 60.47a is
not obtained for any 30 successive
boiler operating days, the following
information obtained under the
requirements of § 60.46a(h) is reported
to the Administrator for that 30-day
period:
(1) The number of hourly averages
available for outlet emission rates (no)
and inlet emission rates (n,) as
applicable.
(2) The standard deviation of hourly
averages for outlet emission rates (s0)
and inlet emission rates (s,) as
applicable.
(3) The lower confidence limit for the
mean outlet emission rate (E0*) and the
upper confidence limit for the mean inlet
emission rate (E,*) as applicable.
(4) The applicable potential
combustion concentration.
(5) The ratio of the upper confidence
limit for the mean outlet emission rate
(E,*) and the allowable emission rate
(Erfd)as applicable.
(d) If any standards under § 60.43a are
exceeded during emergency conditions
because of control system malfunction,
the owner or operator of the affected
facility shall submit a signed statement:
(1) Indicating if-emergency conditions
existed and requirements under
§ 60.46a(d) were met during each period,
and
(2) Listing the following information:
(i) Time periods the emergency
condition existed;
(ii) Electrical output and demand on
the owner or operator's electric utility
system and the affected facility;
(iii) Amount of power purchased from
interconnected neighboring utility
companies during the emergency period;
(iv) Percent reduction in emissions
achieved;
(v) Atmospheric emission rate (ng/J)
of the pollutant discharged; and
(vi) Actions taken to correct control
system malfunction.
(e) If fuel pretreatment credit toward
the sulfur dioxide emission standard
under § 60.43a is claimed, the owner or
operator of the affected facility shall
submit a signed statement:
(1) Indicating what percentage
cleaning credit was taken for the
calendar quarter, and whether the credit
was determined in accordance with the
111-38
-------
provisions of 5 60.48a and Method 19
(Appendix A); and
(2) Listing the quantity, heat content.
and date each pretreated fuel shipment
was received during the previous
quarter; the name and location of the
fuel pretreatment facility; and the total
quantity and total heat content of all
fuels received at the affected facility
during the previous quarter.
(f) For any periods for which opacity,
sulfur dioxide or nitrogen oxides
emissions data are not available, the
owner or operator of the affected facility
shall submit a signed statement
indicating if any changes were made in
operation of the emission control system
during the period of data unavailability.
Operations of the control system and -
affected facility during periods of data
unavailability are to be compared with
operation of the control system and
affected facility before and following the
period of data unavailability.
(g) The owner or operator of the
affected facility shall submit a signed
statement indicating whether:
(1) The required continuous
monitoring system calibration, span, and
drift checks or other periodic audits
have or have not been performed as
specified.
(2) The data used to show compliance
was or was not obtained in accordance
with approved methods and procedures
of this part and is representative of
plant performance.
(3] The minimum data requirements
have or have not been met; or, the
minimum data requirements have not
been met for errors that were
unavoidable. v
(4) Compliance with the standards has
or has not been achieved during the
reporting period.
(h) For the purposes of the reports
required under § 60.7, periods of excess
emissions are defined as all 6-minute
periods during which the average
opacity exceeds the applicable opacity
standards under § 60.42a(b). Opacity
levels in excess of the applicable
opacity standard and the date of such
excesses are to be submitted to the
Administrator each calendar quarter.
(i) The owner or operator of an
affected facility shall submit the written
reports required under this section and
subpart A to the Administrator for every
calendar quarter. All quarterly reports
shall be postmarked by the 30th day
following the end of each calendar
quarter.
(Sec. 114. Clean Air Act as amended (42
U.S.C. 7414).)
Proposed/effective
43 FR 42154, 9/19/78
Promulgated
44 FR 33580, 6/11/79 (98)
Revised
45 FR 8211, 2/6/80 (110)
111-39
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Subpart E—Standards of Performance
for Incinerators
§ 60.50 Applicability and designation of
affected facility. 8, 64
(a) The provisions of this subpart are
applicable to each Incinerator of more
than 45 metric -tons per day charging
rate (50 tons/day), which is the affected
facility.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after August 17,
1971, is subject to the requirements of
this subpart.
§ 60.51 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and In Subpart A
of this part.
(a) "Incinerator" means any furnace
used in the process of burning solid waste
for the purpose of reducing the volume
of the waste by removing combustible
matter.8
(b) "Solid waste" means refuse, more
than 50 percent of which Is municipal
type waste consisting of a mixture of
paper, wood, yard wastes, food wastes,
plastics, leather, rubber, and other com-
bustibles, and noncombustible materials
such as glass and rock.
(c)"Day" means 24 hours.8
§ 60.52 Standard for participate matter.8
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 Is completed, no owner
or operator subject to the provisions of
this part shall cause to be discharged
into the atmosphere from any affected
facility any gases which contain par-
ticulate matter in excess of 0.18 g/dscm
(0.08 gr/dscf) corrected to 12 percent
CO,.
§ 60.53 Monitoring of operations.8
(a) The owner or operator of any In-
cinerator subject to the provisions of this
part shall record the daily charging rates
and hours of operation.
(Sec. 114. Clean Air Act is amended (42
U.S.C. 7414)). 68, 83
§ 60.54 Test methods and procedures.8
(a) The reference methods In Ap-
pendix A to this part, except as provided
for In S 60.8(b), shall be used to deter-
mine compliance with the standard pre-
scribed in § 60.52 as follows:
(1) Method 5 for the concentration of
particulate matter and the associated
moisture content;
(2) Method 1 for sample and velocity
traverses;
(3) Method 2 for velocity and volu-
metric flow rate; and
(4) Method 3 for gas analysis and cal-
culation of excess air, using the Inte-
grated sample technique.
(b) For Method 5, the sampling time
for each run shall be at least 60 minutes
and the minimum sample volume shall
be 0.85 dscm (3G.O dscf) except that
smaller sampling times or sample vol-
umes, when necessitated by process vari-
ables or other factors, may be approved
by the Administrator.
(c) If a wet scrubber is used, the gas
analysis sample shall reflect flue gas con-
ditions after the scrubber, allowing for
carbon dioxide absorption by sampling
the gas on the scrubber inlet and outlet
sides according to either the procedure
under paragraphs (c) (1) through (c) (5)
of this section or the procedure under
paragraphs (c) (1), (c) (2) and (c) (6)
of this section as follows:
(1) The outlet sampling site shall be
the same as for the particulate matter
measurement. The inlet site shall be
selected according to Method 1, or as
specified by the Administrator.
(2) Randomly select 9 sampling points
within the cross-section at both the Inlet
and outlet sampling sites. Use the first
set of three for the first run, the second
set for the second run, and the third set
for the third run.
(3) Simultaneously with each par-
ticulate matter run, extract and analyze
for CO, an integrated gas sample accord-
Ing to Method 3, traversing the three
sample points and sampling at each
point for equal Increments of time. Con-
duct the runs at both inlet and outlet
sampllrig sites.
(4) Measure the volumetric flow rate
at the inlet during each particulate mat-
ter run according to Method 2, using the
full number of traverse points. For the
inlet make two full velocity traverses ap-
proximately one hour apart during each
run and average the results. The outlet
volumetric flow rate may be determined
from the particulate matter run
(Method 5).
(5) Calculate the adjusted CO, per-
centage using the following equation:
(% CO.) .di = (% CO,) di (Qdi/Qd.)
where:
(% CO,) >d) is the adjusted CO. percentage
which removes the effect of
CO, absorption and dilution
air,
(% CO,)di is the percentage of CO. meas-
ured before the scrubber, dry
basis,
Qdi is the volumetric flow rate be-
fore the scrubber, average of
two runs, dscf/mln (using
Method 2), and
Qdo Is the volumetric flow rate after
the scrubber, dscf/mln (us-
ing Methods 2 and 8).
(6) Alternatively, the following pro-
cedures may be substituted for the pro-
cedures under paragraphs (c) (3), (4).
and (5) of this section:
(1) Simultaneously with each particu-
late matter run, extract and analyze for
CO,, O,, and N, an integrated gas sample
according to Method 3, traversing the
three sample points and sampling for
equal increments of time at each point.
Conduct the runs at bcth the inlet and
outlet sampling sites.
(11) After completing the analysis of
the gas sample, calculate the percentage
of excess air (% EA) for both the Inlet
and outlet sampling sites using equation
3-1 In Appendix A to this part.
(Ill) Calculate the adjusted CO, per-
centage using the following equation;
.=(% coo..
rloo+(%EA>'i
1_100+(%KA).J
where :
( % CO,) .dj Is the adjusted outlet CO» per-
centage,
( % CO,) m is the percentage of COi meas-
ured before the scrubber, drj
basis,
( % EA) i la the percentage of excess all
at the inlet, and
( % EA) » is the percentage of excess air
at the outlet.
(d) Particulate matter emissions, ex-
pressed in g/dscm, shall be corrected to
12 percent CO, by using the following
formula:
120
%COi
where:
Cu is the concentration of partlculat*
matter corrected to 12 percent
CO..
e Is the concentration of partioulate
matter as measured by Method 6,
and
% COt la the percentage of CO. as meas-
ured by Method 3, or when ap-
plicable, the adjusted outlet CO,
percentage as determined by
paragraph (c) of this section.
Act
(42
Proposed/effective
15704, 8/17/71
opos
FR
Promulgated
36 FR 24876, 12/23/71 (1)
Revised
39 FR 20790. 6/14/74 (8)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
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Subpart F—Standards of Performance
for Portland Cement Plant*
§ 60.60 Applicability and designation of
affected facility. 64
(a) The provisions of this subpart are
applicable to the following affected fa-
cilities in Portland cement plants: kiln,
clinker cooler, raw mill system, finish
mill system, raw mill dryer, raw material
storage, clinker storage, finished product
storage, conveyor transfer points, bag-
ging and bulk loading and unloading sys-
tems.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after August 17,
1971, is subject to the requirements of
this subpart.
§ 60.61 Definitions.
As used In this subpart, all terms not
defined herein shall have the meaning
given them in the Act and In Subpart A
of this part.
(a) "Portland cement plant" means
any facility manufacturing Portland ce-
ment by either the wet or dry process.8
g 60.62 Standard for paniculate matter.8
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any kiln any
gases which:
(1) Contain participate matter In ex-
cess of 0.15 kg per metric ton of feed
(dry basis) to the kiln (0.30 Ib per ton).
(2) Exhibit greater than 20 percent
opacity.10
(b) On and after the date on which
the performance test required to be con-
ducted by { 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any clinker
cooler any gases which:
(1) Contain participate matter in ex-
cess of 0.050 kg per metric ton of feed
(dry basis) to the kiln (0.10 Ib per ton).
(2) Exhibit 10 percent opacity, or
greater.
(c) On and after the date on which
the performance test required to be con-
ducted by { 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any affected
facility other than the kiln and clinker
cooler any gases which exhibit 10 percent
opacity, or greater, 'a
§ 60.63 Monitoring of operations.8
(a) The owner or operator of any
Portland cement plant subject to the pro-
visions of this part shall record the daily
production rates and kiln feed rates.
(Sec. 114. Clean Air Act Is amended (42
U.S.C. 7414)). 68, 83
§ 60.64 Test methods and procedures^
(a) The reference methods in Appen-
dix A to this part, except as provided for
in { 60.8(b), shall be used to determine
compliance with the standards pre-
scribed in §60.62 as follows:
(1) Method 5 for the concentration
of participate matter and the associated
moisture content;
(2) Method 1 for sample and velocity
traverses;
(3) Method 2 for velocity and volu-
metric flow rate; and
(4) Method 3 for gas analysis.
(b) For Method 5, the minimum sam-
pling time and minimum sample volume
for each run, except when process varia-
bles or other factors justify otherwise to
the satisfaction of the Administrator.
shall be as follows:
(1) 60 minutes and 0.85 dscm (30.0
dscf) for the kiln.
(2) 60 minutes and 1.15 dscm (40.6
dscf) for the clinker cooler.
(c) Total kiln feed rate (except fuels),
expressed in metric tons per hour on a
dry basis, shall be determined during
each testing period by suitable methods;
and shall be confirmed by a material bal-
ance over the production system.
(d) For each run, participate matter
emissions, expressed in g/metric ton of
kiln feed, shall be determined by divid-
ing the emission rate in g/hr by the kiln
feed rate. The emission rate shall be
determined by the equation, g/hr=Qsx
c, where Q.=volumetric flow rate of the
total effluent in dscm/hr as determined
In accordance with paragraph (a) (3) of
this section, and c=particulate concen-
tration in g/dscm as determined In ac-
cordance with paragraph (a)(l) of this
section.
(Sec. 114. Clean Air Act Is amended (42
U.S.C. 7414)). 68, 83
Proposed/effecti ve
36 FR 15704, 8/17/71
Promulgated
36 FR 24876, 12/23/71 (1)
Revised
39 FR 20790.
39 FR 39872,
40 FR 46250.
42 FR 37936,
42 FR 41424,
43 FR 8800,
6/14/74 (8)
11/12/74 (10)
10/6/75 (18)
7/25/77 (64)
8/17/77 (68)
3/3/78 (83)
111-41
-------
Subpart G—Standards of Performance
for Nitric Acid Plants
§ 60.70 Applicability and designation of
affected facility. 64
(a) The provisions of this subpart are
applicable to each nitric acid production
unit, which is the affected facility.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after August 17,
1971, is subject to the requirements of
this subpart.
§ 60.71 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart A
of this part.
(a) "Nitric acid production unit"
means any facility producing weak nitric
acid by either the pressure or atmos-
pheric pressure process.
(b) "Weak nitric acid" means acid
which is 30 to 70 percent in strength.
method test data averages by the moni-
toring data averages to obtain a ratio ex-
pressed in units of the applicable stand-
ard to units of the monitoring data, i.e.,
kg/metric ton per ppm (Ib/short ton per
ppm)-. The conversion factor shall be re-
established during any performance test
under i 60.8 or any continuous .monitor-
ing system performance evaluation under
§60.13(c).
(c) The owner or operator shall record.
the daily production rate and hours of
operation.
(d) [Reserved] 8
(e) For the purpose 6f reports required
under § 60.7(c), periods of excess emis-
sions that shall be reported are defined
as any three-hour period during which
the average nitrogen oxides emissions
(arithmetic average of three contiguous
one-hour periods) as measured by a con-
tinuous monitoring system exceed the
standard under § 60.72(a).4»'8
(Sec. 114, Clean Air Act ts amended (42
U.S.C. 7414)). *8, 83
§ 60.72 Standard for nitrogen oxide*.3/8
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 Is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any affected
facility any gases which:
(1) Contain nitrogen oxides, ex-
pressed as NO*, In excess of 1.5 kg per
metric ton of acid produced (3.0 Ib per
ton), the production being expressed as
100 percent nitric acid.
(2) Exhibit 10 percent opacity, or
greater. 18
1 ft
§ 60.73 Emission monitoring.
(a) A continuous monitoring system
for the measurement of nitrogen oxides
shall be installed, calibrated, maintained,
and operated by the owner or operator.
The pollutant gas used to prepare cali-
bration gas mixtures under paragraph
2.1, Performance Specification 2 and for
calibration checks under § 60.13 (d) to
this part, shall be nitrogen dioxide (NO:) .
The span shall be set at 500 ppm of nitro-
gen dioxide. Reference Method 7 shall
be used for conducting monitoring sys-
tem performance evaluations under 5 60.-
(b) . The owner or operator shall estab-
lish a conversion factor for the purpose
of converting monitoring data into units
of the applicable standard (kg/metric
ton, Ib/short ton) . The conversion factor
shall be established by measuring emis-
sions with the continuous 'monitoring
system concurrent with measuring .emis-
sions with the applicable reference meth-
od tests. Using only that portion of the
continuous monitoring emission data
that reoresents emission measurements
concurrent with the reference method
test periods, the conversion factor shall
be determined by dividing the reference
§ 60.74 Te»t method* and procedure*. 8
(a) The reference methods in Appen-
dix A to this part, except as provided for
In 5 60.8(b), shall be used to determine
compliance with the standard prescribed
In { 60.72 as follows:
(1) Method 7 for the concentration of
NO,: -
(2) Method 1 for sample and velocity
traverses;
(3) Method 2 for velocity and volu-
metric flow rate; and
(4) Method 3 for gas analysis.
(b) For Method 7, the sample site shall
be selected according to Method 1 and
the sampling point shall be the centroid
of the stack or duct or at a point no
closer to the walls than l.m (3.28 ft).
Each run shall consist of at least four
grab samples taken at approximately 15-
minutes intervals. The arithmetic mean
of the samples shall constitute the run
value. A velocity traverse shall be per-
formed once per run.
(c) Acid production rate, expressed in
metric tons per hour of 100 percent nitric
acid, shall be determined during each
testing period by suitable methods and
shall be confirmed by a material balance
over the production system.
(d) For each run, nitrogen oxides, ex-
pressed in g/metrlc ton of 100 percent
nitric acid, shall be determined by divid-
ing the emission rate in g/hrby the acid
production rate. The emission rate shall
be determined by the equation.
g/hr-Q.xc
where Q,—volumetric flow- rate of the
effluent in dscm/hr, as determined in ac-
cordance with paragraph (a) (3) of this
section, and c—NO, concentration in
g/dscm, as determined in accordance
with paragraph (a) (1) of this section.
(Sec. 114. Clean Air Act la amended (42
U.S.C. 7414)). *8.83
Proposed/effecti ve
36 FR 15704, 8/17/71
Promulgated
36 FR 24876, 12/23/71 (1)
Revised
38 FR 13562.
38 FR 28564,
39 FR 20790,
40 FR 46250,
42 FR 37936,
42 FR 41424,
43 FR 8800,
5/23/73 (3)
10/15/73 (4)
6/14/74 (8)
10/6/75 (18)
7/25/77 (64)
8/17/77 (68)
3/3/78, (83)
111-42
-------
Subport H—Standards of Performance
for Sulfuric Acid Plants
60.80 Applicability and designation of
affected facility. 64
(a) The provisions of this subpart are
applicable to each sulfuric acid produc-
tion unit, which is the affected facility.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after August 17.
1971. is subject to the requirements of
this subpart.
g 60.81 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart A
of this part.
(a) "Sulfuric acid production unit"
means any facility producing sulfuric
acid by the contact process by burning
elemental sulfur, alkylation acid, hydro-
gen sulfide, organic sulfides and rner-
captans, or acid sludge, but does not in-
clude facilities where conversion to sul-
furic acid is utilized primarily as a means
of preventing emissions to the atmos-
phere of sulfur dioxide or other sulfur
compounds.
(b) "Acid mist- means sulfuric acid
mist,, as measured by Method 8 of Ap-
pendix A to this part or an equivalent or
alternative method. 8
calibration checks under § 60.13(d) to
this part, shall be sulfur dioxida (SO..).
Reference Method 8 shall be used for
conducting monitoring system perform-
ance evaluations under S 60.13(c) ex-
cept that only the sulfur dioxide portion
of the Method 8 results shall be used. The
scan shall be set at 1000 ppm of sulfur
dioxide.
(b) The owner or operator snail estab-
lish a conversion factor for the purpose
of converting monitoring data into units
of the applicable standard (kg/metric
ton, Ib/short ton) . The conversion f ac-
tor shall be determined, as a minimum,
three times daily by measuring the con-
centration of sulfur dioxide entering the
converter using suitable methods (e.g.,
the Reich test. National Air Pollution
Control Administration Publication No.
999-AP-13 and calculating the appro-
priate conversion factor for each eight-
hour period as follows:
ri.ooo-o.oi5r-]
L r-s J
^^Ruct
«,
§ 60.82 Standard for tulfur dioxide.8
(a) On and after the date on which the
'ormance test required to be con-
iucted by t 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any affected
facility any gases which contain sulfur
dioxide in excess of 2 kg per metric ton
of acid produced (4 Ib per ton), the pro-
duction being expressed as 100 percent
RSO,.
8 60.83 Standard for acid mist.3'8
(a) On and after the date on which the
performance test required to be con-
ducted by i 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any affected
facility any gases which:
(1) Contain acid mist, expressed as
HiSOt, in excess of 0.075 kg per metric
ton of acid produced (0.15 Ib per ton),
the production being expressed as 100
percent HjSO..
<3> Exhibit 10 percent opacity, or
greater, is
§ 60.84 Emission monitoring. 18
(a) A continuous monitoring, system
for the measurement of sulfur dioxide
shall be installed, calibrated, maintained.
and operated by the owner or operator.
The pollutant gas used to prepare cali-
ation gas mixtures under paragraph
Performance Specification 2 and for
where;
CF ^conversion factor (kg/metric ton per
ppm. Ib/short ton per .ppm).
k ^constant derived from material bal-
ance. For determining CF In metric
units, k =0.0653. For determining CF
in English units. k = 0.1 306.
i = percentage of sulfur dioxide by vol-
ume entering the gas converter. Ap-
propriate corrections must be made
for air Injection plants subject to the
Administrator's approval.
s = percentage of sulfur dioxide by -vol-
ume in the emissions to the atmos-
phere determined by the continuous
monitoring system required under
paragraph (a) of this section.
(c) The owner or operator shall re-
cord all conversion factors and values un-
der paragraph (b) of this section from
which they were computed (I.e., CF, r,
and s).
(d) [Reserved] 8
(e) For toe purpose of reports under
S60.7(c), periods of excess emissions
shall be all three-hour periods (or the
arithmetic average of three consecutive
one-hour periods) during which the in-
tegrated average sulfur dioxide emissions
exceed the applicable standards under
S6082. 4/18
(Sec. 114, Clean Air Act is amended (42
UJS.C. 7414)). *8 83
§ 60.85 Test method* and procedure*.8
(a) The reference methods In Appen-
dix A to this part, except as provided for
in { 60.8(b), shall be used to determine
compliance with the standards pre-
scribed in 55 60.82 and 60.83 as follows:
. (1) Method 8 for the concentrations of
SO, and acid mist;
(2). Method 1 for sample and velocity
traverses;
(3) Method 2 for velocity and volu-
metric Sow rate; and
(4) Method 3 for gas analysis.
(b) The moisture content can be con-
sidered to be zero. For Method 8 the sam-
pling time for each run shall be at least
60 minutes and the minimum sample vol-
ume shall be 1.15 dscm.(40.6 dscf) except
that smaller sampling times or sample
volumes, when necessitated by process
variables or other factors, may be ap-
proved by the Administrator.
(c) Acid production rate, expressed in
metric tons per hour of 100 percent
HiSO«. shall be determined during each
testing period by suitable methods and
•hall be confirmed by a material bal-
ance' over the production system.
(d) Acid mist and sulfur dioxide emis-
sions, expressed in g/metric ton of 100
percent &SO., shall be determined by
dividing the emission rate in g/hr by the
acid production rate. The emission rate
shall be determined by the equation,
B/hr=Q.xc, where Q.=volume trie flow
rate of the effluent in dscm/hr as deter-
mined in accordance with paragraph
(a) (3) of this section, and c=acid mist
and SO, concentrations in g/dscm as
determined in accordance with para-
graph (a) (1) of this section.
(Sec. 114. Clean Air Act U amended (43
U.S.C. 7414)). 68'83
Proposed/effecti ve
36 FR 15704, 8/17/71
Promulgated
36 FR 24876, 12/23/71 (1)
Revised
38 FR 13562,
38 FR 28564,
39 FR 20790,
40 FR 46250,
42 FR 37936,
42 FR 41424,
43 FR 8800,
5/23/73 (3)
10/15/73 (4)
6/14/74 (8)
10/6/75 (18)
7/25/77 (64)
8/17/77 (68)
3/3/78 (83)
111-43
-------
Subpart I—Standards of Performance
for Asphalt Concrete Plants5-100
§ 60.90 Applicability and designation of
affected facility.
(a) The affected facility to which
the provisions of this subpart apply is
each asphalt concrete plant. For the
purpose of this subpart, an asphalt
concrete plant is comprised only of
any combination of the following:
Dryers; systems for screening, han-
dling, storing, and weighing hot aggre-
gate; systems for loading, transferring,
and storing mineral filler; systems for
mixing asphalt concrete; and the load-
ing, transfer, and storage systems asso-
ciated with emission control systems.
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after June
11, 1973, is subject to the requirements
of this subpart.
when necessitated by process variables
or other factors, may be approved by
the Administrator.
(Sec. 114, Clean Air Act as amended (42
U.S.C. 7414))68-83
§ 60.91 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart
A of this part.
(a) "Asphalt concrete plant" means
any facility, as described in § 60.90,
used to manufacture asphalt concrete
by heating and drying aggregate and
mixing with asphalt cements.
§ 60.92 Standard for participate matter.
(a) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall discharge or
cause the discharge into the atmos-
phere from any affected facility any
gases which:
(1) Contain particulate matter in
excess of 90 mg/dscm (0.04 gr/dscf).
(2) Exhibit 20 percent opacity, or
greater.'8
§ 60.93 Test methods and procedures.
(a) The reference methods appended
to this part, except as provided for in
i 60.8(b), shall be used to determine
compliance with the standards pre-
scribed in § 60.92 as follows:
(1) Method 5 for the concentration
of particulate matter and the associat-
ed moisture content,
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and volu-
metric flow rate, and
(4) Method 3 for gas analysis.
(b) For Method 5, the sampling time
for each run shall be at least 60 min-
utes and the sampling rate shall be at
least 0.9 dscm/hr (0.53 dscf/min)
except that shorter sampling times,
Proposed/effective
38 FR 15406, 6/11/73
Promulgated
39 FR 9308, 3/8/74 (5)
Revised
40 FR 46250, 10/6/75 (18)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
Reviewed
44 FR 51225, 8/31/79 (100)
111-44
-------
for
Seminaries5
§60.100 Applicability end designation of
affected facility.64-86
(a) The provisions of this subpart are
applicable to the following affected
facilities in petroleum refineries: fluid
catalytic cracking unit catalyst
regenerators, fuel gas combustion
devices, and all Claus sulfur recovery
plants except Claus plants of 20 long
tons per day (LTD) or less. The Claus
sulfur recovery plant need not be
physically located within the boundaries
of a petroleum refinery to be an affected
facility, provided it processes gases
produced within a petroleum refinery.
(b) Any fluid catalytic cracking unit
catalyst regenerator or fuel gas com-
bustion device under paragraph (a) of
this section which commences con-
struction or modification after June
11, 1973, or any Claus sulfur recovery
plant under paragraph (a) of this sec-
tion which commences construction or
modification after October 4, 1976, is
subject to the requirements of this
part.
§60.101 definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart
A.
(a) "Petroleum refinery" means any
facility engaged in producing gasoline,
kerosene, distillate fuel oils, residual
fuel oils, lubricants, or other products
through distillation of petroleum or
through redistillation, cracking or re-
forming of unfinished petroleum de-
rivatives.
(b) "Petroleum" means the crude oil
removed from the earth and the oils
derived from tar sands, shale, and coal.
(c) "Process gas" means any gas gen-
erated by a petroleum refinery process
unit, except fuel gas and process upset
gas as defined in this section.
(d) "fuel gas" means any' gas which is
generated at a petroleum refinery and
which is combusted. Fuel gas also
includes natural gas when the natural
gas is combined and combusted in any
proportion with a gas generated at a
refinery. Fuel gas does not include gases
generated by catalytic cracking unit
catalyst regenerators and fluid coking
burners.121
(e) "Process upset gas" means any
gas generated by a petroleum refinery
process unit as a result of start-up,
shut-down, upset or malfunction.
(f) "Refinery process unit" means
any segment of the petroleum refinery
in which a specific processing oper-
ation is conducted.
(g) "Fuel gas combustion device"
means any equipment, such as process
heaters, boilers and flares used to com-
bust fuel gas, except facilities in which
gases are combusted to produce sulfur
or sulluric acid.38
(h) "Coke buPn-off" means the coke
removed from the surface of the fluid
catalytic cracking unit catalyst by
combustion in the catalyst regenera-
tor. The rate of coke burn-off is calcu-
lated by the formula specified in
160.106.
(i) "Claus sulfur recovery plant"
means a process unit which recovers
sulfur from hydrogen sulfide by a
vapor-phase catalytic reaction of
sulfur dioxide and hydrogen sulfide.86
(j) "Oxidation control system"
means an emission control system
which reduces emissions from sulfur
recovery plants by converting these
emissions to sulfur dioxide.86
(k) "Reduction control system"
means an emission control system
which reduces emissions from sulfur
recovery plants by converting these
emissions to hydrogen sulfide.86
(1) "Reduced sulfur compounds"
means hydrogen sulfide (H2S), car-
bonyl sulfide (COS) and carbon disul-
fide
-------
Performance Specification 2 and for
calibration checks under § 60.13(d),
shall be sulfur dioxide (SO,). The span
shall be set at 100 ppm. For conduct-
ing monitoring system performance
evaluations under § 60.13(c), Reference
Method 6 shall be used.
(4) An instrument for continuously
monitoring and recording concentra-
tions of hydrogen sulfide in fuel gases
burned in any fuel gas combustion
device, if compliance with
f 60.104(a)(l) is achieved by removing
H2S from the fuel gas before it is
burned; fuel gas combustion devices
having a common source of fuel gas
may be monitored at one location, if
monitoring at this location accurately
represents the concentration of HjS in
the fuel gas burned. The span of this
continuous monitoring system shall be
300 ppm.86
(5) An instrument for continuously
monitoring and recording concentra-
tions of SO, in the gases discharged
into the atmosphere from any Claus
sulfur recovery plant if compliance
with § 60.104(a)(2) is achieved through
the use of an oxidation control system
or a reduction control system followed
by incineration. The span of this con-
tinuous monitoring system shall be
sent at 500 ppm.86
(6) An instrument(s) for continuous-
ly monitoring and recording the con-
centration of H,S and reduced sulfur
compounds in the gases discharged
into the atmosphere from any Claus
sulfur recovery plant if compliance
with § 60.104(a)(2) is achieved through
the use of a reduction control system
not followed by incineration. The
span(s) of this continuous monotoring
system(s) shall be set at 20 ppm for
monitoring and recording the concen-
tration of H,S and 600 ppm for moni-
toring and recording the concentration
of reduced sulfur compounds.86
(b) [Reserved]
(c) The average coke burn-off rate
(thousands of kilogram/hr) and hours
of operation for any fluid catalytic
cracking unit catalyst regenerator sub-
ject to § 60.102 or § 60.103 shall be re-
corded daily.
(d) For any fluid catalytic cracking
unit catalyst regenerator which is sub-
ject to § 60.102 and which utilizes an
incinerator-waste heat boiler to com-
bust the exhaust gases from the cata-
lyst regenerator, the owner or opera-
tor shall record daily the rate of com-
bustion of liquid or solid fossil fuels
(liters/hr or kilograms/hr) and the
hours of operation during which liquid
or solid fossil fuels are combusted in
the incinerator-waste heat boiler.
(e) For the purpose of reports under
i 60.7(c), periods of excess emissions
that shall be reported are defined as
follows:
(1) Opacity. All one-hour periods
which contain two or more six-minute
periods during which the average
opacity as measured by the continuous
monitoring system exceeds 30 percent' (4) Any six-hour period during
(2) Carbon monoxide. All hourly pe-
riods during which the average carbon
monoxide concentration in the gases
discharged into the atmosphere from
any fluid catalytic cracking unit cata-
lyst regenerator subject to § 60.103 ex-
ceeds 0.050 percent by volume.86
(3) Sulfur dioxide, (i) Any three-
hour period during which the average
concentration of H2S in any fuel gas
combusted in any fuel gas combustion
device subject to § 60.104(a)(l) exceeds
230 mg/dscm (0.10 gr/dscf), if compli-
ance is achieved by removing H,S from
the fuel gas before it is burned; or any
three-hour period during which the
average concentration of SO, in the
gases discharged into the atmosphere
from any fuel gas combustion device
subject to § 60.104(a)(l) exceeds the
level specified in § 60.104(a)(l), if com-
pliance is achieved by removing SO,
from the combusted fuel gases.86
(ii) Any twelve-hour period during
which the average concentration of
SO, in the gases discharged into the
atmosphere from any Claus sulfur re-
covery plant subject to § 60.104(a)(2)
exceeds 250 ppm at zero percent
oxygen on a dry basis if compliance
with § 60.104(b) is achieved through
the use of an oxidation control system
or a reduction control system followed
by incineration; or any twelve-hour
period during which the average con-
centration of H,S, or reduced sulfur
compounds in the gases discharged
into the atmosphere of any Claus
sulfur plant subject to § 60.104(a)(2)(b)
exceeds 10 ppm or 300 ppm, respec-
tively, at zero percent oxygen and on a
dry basis if compliance is achieved
through the use of a reduction control
system not followed by incineration.86
which the average emissions (arithme-
tic average of six contiguous one-hour
periods) of sulfur dioxide as measured
by a continuous monitoring system
exceed the standard under § 60.104.
(Sec. 114. Clean Air
U.S.C. 7414»68-83
Act as amended (42
§ 60.106 Test methods and procedures.
(a) For the purpose of determining
compliance with § 60.102(a)(l). the fol-
lowing reference methods and calcula-
tion procedures shall be used:
(1) For gases released to the atmos-
phere from the fluid catalytic cracking
unit catalyst regenerator:
(i) Method 5 for the concentration
of particulate matter and moisture
content,
(ii) Method 1 for sample and velocity
traverses, and
(iii) Method 2 for velocity and volu-
metric flow rate.
(2) For Method 5. the sampling time
for each run shall be at least 60 min-
utes and the sampling rate shall be at
least 0.015 dscm/min (0.53 dscf/min),
except that shorter sampling times
may be approved by the Administrator
when process variables or other fac-
tors preclude sampling for at least 60
minutes.
(3) For exhaust gases from the fluid
catalytic cracking unit catalyst regen-
erator prior to the emission control
system: the integrated sample tech-
niques of Method 3 and Method 4 for
gas analysis and moisture content, re-
spectively; Method 1 for velocity tra-
verses; and Method 2 for velocity and
volumetric flow rate.
(4) Coke burn-off rate shall be deter-
mined by the following formula:
R.-0.2982 Quit (%COi+%CO) +2.088 QRA-0.0994 QBE
(Metric Units)
R.--0.0186 QRE (%COrf%CO)+0.1303 QHA-0.0062 QRS (^j2+%COt+%0.) (English Units)
where: »
R*=coke burn-off rate, kg/hr (English units: Ib/br).
0.2982=metrtc units material balance factor divided by 100, kg-min/hr-m».
0.018«= English units material balance (actor divided by 100, Ib-mln/hr-ft'.
Q»s=Duld catalytic cracking unit catalyst regenerator eibaust gas flow rat« before entering the emission
control system, as determined by method 2, dscm/min (English units: dscf/min).
%COi=perccnt carbon dioiide by volume, dry basis, as determined by Method 3.
Tc CO = percent carbon raonoilde by volume, dry basis, as determined by Method 3.
% Oi=pereent oiygen by volume, dry basis, as determined by Method 3.
2.088=metrlc units material balance factor divided by 100, kg-mln/hr-m'.
0.1303=Engllsh units material balance factor divided by 100, Ib-mln/hr-ft'.
QRA=alr rate to fluid catalytic cracking unit catalyst regenerator, as determined from fluid catalytic cracking
unit control room instrumentation, dscm/min (English units: dscf/min).
0.0994=metric units material balance factor divided by 100, kg-min/hr-m1.
0.0062= English units material balance factor divided by 100, Ib-mln/hr-ft'.
(5) Particulate emissions shall be determined by the following equation :
where:
80XHH'
8.57X10-»°
Rl=(60X10-»)QnvC. (Metric Units)
R«~(8.S7X10-t)QRvC. (English Units)
R,-particulate emission rate, kg/hr (English units: Ib/hr).
=me trie units conversion factor, min-kg/hr-mg.
• English units conversion factor, min-lb/lir-gr.
QRv=volumetric flow rate of eases discharged Into the atmosphere from the fluid catalytic cracking unit
catalyst regenerator following the emission control system, as determined by Method 2, dscm/min
(English units: dscf/min).
C.=particulate emission concentration discharged into the atmosphere, as determined by Method 8,
mg/dscm (English units: gr/dscf).
111-46
-------
(6) For each run. emissions expressed In kg/1000 kg (English units: lb/1000 Ib)
of coke burn-off In the catalyst regenerator shall be determined by the following
equation:
R.=1000g^ (Metric or English Units)
where:
K,= particular emission rate, kg/1000 kg (English units: lb/1000 Ib) of coke burn-ofi In the fluid catalytic crack-
ing unit catalyst regenerator.
lCOO=oonverslon factor, kg to 1000 kg (English units: Ib to 1000 Ib).
RB=participate emission rate, kg/br (English units: Ib/hr).
Bo=coke burn-oB rate, kg/hr (English units: Ib/hr).
(7) Zn those Instances !a which auxiliary liquid or solid fossil fuels are burned
In an taclnerator-waste heat boiler, the rate of participate matter emissions per-
mitted under 8 60.102 (b) must be determined. Auxiliary fuel heat Input, expressed
In millions of cal/hr (English units: Millions of Btu/hr) shall be calculated for
each run by fuel flow rate measurement and analysis of the liquid or solid auxiliary
fossil fuels. For each run, the rate of participate emissions permitted under
g 30.102(b) shall be calculated from the following equation:
R.=1.0-f?JiJ! (Metric Units)
XVe
R.°1.0+°''° "• (English Units)
There:
H.=allowable participate emission rate, kg/1000 kg (English units: lb/1000 Ib) of coke burn-ofi In the
fluid catalytic cracking unit catalyst regenerator.
1.0= emission standard, 1.0 kg/1000 kg (English units: 1.0 lb/1000 Ib) of coke burn-off In the fluid catalytic
cracking unit catalyst regenerator.
0.18= metric unit? maiimum allowable Incremental rate of paniculate emissions, g/mlllion cal.
0.10= English units maximum allowable Incremental rate of paniculate emissions. Ib/mlllion Btu.
H = heat input from solid or liquid fossil fuel, million cal/hr (English units: million Btu/hr).
R«=coke burn-off rate, kg/hr (English units: Ib/hr).
(b) For the purpose of determining
compliance with g 60.103, the integrated
sample technique of Method 10 shall be
used. The sample shall be extracted at a
rate proportional to the gas velocity at a
sampling point near the centroid of the
duct. The sampling time shall not be less
than 60 minutes.
(c) For the purpose of determining
compliance with § 60.104 (a X1),
Method 11 shall be used to determine
the concentration of, H,S and Method
6 shall be used to determine the con-
centration of SOj.86
(1) If Method 11 is used, the gases
sampled shall be introduced into the
sampling train at approximately atmo-
spheric pressure. Where refinery fuel
gas lines are operating at pressures
substantially above atmosphere, this
may be accomplished with a flow con-
trol valve. If the line pressure is high
enough to operate the sampling train
without a vacuum pump, the pump
may be eliminated from the sampling
train. The sample shall be drawn from
a point near the centroid of the fuel
gas line. The minimum sampling time
shall be 10 minutes and the minimum
sampling volume 0.01 dscm (0.35 dscf)
for each sample. The arithmetic aver-
age of two samples of equal sampling
time shall constitute one run. Samples
shall be taken at approximately 1-
hour Intervals. For most fuel gases,
sample times exceeding 20 minutes
may result in depletion of the collect-
ing solution, although fuel gases con-
taining low concentrations of hydro-
gen sulfide may necessitate sampling
for longer periods of time.86
(2) If Method 6 is used. Method 1
shall be used for velocity traverses and
Method 2 for determining velocity and
volumetric flow rate. The sampling
site for determining SO, concentration
by Method 6 shall be the same as for
determining volumetric flow rate by
Method 2. The sampling point in the
duct for determining SO* concentra-
tion by Method 6 shall be at the cen-
troid of the cross section if the cross
sectional area is less than 5 m2 (54 ft')
or at a point no closer to the walls
than 1 m (39 inches) if the cross sec-
tional area is 5 m1 or more and the
centroid is more than one meter from
the wall. The sample shall be extract-
ed at a rate proportional to the gas ve-
locity at the sampling point. The mini-
mum sampling time shall be 10 min-
utes -and the minimum sampling
volume 0.01 dscm (0.35 dscf) for each
sample. The arithmetic average of two
samples of equal sampling time shall
constitute one run. Samples shall be
taken at approximately 1-hour inter-
vals.86
(d) For the purpose of determining
compliance with §60.104(a)(2>,
Method 6 shall be used to determine
the concentration of SO, and Method
15 shall be used to determine the con-
centration of H,S and reduced sulfur
compounds.86
(1) If Method 6 Is used, the proce-
dure outlined In paragraph (c)(2) of
this section shall be followed except
that each run shall span a minimum
of four consecutive hours of continu-
ous sampling. A number of separate
samples may be taken for each run,
provided the total sampling time of
these samples adds up to a minimum
of four consecutive hours. Where more
than one sample is used, the average
SO, concentration for the run shall be
calculated as the time weighted aver-
age of the SO, concentration for each
sample according to the formula:
If
Where:
C» = SOi concentration for the run.
N=Number of samples.
Csi =SO, concentration for sample i
1st = Continuous sampling time of sample i.
T=Total continuous sampling time of all
N samples.86
(2) If Method 15 is used, each run
shall consist of 16 samples taken over
a minimum of three hours. The sam-
pling point shall be at the centroid of
the cross section of the duct if the
cross sectional area is less than 5 m'
(54 ft2) or at a point no closer to the
walls than 1 m (39 inches) if the cross
sectional area is 5 m3 or more and the
centroid is more than 1 meter from
the wall. To insure minimum residence
time for the sample inside the sample
lines, the sampling rate shall be at
least 3 liters/minute (0.1 ftVmin). The
SO, equivalent for each run shall be
calculated as the .arithmetic average of
the SO3 equivalent of each sample
during the run. Reference Method 4
shall be used to determine the mois-
ture content of the gases. The sam-
pling point for Method 4 shall be adja-
cent to the sampling point for Method
15. The sample shall be extracted at a
rate proportional to the gas velocity at
the sampling point. Each run shall
span a minimum of four consecutive
hours of continuous sampling. A
number of separate samples may be
taken for each run provided the total
sampling time of these samples adds
up to a minimum of four consecutive
hours. Where more than one sample is
used, the average moisture content for
the run shall be calculated as the time
weighted average of the moisture con-.
tent of each sample according to the
formula:
»„=
B*,=Proportion by volume of water vapor
in the gas stream for the run.
W=Number of samples.
B,, = Proportion by volume of water vapor
in the gas stream for the sample C
t, = Continuous sampling time for sample
i.
7= Total continuous sampling; time of all
N samples.
(Sec. 114 of the Clean Air Act, as amended
[42U.S.C. 74143).86
Proposed/effective
38 FR 15406, 6/11/73
41 FR 43866, 10/4/76
Promulgated
39 FR 9308, 3/8/74 (5)
Revised
40 FR 46250.
42 FR 32426.
42 FR 37936,
42 FR 39389,
42 FR 41424,
43 FR 8800,
43 FR 10866,
44 FR 13480,
44 FR 61542,
45 FR 79452,
10/6/75 (18)
6/24/77 (61)
7/25/77 (64)
8/4/77 (66)
8/17/77 (68)
3/3/78 (83)
3/15/78 (86)
3/12/79 (96)
10/25/79 (103)
12/1/80 (121)
iii-47
-------
Subpart K—Standards of Performance
for Storage Vessels for Petroleum
Liquids Constructed After June 11,
1973 and Prior to May 19,1978m
160.110 Applicabilitr and dc»i(cnation
of affected facility.*'
(a) Except as provided In ( 60.110(b),
the affected facility to which this sub-
part applies is each storage vessel for
petroleum liquids which has a storage
capacity greater than 151,412 liters
(40.000 gallons).
(b) This subpart does not apply to
storage vessels for petroleum or conden-
sate stored, processed, and/or treated at
a drilling and production facility prior
to custody transfer.8
(c> Subject to the requirements of
this subpart is any facility under para-
graph (a) of this section which:
(1) Has a capacity greater than 151,
416 liters (40,000 gallons), but not
exceeding 246,052 liters (65,000 gallons),
and commences construction or
modification after March 8,1974, and
prior to May 19,1978."1
(2) Has a capacity greater than 246,052
liters (65,000 gallons) and commences
construction or modification after June
11,1973, and prior to May 19,1978."'
§ 60.111 Definitions.
As used in this subpart, all terms not
denned herein shall have the meaning
given them in the Act and in Subpart A
of this part.
(a) "Storage vessel" means any tAri|r.
reservoir, or container used for the
storage of petroleum liquids, but does
not Include:
(1) Pressure vessels which are designed
to operate In excess of 15 pounds per
square Inch gauge without emissions to
the atmosphere except under emergency
conditions,
(2) Subsurface caverns or porous rock
reservoirs, or
(3) Underground tanks If the total
volume of petroleum liquids added to
and taken from a tank annually does
not exceed twice the volume of the tank.
(b) "Petroleum liquids" means
petroleum, condensate, and any finished
or intermediate products manufactured
in a petroleum refinery but does not
mean Nos. 2 through 6 fuel oils as
specified in ASTM-D-396-78, gas
turbine fuel oils Nos. 2-GT through 4—
GT as specified in ASTM-D-2880-78, or
diesel fuel oils Nos. 2-D and 4-D as
specified in ASTM-D-97578.'11
(c) "Petroleum refinery" means each
facility engaged in producing gasoline,
kerosene, distillate fuel oils, residual
fuel oils, lubricants, or other products
through distillation of petroleum or
.through redistillation, cracking,
extracting, or reforming of unfinished
petroleum derivatives. '
(d) "Petroleum" means the crude oil
removed from the earth and the oils
derived from tar sands, shale, and coal.8
(e) "Hydrocarbon" means any organic
compound consisting predominantly of
carbon and hydrogen.6
(f) "Condensate" means hydrocarbon
liquid separated from natural gas which
condenses due to changes In the tem-
perature and/or pressure and remains
liquid at standard conditions.
(g) "Custody transfer" means the
transfer of produced petroleum and/or
condensate, after processing and/or
treating in the producing operations.
from storage tanks or automatic trans-
fer facilities to pipelines or any other
forms of transportation.8
(h) "Drilling and production fa, 'llty"
means all drilling and servicing equip-
ment, wells, flow lines, separators, equip-
ment, gathering lines, and auxiliary non-
r.ransportation-related equipment used
in the production of petroleum but does
not include natural gasoline plants.8
(1) "True vapor pressure" means the
equilibrium partial pressure exerted by
• a petroleum liquid as determined In ac-
cordance with methods described In
American Petroleum Institute Bulletin
2517, Evaporation Loss from Floating
Roof Tanks, 1962.
(J) "Floating roof" means a storage
vessel cover consisting of a double deck,
pontoon single deck. Internal floating
cover or covered floating roof, which rests
upon and Is supported by the petroleum
liquid being contained, and is equipped
with a closure seal or seals to close the
space between the roof edge and tank
wall.
(k) "Vapor recovery system" means a
vapor gathering system capable of col-
lecting all hydrocarbon vapors and gases
discharged from the storage vessel and
a vapor disposal system capable of proc-
essing such hydrocarbon vapors and
eases so as to prevent their emission to
the atmosphere. ,
(1) "Reid vapor pressure" Is the abso-
lute vapor pressure of volatile crude oil
and volatile non-viscous petroleum
liquids, except liquified petroleum gases,
as determined by ASTM-D-323-68 (re-
approved 1968).
{60.112 Standard for volatile organic
compounds (VOC).1"
(a) The owner or operator of any stor-
age vessel to which this subpart applies
shall store petroleum liquids as follows:
(1) If the true vapor pressure of the
petroleum liquid, as stored. Is equal to
or greater than 78 mm Hg (1.5 psia) but
not greater than 570 mm Hg (11.1 psla),
the storage vessel shall be equipped with
a floating roof, a vapor recovery system,
or their equivalents.
(2) If the true vapor pressure of the
petroleum liquid as stored is greater than
570 mm Hg (ll.i psia). the storage ves-
sel shall be equipped with a vapor re-
covery system or Its equivalent.
! 60.113 Monitoring of operations.111
(a) Except as provided in paragraph
(d) of this section, the owner or operator
subject to this subpart shall maintain a
record of the petroleum liquid stored,
the period of storage, and the maximum
true vapor pressure of that liquid during
the respective storage period.
(b) Available data on the typical Reid
vapor pressure and the maximum
expected storage temperature of the
stored product may be used to
determine the maximum true vapor
pressure from nomographs contained in
API Bulletin 2517, unless the
Administrator specifically requests that
the liquid be sampled, the actual storage
temperature determined, and the Reid
vapor pressure determined from the
sample(s).
(c) The true vapor pressure of each
type of crude oil with a Reid vapor
pressure less than 13.8 kPa (2.0 psia) or
whose physical properties preclude
determination by the recommended
method is to be determined from
available data and recorded if the
estimated true vapor pressure is greater
than 6.9 kPa (1.0 psia).
(d) The following are exempt from the
requirements of this section:
(1) Each owner or operator of each
affected facility which stores petroleum
liquids with a Reid vapor pressure of
less than 6.9 kPa (1.0 psia} provided the
maximum true vapor pressure does not
exceed 6.9 kPa (1.0 psia).
(2) Each owner or operator of each
affected facility equipped with a vapor
recovery and return or disposal system
in accordance with the requirements of
{ 60.112.
(Sec. 114, Clean Air Act U amended (42
U.S.C. 7414)).68 83
Proposed/effective
38 FR 15406, 6/11/73
Promulgated
39 FR 9308, 3/8/74 (5)
Revised
39 FR 20790, 6/14/74 (8)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
45 FR 23374, 4/4/80 (111)
111-48
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Subpart Ka—Standards ©7
Performance for Storage Vessels for
(Petroleum Liquids Constructed After
May 1®, ne7®
§ SO. 11 Oa Applicability and designation of
affected facility.
(a) Except as provided in paragraph
{b) of this section, the affected facility to
which this subpart applies is each
storage vessel for petroleum liquids
which has a storage capacity greater
than 151.416 liters (40,000 gallons) and
for which construction is commenced
after May 18,1978.
(b) Each petroleum liquid storage
vessel with a capacity of less than
1,589,873 liters (420,000 gallons) used for
petroleum or condensate stored,
processed, or treated prior to custody
transfer is not an affected facility and,
therefore, is exempt from the
requirements of this subpart
i &0.1fia Definitions.
In addition to the terms and their
definitions listed in the Act and Subpart
A of this part the following definitions
apply in this subpart:
(a) "Storage vessel" means each tank,
reservoir, or container used for the
storage of petroleum liquids, but does
not include:
(1) Pressure vessels which are
designed to operate in excess of 204.9
kPa (15 psig) without emissions to the
atmosphere except under emergency
conditions.
(2) Subsurface caverns or porous rock
reservoirs, or
(3) Underground tanks if the total
volume of petroleum liquids added to
and taken from a tank annually does not
exceed twice the volume of the tank.
(b) "Petroleum liquids" means
petroleum, condensate, and any finished
or intermediate products manufactured
in a petroleum refinery but does not
mean Nos. 2 through 6 fuel oils as '
specified in ASTM-D-396-78, gas
turbine fuel oils Nos. 2-GT through 4-
GT as specified in ASTM-D-2880-78, or
diesel fuel oils Nos. 2-D and 4-D as
specified in ASTM-D-975-78.
(c) "Petroleum refinery" means each
facility engaged in producing gasoline,
kerosene, distillate fuel oils, residual
fuel oils, lubricants, or other products
through distillation of petroleum or
through redistillation, cracking,
extracting, or reforming of unfinished
petroleum derivatives.
(d) "Petroleum" means the crude oil
removed from the earth and the oils
derived from tar oands, shale, and coal.
(e) "Condensate" means hydrocarbon
liquid separated from natural gas which
condenses due to changes in the
temperature or pressure, or both, and
remains liquid at standard conditions.
(f) 'True vapor pressure" means the
equilibrium partial pressure exerted by
a petroleum liquid such as determined in
accordance with methods described in
American Petroleum Institute Bulletin
2517, Evaporation Loss from Floating
Roof Tanks, 1962.
(g) "Reid vapor pressure" is the
absolute vapor pressure of volatile
crude oil and volatile non-viscous
petroleum liquids, except liquified
petroleum gases, as determined by
ASTM-D-323-58 (reapproved 1968).
(h) "Liquid-mounted seal" means a
foam or liquid-filled primary seal
mounted in contact with the liquid
between the tank wall and the floating
roof continuously around the
circumference of the tank.
(i) "Metallic shoe seal" includes but is
not limited to a metal sheet held
vertically against the tank wall by
springs or weighted levers and is
connected by braces to the floating roof.
A flexible coated fabric (envelope)
spans the annular space between the
metal sheet and the floating roof.
(j) "Vapor-mounted seal" means a
foam-filled primary seal mounted
continuously around the circumference
of the tank so there is an annular vapor
space underneath the seal. The annular
vapor space is bounded by the bottom of
the primary seal, the tank wall, the
liquid surface, and the floating roof.
(k) "Custody transfer" means the
transfer of produced petroleum and/or
condensate, after processing and/or
treating in the producing operations,
from storage tanks or automatic transfer
facilities to pipelines or any other forms
of transportation.
§ SO. H12a Standard for volatile organic
compounds (VOC).
(a) The owner or operator of each
storage vessel to which this subpart
applies which contains a petroleum
liquid which, as stored, has a true vapor
pressure equal to or greater than 10.3
kPa (1.5 psia) but not greater than 76.6
kPa (11.1 peia) shall equip the storage
vessel with one of the following:
(1) An external floating roof,
consisting of a pontoon-type or double-
deck-type cover that rests on the surface
of the liquid contents and is equipped
with a closure device between the tank
wall and the roof edge. Except as
provided in paragraph (a)(l)(ii)(D) of
this section, the closure device is to
consist of two seals, one above the
other. The lower seal is referred to as
the primary seal and the upper seal is
referred to as the secondary seal. The
roof is to be floating on the liquid at all
times (i.e.. off the roof leg supports)
except during initial fill and when the
tank is completely emptied and
subsequently refilled. The process of
emptying and refilling when the roof is
resting on the leg supports shall be
continuous and shall be accomplished
as rapidly as possible.
(i) The primary seal is to be either a
metallic shoe seal, a liquid-mounted
seal, or a vapor-mounted seal. Each seal
is to meet the following requirements:
(A) The accumulated area of gaps
between the tank wall and the metallic
shoe seal or the liquid-mounted seal
shall not exceed 212 cm*per meter of
tank diameter (10.0 in 2per ft of tank
diameter) and the width of any portion
of any gap shall not exceed 3.81 cm (1 Vz
in).
(B) The accumulated area of gaps
between the tank wall and the
secondary seal used in combination
with a metallic shoe or liquid-mounted
primary seal shall not exceed 21.2 cm2
per meter of tank diameter (1.0 in2 per ft.
of tank diameter) and the width of any
portion of any gap shall not exceed 1.27
cm {'/a in.). There shall be no gaps
between the tank wall and the
secondary seal used in combination
with a vapor-mounted primary seal.122
(C) One end of the metallic shoe is to
extend into the stored liquid and the
other end is to extend a minimum
vertical distance of 61 cm (24 in) above
the stored liquid surface.
(D) There are to be no holes, tears, or
other openings in the shoe, seal fabric,
or seal envelope.
(ii) The secondary seal is to meet the
following requirements:
(A) The secondary seal is to be
installed above the primary seal so that
it completely covers the space between
the roof edge and the tank wall except
as provided in paragraph (a)(l)(ii)(B) of
this section.
(B) The accumulated area of gaps
between the tank wall and the
secondary seal shall not exceed 21.2 cm8
per meter of tank diameter (1.0 insper ft
of tank diameter) and the width of any
portion of any gap shall not exceed 1.27
cm(%in).
(C) There are to be no holes, tears or
other openings in the seal or seal fabric,
(D) The owner or operator is
exempted from the requirements for
secondary seals and the secondary seal
gap criteria when performing gap
measurements or inspections of the
primary seal.
(iif Each opening in the roof except
for automatic bleeder vents and rim
space vents is to provide a projection
below the liquid surface. Each opening
in the roof except for automatic bleeder
vents, rim space vents and leg sleeves is
to be equipped with a cover, seal or lid
which is to be maintained in a closed
position at all times (i.e., no visible gap)
except when the device is in actual use
or as described in pargraph (a)(l)(iv) of
this section. Automatic bleeder vents
111-49
-------
are to be closed at all times when the
roof is floating, except when the roof is
being floated off or is being landed on
the roof leg supports. Rim vents are to
be set to open when the roof is being
floated off the roof legs supports or at
the manufacturer's recommended
setting.
(iv) Each emergency roof drain is to
be provided with a slotted membrane
fabric cover that covers at least 90
percent of the area of the opening.
(2) A fixed roof with an internal
floating type cover equipped with.a
continuous closure device between the
tank wall and the cover edge.'The cover
is to be floating at all times, (i.e., off the
leg supports) except during initial fill
and when the tank is completely
emptied and subsequently refilled. The
process of emptying and refilling when
the cover is resting on the leg supports
shall be continuous and shall be
accomplished as rapidly as possible.
Each opening in the cover except for
automatic bleeder vents and the rim
space vents is to provide a projection
below the liquid surface. Each opening
in the cover except for automatic
bleeder vents, rim space vents, stub
drains and leg sleeves is to be equipped
with a cover, seal, or lid which is to be
maintained in a closed position at all
times (i.e., no visible gap) except when
the device is in actual use. Automatic
bleeder vents are to be closed at all
times when the cover is floating except
when the cover is being floated off or is
being landed on the leg supports. Rim
vents are to be set to open only when
the cover is being floated off the leg
supports or at the manufacturer's
recommended setting.
(3) A vapor recovery system which
collects all VOC vapors and gases
discharged from the storage vessel, and
a vapor return or disposal system which
is designed to process such VOC vapors
and gases so as to reduce their emission
to the atmosphere by at least 95 percent
by weight.
(4) A system equivalent to those
described in paragraphs (a)(l). (a)(2), or
(a) (3) of this section as provided in
S 60.114a.
(b) The owner or operator of each
storage vessel to which this subpart
applies which contains a petroleum
liquid which, as stored, has a true vapor
pressure greater than 76.6 kPa (11.1
psia), shall equip the storage vessel with
a vapor recovery system which collects
all VOC vapors and gases discharged
from the storage vessel, and a vapor
return or disposal system which is
designed to process such VOC vapors
and gases so as to reduce their emission
to the atmosphere by at least 95 percent
by weight
§60.113a Testing and procedures.
(a) Except as provided in § 60.8(b)
compliance with the standard
prescribed in § 60.112a shall be
determined as follows or in accordance
with an equivalent procedure as
provided in § 60.114a.
(1) The owner or operator of each
storage vessel to which this subpart
applies which has an external floating
roof shall meet the following
requirements:
(i) Determine the gap areas and
maximum gap widths between the
primary seal and the tank wall, and the
secondary seal and the tank wall
according to the following frequency
and furnish the Administrator with a
written report of the results within 60
days of performance of gap
measurements:
(A) For primary seals, gap
measurements shall be performed within
60 days of the initial fill with petroleum
liquid and at least once every five years
thereafter. All primary seal inspections
or gap measurements which require the
removal or dislodging of the secondary
seal shall be accomplished as rapidly as
possible and the secondary seal shall be
replaced as soon as possible.
(B) For secondary seals, gap
measurements shall be performed within
60 days of the initial fill with petroleum
liquid and at least once every year
thereafter.
(C) If any storage vessel is out of
service for a period of one year or more.
subsequent refilling with petroleum
liquid shall be considered initial fill for
the purposes of paragraphs (a](l)(i)(A)
and (a)(l)(i)((B) of this section.
(ii) Determine gap widths in the
primary and secondary seals
individually by the following
procedures:
(A) Measure seal gaps, if any, at one
or more floating roof levels when the
roof is floating off the roof leg supports.
(B) Measure seal gaps around the
entire circumference of the tank in each
place where a Va" diameter uniform
probe passes freely (without forcing or
binding against seal) between the seal
and the tank wall and measure the
circumferential distance of each such
location.
(C) The total surface area of each gap
described in paragraph (a)(l](ii)(B) of
this section shall be determined by using
probes of various widths to accurately
measure the actual distance from the
tank wall to the seal and multiplying
each such width by its respective
circumferential distance.
(iii) Add the gap surface area of each
gap location for the primary seal and the
secondary seal individually. Divide the
sum for each seal by the nominal
diameter of the tank and compare each
ratio to the appropriate ratio in the
standard in § 60.112a(a)(l)(i) and
S 60.112a(a](l)(ii).
(iv) Provide the Administrator 30 days
prior notice of the gap measurement to
afford the Administrator the opportunity
to have an observer present.
(2) The owner or operator of each
storage vessel to which this subpart
applies which has a vapor recovery and
return or disposal system shall provide
the following information to the
Administrator on or before the date on
which construction of the storage vessel
commences:
(i) Emission data, if available, for a
similar vapor recovery and return or
disposal system used on the same type
of storage vessel, which can be used to
determine the efficiency of the system.
A complete description of the emission
measurement method used must be
included.
(ii) The manufacturer's design
specifications and estimated emission
reduction capability of the system.
(iii) The operation and maintenance
plan for the system.
(iv) Any other information which will
be useful to the Administrator in
evaluating the effectiveness of the
system in reducing VOC emissions.
(Sec. 114, Clean Air Act as amended (42
U.S.C. 7414))
8 60.114a Equivalent equipment and
procedures.
(a) Upon written application from an
owner or operator and after notice and
opportunity for public hearing, the
Administrator may approve the use of
equipment or procedures, or both, which
have been demonstrated to his
satisfaction to be equivalent in terms of
reduced VOC emissions to the
atmosphere to the degree prescribed for
compliance with a specific paragraph(s)
of this subpart.
(b) The owner or operator shall
provide the following information in the
application for determination of
equivalency:
(1) Emission data, if available, which
can be used to determine the
effectiveness of the equipment or
procedures in reducing VOC emissions
from the storage vessel. A complete
description of the emission
measurement method used must be
included.
(2) The manufacturer's design .
specifications and estimated emission
reduction capability of the equipment
(3) The operation and maintenance
plan for the equipment
(4) Any other information which will
be useful to the Administrator in
evaluating the effectiveness of the
111-50
-------
equipment or procedures in reducing
VOC emissions.
(Sec. 114 of the Clean Air Act as amended (42
U.S.C. 7414))
§ 60.115a Monitoring of operations.
(a) Except as provided in paragraph
(d) of this section, the owner or operator
subject to this subpart shall maintain a
record of the petroleum liquid stored,
the period of storage, and the maximum
true vapor pressure of that liquid during
the respective storage period.
(b) Available data on the typical Reid
vapor pressure and the maximum
expected storage temperature of the
stored product may be used to
determine the maximum true vapor
pressure from nomographs contained in
API Bulletin 2517, unless the
Administrator specifically requests that
the liquid be sampled, the actual storage
temperature determined, and the Reid
vapor pressure determined from the
sample(s).
(c) The true vapor pressure of each
type of crude oil with a Reid vapor
pressure less than 13.8 kPa (2.0 psia) or
whose physical properties preclude
determination by the recommended
method is to be determined from
available data and recorded if the .
estimated true vapor pressure is greater
than 6.9 kPa (1.0 psia).
(d) The following are exempt from the
requirements of this section:
(1) Each owner or operator of each
storage vessel storing a petroleum liquid
with a Reid vapor pressure of less than
6.9 kPa (1.0 psia) provided the maximum
true vapor pressure does not exceed 6.9
kPa (1.0 psia).
(2) Each owner or operator of each
storage vessel equipped with a vapor
recovery and return or disposal system
in accordance with the requirements of
§§ 60.112a(a)(3) and 60.112a(b).
(Sec. 114 of the Clean Air Act as amended (42
U.S.C. 7414))
111-51
Proposed/effectjve
43 FR 21616, 5/18/78
Promulgated
45 FR 23374, 4/4/80 (111)
Revised
45 FR 83228, 12/18/80 (122)
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Subpart L—Standards of Performance
for Secondary Lead Smelters5
§60.120 Applicability and designation of
affected facility.64
(a) The provisions of this subpart
are applicable to the following affect-
ed facilities in secondary lead smelters:
Pot furnaces of more than 250 kg (550
Ib) charging capacity, blast (cupola)
furnaces, and reverberatory furnaces.
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after June
11, 1973, is subject to the requirements
of this subpart.
§60.121 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart
A of this part.
(a) "Reverberatory furnace" in-
cludes the following types of reverber-
atory furnaces: stationary, rotating.
rocking, and tilting.
(b) "Secondary lead smelter" means
any facility producing lead from a
leadbearing scrap material by smelting
to the metallic form.
(c) "Lead" means elemental lead or
alloys in which the predominant com-
ponent is lead.
§60.123 Test methods and procedures.
(a) The reference methods appended
to this part, except as provided for in
§ 60.8 (b), shall be used to determine
compliance with the standards pre-
scribed in § 60.122 as follows:
(1) Method 5 for the concentration
of particulate matter and the associat-
ed moisture content,
(2) Method 1 for sample and velocity
traverses.
(3) Method 2 for velocity and volu-
metric flow rate, and
(4) Method 3 for gas analysis.
(b) For method 5, the sampling time
for each run shall be at least 60 min-
utes and the sampling rate shall be at
least 0.9 dscm/hr (0.53 dscf/min)
except that shorter sampling times,
when necesitated by process variables
or other factors, may be approved by
the Administrator. Particulate sam-
pling shall be conducted during repre-
sentative periods of furnace operation,
including charging and tapping.
(Sec. 114, Clean Air Act as amended (42
U.S.C. 7414 H68-83
§60.122 Standard for particulate matter.
(a) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall discharge or
cause the discharge into the atmos-
phere from a blast (cupola) or rever-
beratory furnace any gases which:
(1) Contain particulate matter in
excess of 50 mg/dscm (0.022 gr/dscf).
(2) Exhibit 20 percent opacity or
greater.
(b) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall discharge or
cause the discharge into the atmos-
phere from any pot furnace any gases
which exhibit 10 percent opacity or
greater.18
Proposed/effective
38 FR 15406, 6/11/73
Promulgated
39 FR 9308, 3/8/74 (5)
Revised
39 FR 13776, 4/17/74 (6)
40 FR 46250, 10/6/75 (18)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-52
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Subpart M—Standards of Perform-
ance for Secondary Brass and
Bronze Ingot Production Plants5
§60.130 Applicability and designation of
affected facility.64
(a) The provisions of this subpart
are applicable to the following affect-
ed facilities in secondary brass or
bronze ingot production plants: Rever-
beratory and electric furnaces of 1,000
kg (2,205 Ib) or greater production ca-
pacity and blast (cupola) furnaces of
250 kg/hr (550 Ib/hr) or greater pro-
duction capacity.
(b) Any facility .under paragraph (a)
of this section that commences con-
struction or modification after June
11, 1973, is subject to the requirements
of this subpart.
§60.131 Definitions.
As used in this subpart. all terms not
defined herein shall have the meaning
given them in the Act and in Subpart
A of this part.
(a) "Brass or bronze" means any
metal alloy containing copper as its
predominant constituent, and lesser
amounts of zinc, tin, lead, or other
metals.
(b) "Reverberatory furnace" in-
cludes the following types of reverber-
atory furnaces: Stationary, rotating.
rocking, and tilting.
(c) "Electric furnace" means any
furnace which uses electricity to pro-
duce over 50 percent of the heat re-
quired in the production of refined
brass or bronze.
(d) "Blast furnace" means any fur-
nace used to recover metal from slag.
§ 60.133 Test methods and procedures.
(a) The reference methods appended
to this part, except as provided for in
§ 60.8(b), shall be used to determine
compliance with the standards pre-
scribed in § 60.132 as follows:
(1) Method 5 for the concentration
of paniculate matter and the associat-
ed moisture content.
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and volu-
metric flow rate, and
(4) Method 3 for gas analysis.
(b) For Method 5, the sampling time
for each run shall be at least 120 min-
utes and the sampling rate shall be at
least 0.9 dscm/hr (0.53 dscf/min)
except that shorter sampling times,
when necessitated by process variables
or other factors, may be approved by
the Administrator. Particulate matter
sampling shall be conducted during
representative periods of charging and
refining, but not during pouring of the
heat.
(Sec. 114. Clean
U.S.C. 7414 ))68.83
Air Act as amended (42
§ 60.132 Standard for particulate matter.
(a) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall discharge or
cause the discharge into the atmos-
phere from a reverberatory furnace
any gases which:
(1) Contain particulate matter in
excess of 50 mg/dscm (0.022 gr/dscf).
(2) Exhibit 20 percent opacity or
greater.
(b) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall discharge or
cause the discharge into the atmos-
phere from any blast (cupola) or elec-
tric furnace any gases which exhibit
10 percent opacity or greater.18
Proposed/effective
38 FR 15406, 6/11/73
Promulgated
39 FR 9308, 3/8/74 (5)
Revised
40 FR 46250, 10/6/75 (18)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-53
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Subpart N—Standards of Performance for
Iron and Steel Plants 5
§60.140 Applicability and designation
of affected facility. 6 4
(a) The affected facility to which the
provisions of this subpart apply Is each
basic oxygen process furnace.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after June 11, 1973,
to subject to the requirements of this
subpart.
§ 60.141 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
(a) "Basic oxygen process furnace"
(BOPF) means any furnace producing
steel by charging scrap steel, hot metal,
and flux materials into a vessel arid in-
troducing a high volume of an oxygen-
rich gas.
(b) "Steel production cycle" means
the operations required to produce each
batch of steel and includes the following
majot functions: Scrap charging, pre-
heating (when used), hot metal charg-
ing, primary oxygen blowing, additional
oxygen blowing (when used), and tap-
ping.
(c) "Startup means the setting into
operation for the first steel production
cycle of a relined BOPF or a BOPP
which has been out of production for a
minimum continuous time period of
eight hours.88
§ 60.142 Standard for parliculute mat-
ter.
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall discharge or cause
the discharge into the atmosphere from
any affected facility any gases which:
(1) Contain participate matter in ex-
cess of 50 mg/dscm (0.022 gr/dscf).
(2) Exit from a control device and
exhibit 10 percent opacity or greater,
except that an opacity of greater than
10 percent but less than 20 percent
jnay occur once per steel production
cycle.88
S 60.143 Monitoring of operations.88
(a) The owner or operator of an af-
fected facility shall maintain a single
time-measuring instrument which
shall be used in recording daily the
time and duration of each steel pro-
duction cycle, and the time and dura-
tion of any diversion of exhaust gases
from the main stack servicing the
BOPF.
(b) The owner or operator of any af-
fected facility that uses venturi scrub-
ber emission control equipment shall
install, calibrate, maintain, and con-
tinuously operate monitoring devices
as follows:
(DA monitoring device for the con-
tinuous measurement of the pressure
loss through the venturi constriction
of the control equipment. The moni-
toring device is to be certified by the
manufacturer to be accurate within
±250 Pa (±1 inch water).
(2) A monitoring device for the con-
tinous measurement of the water
supply pressure to the control equip-
ment. The monitoring device is to be
certified by the manufacturer to be ac-
curate within ±5 percent of the design
water supply pressure. The monitoring
device's pressure sensor or pressure
tap must be located close to the water
discharge point. The Administrator
may be consulted for approval of alter-
native locations for the pressure
sensor or tap.
(3) All monitoring devices shall be
synchronized each day with the time
measuring instrument used under
paragraph (a) of this section. The
chart recorder error directly after syn-
chronization shall not exceed 0.08 cm
(fcsinch).
(4) All monitoring devices shall use
chart recorders which are operated at
a minimum chart speed of 3.8 cm/hr
(1.5 in/hr).
(5) All monitoring devices are to be
recalibreated annually, and at other
times as the Administrator may re-
quire. In accordance with the proce-
duces under § 60.13(b)(3).
(c) Any owner or operator subject to
requirements under paragraph (b) of
this section shall report for each cal-
endar quarter all measurements over
any three-hour period that average
more than 10 percent below the aver-
age levels maintained during the most
recent performance test conducted
under § 60.8 in which the affected fa-
cility demonstrated compliance with
the standard under §60.142(a)(l). The
accuracy of the respective measure-
ments, not to exceed the values speci-
fied in paragraphs (b)(l) and (b)(2) of
this section, may be taken into consid-
eration when determining the mea-
surement results that must be report-
ed.
§ 60.144 Test methods and procedures.
(a) The reference methods appended
to this part, except as provided for in
§60.8(b), shall be used to determine
compliance with the standards prescribed
in § 60.142 as follows:
(1) Method 5 for concentration of
particulate matter and associated mois-
ture content,
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for volumetric flow rate.
and
(4) Method 3 for gas analysis.
(5) Method 9 for visible emissions.
For the purpose of this subpart, opac-
ity observations taken at 15-second in-
tervals immediately before and after a
diversion of exhaust gases from the!
stack may be considered to be consecu-
tive for the purpose of computing an
average opacity for a six-minute
period. Observations taken during a di-
version shall not be used in determin-
ing compliance with the opacity stan-
dard.88
(b) For Method 5, the sampling for
each run shall continue for an integral
number of cycles with total duration of
at least 60 minutes. The sampling rate
shall be at least 0.9 dscm/hr (0.53 dscf/
mln) except that shorter sampling times,
when necessitated by process variables
or other factors, may be approved by the
Administrator. A cycle shall start at the
beginning of either the scrap preheat
or the oxygen blow and shall terminate
immediately prior to tapping.
(c) Sampling of flue gases during
each steel production cycle shall be
discontinued whenever all flue gases
are diverted from the stack and shall
be resumed after each diversion
period.88
Proposed/effecti ve
38 FR 15406, 6/11/73
Promulgated
39 FR 9308, 3/8/74 (5)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83) '
43 FR 15600, 4/13/78 (88)'
111-54
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Subpart O—Standards otf Performance for
Sewago Treatment Plants 5
§ 60.150 Applicability end designation
of affected facility. 75
(a) The affected facility Is each In-
cinerator that combusts wastes contain-
ing more than 10 percent sewage sludge
(dry basis) produced by municipal sew-
age treatment plants, or each incinerator
that charges more than 1000 kg (2205
Ib) per day municipal sewage sludge (dry
basis).
Xb> Any facility under paragraph (a)
of this section that commences construc-
tion or modification after June 11, 1973,
is subject to the requirements of this
subpart.
§ 60.151
As used in this subpart,-all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
§aam«2awll fas- jpartncrnlale small-
Her.
(a) On and after the date on which the
performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator of any sewage sludge incin-
erator subject to the provisions of this
subpart shall discharge or cause the dis-
charge into the atmosphere of:
(1) Particulate matter at a rate in ex-
cess of 0.65 g/kg dry sludge input (1.30
Ib/ton dry sludge input).
(2) Any gases which exihibit 20 per-
cent opacity or greater. '8
| 60.153 Monitoring of operations/
(a) The owner or operator of any
sludge incinerator subject to the provi-
sions of this subpart shall:
(1) Install, calibrate, maintain, and
operate a flow measuring device which
can be used to determine either the mass
or volume of sludge charged to the in-
cinerator. The flow measuring device
shall have 'an accuracy of ±5 percent
over its operating range.
(2) Provide access to the sludge
charged so that a well mixed representa-
tive grab sample of the sludge can be ob-
tained.
(3) Install, calibrate, maintain, and
operate a weighing device for determin-
ing the mass of any municipal solid
waste charged to the incinerator when
sewage sludge and municipal solid waste
are incinerated together. The weighing
device shall have an accuracy of ±5 per-
cent over its operating range.
(Sac. 114. Clean Air Act la amended (42
U.S.C. 7, shall be used to determine
compliance with the standards pre-
scribed in § 60.152 as follows:
(1) Method 5 for concentration of
particulate matter and associated mois-
ture content,
<2> Method 1 for sample and velocity
traverses,
(3) Method 2 for volumetric flow rate,
and
(4) Method 3 for gas analysis.
(b) For Method 5, the sampling time
for each run shall be at least 60 min-
utes and the sampling rate shall be at
least 0.015 dscm/min (0.53 dscf/min),
except that shorter sampling times,
when necessitated by process variables
or other factors, may be approved by the
Administrator.
).
Sv=sludge charged to the Incinerator during the run, m> (English units: gal).
T=duratlon of run, mln (English units: mln).
aoxiO-J=metrtc units conversion factor, l-kg-mln/m8-mg-hr.,
8.021=Engllsh units conversion factor, ff-mln/gal-hr. °
(ii) If the mass of sludge charged U used:
(60)
KDMSM
(Metric or English Units)
whoro:
So=average dry sludge charging rate during the run, kg/hr (English units: Ib/hr).
RoM=average ratio of quantity of dry sludge to quantity of sludge charged to the incinerator, rag/rag (English
units: Ib/lb).
SM=sludge charged during the run, kg (English units: Ib).
T=duration of run, mln (Metric or English units). 6
60=conversion factor, mln/hr (Metric or English units).
(d) Particulate emission rate shall be determined by:
where:
C.Q, (Metric or English Units)
C.0== particulate matter mass emissions, mg/hr (English units: Ib/hr). 7
C.=particulate matter concentration, mg/m< (English units: Ib/dscf).
Q.=volumetric stack gas flow rate, dscm/hr (English units: dscf/br). Q< and C, shall be determined using Method]
2 and 6, respectively.
(e) Compliance with g 60.152(a) shall be determined as follows:
* - (Metric Units)
or
uhoro:
Cd.-=
10-»=
2000=
Cj.=(2000)i^ (English Units)
DO
particulate emission discharge, g/kg dry sludge (English units: Ib/ton dry sludge).
Metric conversion factor, g/mg.
English conversion factor, Ib/ton.
(Sec. 114. Clean Air Act to amended (42
U.S.C. 7414».68.83
Proposed/effective
38 FR 15406, 6/11/73
Promdlgated
39 FR 9308, 3/8/74 (5)
Revised
39 FR 13776,
39 FR 15396,
40 FR 46250,
42 FR 37936,
42 FR 41424,
42 FR 58520,
43 FR 8800,
4/17/74 (6)
5/3/74 (7)
10/6/75 (18)
7/25/77 (64)
8/17/77 (68)
11/10/77 (75)
3/3/78 (83)
111-55
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Subpart P—Standards of Performance for
Primary Copper Smelters 26
160.160 Applicability and designation
of affected facility. «4
(a) The provisions of this subpart are
aplicable to the following affected facili-
ties in primary copper smelters: dryer,
roaster, smelting furnace, and copper
converter.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after October 16.
1974, is subject to the requirements of
this subpart.
§60.161 Definition*.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart
A of this part.
(a) "Primary copper smelter" means
any installation or any intermediate
process engaged in the production of
copper from copper sulfide ore concen-
trates through the use of pyrometallurgl-
cal techniques.
(b) "Dryer" means any facility in
which a copper sulfide ore concentrate
charge is heated in the presence of air
to eliminate a portion of the moisture
from the charge, provided less than 5
percent of the sulfur contained in the
charge is eliminated in the facility.
(c) "Roaster" means any facility in
which a copper sulfide ore concentrate
charge Is heated in the presence of air
to eliminate a significant portion (5 per-
cent or more) of the sulfur contained
in the charge.
(d) "Calcine" means the solid mate-
rials produced by a roaster.
(e) "Smelting" means processing
techniques for the melting of a copper
sulfide ore concentrate or calcine charge
leading to the formation of separate lay-
ers of molten slag, molten copper, and/or
copper matte.
(f) "Smelting furnace" means any
vessel in which the smelting of copper
sulfide ore concentrates or calcines is
performed and in which the heat neces-
sary for smelting is provided by an elec-
tric current, rapid oxidation of a portion
of the sulfur contained in the concen-
trate as it passes through an oxidizing
atmosphere, or the combustion of a fossil
fuel.
(g) "Copper converter" means any
vessel to which copper matte Is charged
and oxidized to copper.
(h) "Sulfuric acid plant" means any
facility producing sulfuric acid by the
contact process.
(i) "Fossil fuel" means natural gas,
petroleum, coal, and any form of solid,
liquid, or gaseous fuel derived from such
materials for the purpose of creating
useful heat.
(j) "Reverberatory smelting furnace"
means any vessel in which the smelting
of copper sulfide ore concentrates or cal-
cines is performed and in which the heat
necessary for smelting is provided pri-
marily by combustion of a fossil fuel.
-------
system installed under paragraph (b) of
this section, exceeds the standard under
I 60.164(a).
(2) Sulfur dioxide. All six-hour periods
during which the average emissions of
sulfur dioxide, as measured by the con-
tinuous monitoring system installed
under I 60.163, exceed the level of the
standard. The Administrator will not
consider emissions in excess of the level
of the standard for less than or equal to
1.5 percent of the six-hour periods dur-
ing the quarter as indicative of a poten-
tial violation of | 60.11 (d) provided the
affected facility, including air pollution
control equipment, is maintained and
operated in a manner consistent with
good air pollution control practice for
minimizing emissions during these pe-
riods. Emissions in excess of the level of
the standard during periods of startup,
shutdown, and malfunction are not to be
included within the 1.5 percent.74
(Sec. 114. Clean Air Act is amended (42
U.S.C. 7414)). 68 83
§ 60.166 Test mclliods and proroilurcs.
(a) The reference methods in Ap-
pendix A to this part, except as provided
for in § 60.8(b), shall be used to deter-
mine compliance with the standards
prescribed In §§ 60.162, 60.163 and
60.164 as follows:
(1) Method 5 for the concentration of
particulate matter and the associated
moisture content.
(2) Sulfur dioxide concentrations shall
be determined using the continuous
monitoring system installed in accord-
ance with § 60.165(b). One 6-hour aver-
ape period shall constitute one run. The
monitoring system drift during any run
shall not exceed 2 percent of span.
(b) For Method 5, Method 1 shall be
used for selecting the sampling site and
the number of traverse points, Method 2
for determining velocity and volumetric
flow rate and Method 3 for determining
the gas analysis. The sampling time for
each run shall be at least 60 minutes and
the minimum sampling volume shall be
0.85 dscm (30 dscf) except that smaller
times or volumes, when necessitated by
process variables or other factors, may
be approved by the Administrator.
(Sec. 114. Clean Air Act li amended (42
U-S.C. 7414)). °8 83
Proposed/effective
39 FR 37040, 10/16/74
Promulgated
41 FR 2331, 1/15/76 (26)
Revised
41 FR 8346, 2/26/76 (30)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
42 FR 57126, 11/1/77 (74)
43 FR 8800, 3/3/78 (83)
ITl-57
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Subpart Q—Standards o? Performance flw
Primary Zinc Smoltsro 2*
Q (MJ.I?(D) AppillneafoSIiBy cuadl
duff affl(3i8©ill (foefflntty.*4
(s) The provisions of tills subpart ISPS
oppllcable to the following affected facili-
ties in primary zinc smelters: roaster and
ointerins machine.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion os modification after October 13,
J07<3, is subject to ®ie requirements of
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any sintering
machine any visible emissions which ex-
hibit greater than 20 percent opacity.
(b) On and after the date on which
the performance test required to be con-
ducted by 8 60.8 is completed, no owner
or operator subject to the provisions of
fchis subpart shall cause to be discharged
Into toe atmosphere from any affected
facility that uses a sulfurlc acid plant to
comply with the standard set forth In
0 SO.173, any visible emissions which ex-
hibit greater than 30 percent opacity.
% 60.171 Definitions.
As used In this subpart, all terms not
defined herein shall have the meaning
given them in the Act and In subpart A
of this part.
(a) "Primary zinc smelter" means any
Installation engaged In the production, or
any Intermediate process in the produc-
tion, of zinc or zinc oxide from zinc sul-
flde ore concentrates through the use
of pyrometallurgical techniques.
(b) "Roaster" means any facility In
which a zinc sulflde ore concentrate
charge Is heated in the presence of air
to eliminate a significant portion (more
than 10 percent) of the sulfur contained
in the charge.
(c) "Sintering machine" means any
furnace In which calcines are heated in
the presence of air to agglomerate the
calcines into a hard porous mass called
"sinter."
. (d) "Sulfuric acid plant" means any
facility producing sulfuric acid by the
contact process.
§ 60.172 Standard for portictilBle mat-
tier.
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 Is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any sintering
machine any gases which contain par-
Uculate matter in excess of 50 mg/dscm
(0.022 gr/dscf).
Q 60.173 Standard for oulfur dioxide.
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any roaster
any gases which contain sulfur dioxide in
excess of 0.065 percent by volume.
(b) Any sintering . machine which
eliminates more than 10 percent of the
sulfur Initially contained In the zinc
sulfide ore concentrates will be consid-
ered as a roaster under paragraph (a)
of (Site section.
0 £0.174 Standard (or vioiUc emisoiona.
(a) On and after the date on which the
performance test required to be con-
(c) For the purpose of reports required
under § 60.7(c), periods of excess emis-
sions that shall be reported are defined
as follows:
(1) Opacity. Any six-minute period
during which the average opacity, os
measured by the continuous monitoring
system Installed under paragraph (a) of
this section, exceeds the standard under
0 80.174(a).
(2) Sulfur dioxide. Any two-hour pe-
riod, as described in paragraph (b) of
this section, during which the average
emissions of sulfur dioxide, as measured
by the continuous monitoring system In-
stalled under paragraph (a) of this sec-
tion, exceeds the standard under g 60.173.
8 fi©.I75 Monitoring of operations.
(a) The owner or operator of any pri-
mary zinc smelter subject to the provi-
sions of this subpart shall Install and
operate:
(1) A continuous monitoring system to
monitor and record the opacity of gases
discharged into the atmosphere from any
sintering machine. The span of this sys-
tem shall be set at 80 to 100 percent
opacity.
(2) A continuous monitoring system to
monitor and record sulfur dioxide emis-
sions discharged Into the atmosphere
from any roaster subject to § 60.173. The
span of this system shall be set at a
sulfur dioxide concentration of 0.20 per-
cent by volume.
(1) The continuous monitoring system
performance evaluation required under
8 60.13(c) shall be completed prior to the
initial performance test required under
8 60.8. During the performance evalua-
tion, the span of the continuous monitor-
ing system may be set at a sulfur dioxide
concentration of 0.15 percent by volume
if necessary to maintain the system out-
put between 20 percent and 90 percent
of full scale. Upon completion of the con-
tinuous monitoring system performance
evaluation, the span of the continuous
monitoring system shall be set at a sulfur
dioxide concentration of 0.20 percent by
volume.
(ii) For the purpose of the continuous
monitoring system performance evalua-
tion required under § 60.13(c), the ref-
erence method referred to under the
Field Test for Accuracy (Relative) in
Performance Specification 2 of Appendix
B to this part shall be Reference Method
6. For the performance evaluation, each
concentration measurement shall be of
one hour duration. The pollutant gas
used to prepare the calibration gas mix-
tures required under paragraph 2.1, Per-
formance Specification 2 of Appendix B,
and for calibration checks under § 60.13
(d), shall be sulfur dioxide.
(b) Two-hour average sulfur dioxide
concentrations shall be calculated and
recorded daily for the twelve consecutive
2-hour periods of each operating day.
Each' two-hour average shall be deter-
mined as the arithmetic mean of the ap-
propriate two contiguous one-hour aver-
age sulfur dioxide concentrations pro-
vided by the continuous monitoring sys-
tem installed under paragraph (a) of
this section.
(Sec. 110. Clean Air Act lo amended «13
U.S.C.
§ 60.176 Teat imcthodo and procedures.
(a) The reference methods in Appen-
dix A to this part, except as provided for
in § 60.8(b), shall be used to determine
compliance with the standards pre-
scribed in |§ 60.172, 60.173 and 60.174 as
follows :
(1) Method 5 for the concentration of
particulate matter and the associated
moisture content.
(2) Sulfur dioxide concentrations shall
be determined using the continuous
monitoring system installed in accord-
ance with 8 60.175(a). One 2-hour aver-
age period shall constitute one run.
(b) For Method 5, Method 1 shall be
used for selecting the sampling site and
the number of traverse points, Method 2
for determining velocity and volumetric
flow rate and Method 3 for determining
the gas analysis. The sampling time for
each run shall be at least 60 minutes and
the minimum sampling volume shall be
0.85 dscm (30 dscf) except that smaller
times or volumes, .when necessitated by
process variables or other factors, may be
approved by the Administrator.
(Sec. 114. Clean Air Act is amended (42
U.S.C. 7414)). 68. 63
Proposed/effective
39 FR 37040, 10/16/74
Promulgated
41 FR 2331, 1/15/76 (26)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-58
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Subpart R—Standards of Performance for
Primary Lead Smelter* "
§60.180 Applicability and designation
of affected facility.*4
(a) The provisions of this subpart are
applicable to the following affected
facilities in primary lead smelters: sin-
tering machine, sintering machine dis-
.charge end, blast furnace, dross rever-
beratory furnace, electric smelting fur-
nace, and converter.
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after October
16. 1974, is subject to the requirements
of this subpart.
g 60.181 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and In subpart A
of this part.
(a) "Primary lead smelter" means any
Installation or any intermediate process
engaged in the production of lead from
lead sulflde ore concentrates through
the use of pyrometallurgical techniques.
(b) "Sintering machine" means any
furnace in which a lead sulflde ore con-
centrate charge is heated in the presence
of air to eliminate sulfur contained in
the charge and to agglomerate the
charge into a hard porous mass called
"sinter."
(c) "Sinter bed" means the lead sulflae
ore concentrate charge within a sinter-
ing machine.
(d) "Sintering machine discharge end"
means any apparatus which receives sin-
ter as It is discharged from the conveying
grate of a sintering machine.
(e) "Blast furnace" means any reduc-
tion furnace to which sinter Is charged
and which forms separate layers of
molten slag and lead bullion.
(f) "Dross reverberatory furnace"
means any furnace used for the removal
or refining of impurities from lead
bullion.
(g) "Electric smelting furnace" means
any furnace in which the heat necessary
for smelting of the lead sulflde ore con-
centrate charge is generated by passing
an electric current through a portion of
the molten mass in the furnace.
(h) "Converter" means any vessel to
which lead concentrate or bullion is
charged and refined.
(D "Sulfuric acid plant" means any
facility producing sulfuric acid by the
contact process.
| 60.182 Standard for paniculate mat-
ter.
(a) On and after the date on which
the performance test required to be con-
ducted by { 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any blast fur-
nace, dross reverberatory furnace, or
sintering machine discharge end any
gases which contain particulate matter
in excess of 59 mg/dscm (0.022 gr/dscf).
§ 60.183 Standard for »ulfur dioxide.
(a) On and after the date on which
the performance test required to be con-
ducted by I 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any sintering
machine, electric smelting furnace, or
converter gases which contain sulfur di-
oxide In excess of 0.065 percent by
volume.
§ 60.184 Standard for visible emissions.
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any blast fur-
nace, dross reverberatory furnace, or
sintering machine discharge end any
visible emissions which exhibit greater
than 20 percent opacity.
(b) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any affected
facility that uses a sulfuric acid plant to
comply with the standard set forth in
{60.183, any visible emissions which
exhibit greater than 20 percent opacity.
| 60.185 Monitoring of operations.
(a) The owner or operator of any
primary lead smelter subject to the pro-
visions of this subpart shall install and
operate:
(1) A continuous monitoring system
to monitor and record the opacity of
gases discharged into the atmosphere
from any blast furnace, dross rever-
beratory furnace, or sintering machine
discharge end. The span of this system
shall be set at 80 to 100 percent opacity.
(2) A continuous monitoring system
to monitor and record sulfur dioxide
emissions discharged into the atmos-
phere from any sintering machine,
electric furnace or converter subject to
§ 60.183. The span of this system shall
be set at a sulfur dioxide concentration
of 0.20 percent by volume.
(1) The continuous monitoring system
performance evaluation required under
§ 60.13(c) shall be completed prior to the
initial performance test required under
§ 60.8. During the performance evalua-
tion, the span of the continuous moni-
toring system may be set at a sulfur
dioxide concentration of 0.15 percent by
volume if necessary to maintain the sys-
tem output between 20 percent and 90
'percent of full scale. Upon completion
of the continuous monitoring system
performance evaluation, the span of the
continuous monitoring system shall be
set at a sulfur dioxide concentration of
0.20 percent by volume.
(ii) For the purpose of the continuous
monitoring system performance evalua-
tion required under § 60.13 (c), the refer-
ence method referred to under the Field
Test for Accuracy (Relative) in Per-
formance Specification 2 of Appendix B
to this part shall be Reference Method
6. For the performance evaluation, each
concentration measurement shall be of
one hour duration. The pollutant gases
used to prepare the calibration gas mix-
tures required under paragraph 2.1, Per-
formance Specification 2 of Appendix B,
and for calibration checks under § 60.13
(d), shall be sulfur dioxide.
(b) Two-hour average sulfur dioxide
concentrations shall be calculated and
recorded daily for the twelve consecu-
tive two-hour periods of each operating
day. Each two-hour average shall be de-
termined as the arithmetic mean of the
appropriate two contiguous one-hour
average sulfur dioxide concentrations
provided by the continuous monitoring
system installed under paragraph (a) of
this section.
(c) For the purpose of reports re-
quired under § 60.7(c), periods of excess
emissions that shall be reported are de-
fined as follows:
(1) Opacity. Any six-minute period
during which the average opacity, as
measured by the continuous monitoring
system installed under paragraph (a) of
this section, exceeds the standard under
§60.184(a).
(2) Sulfur dioxide. Any two-hour pe-
riod, as described in paragraph (b) of
this section, during which the average
emissions of sulfur dioxide, as measured
by the continuous monitoring system in-
stalled under paragraph (a) of this sec-
tion, exceeds the standard under § 60.183.
Act " Mnended <42
§ 60.186 Test methods and procedures.
(a) The reference methods in Appen-
dix A to this part, except as provided for
in § 60.8(b), shall be used to determine
compliance with the standards pre-
scribed in §§ 60.182, 60.183 and 60.184 as
follows:
(1) Method 5 for the concentration
of particulate matter and the associated
moisture content.
(2) Sulfur dioxide concentrations shall
be determined using the continuous
monitoring system installed in accord-
ance with § 60.185(a). One 2-hour aver-
age period shall constitute one run.
(b) For Method 5, Method 1 shall be
used for selecting the sampling site and
the number of traverse points, Method 2
for determining velocity and volumetric
flow rate and Method 3 for determining
the gas analysis. The sampling time for
each run shall be at least 60 minutes and
the minimum sampling volume shall be
0.85 dscm (30 dscf) except that smaller
times or volumes, when necessitated by
process variables or other factors, may be
approved by the Administrator.
(Sec. 114. Cleaji Air Act is amended (42
U.S.C. 7414)). 48. 83
Proposed/effective Revised
39 FR 37040, 10/16/74 4~2 FR 37936, 7/25/77 (6'
Promulgated 42 FR 41424, 8/17/77 (6f
41 FR 2331, 1/15/76 (26)43 FR 8800, 3/3/78 (83)
111-59
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Subpart §=Standards of l?erformane®
tor Primary Aluminum Reduction
Authority: Sections 111 and 301 (a) of the
Clean Air Act as amended (42 U.S.C. 7411.
7601 (a)), and additional authority as noted
below.
§ 80.160 AppMeability ana assignation of
affected facility.64
(a) The affected facilities in'primary
aluminum reduction plants to which this
subpart applies are potroom groups and
anode bake plants.11*
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after October
33, 1974, is subject to the requirements
of this subpart.
114
§60.101
As used in this subpart. all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
"Aluminum equivalent" means an
amount of aluminum which can be
produced from a Mg of anodes produced
by an anode bake plant as determined
by i eo.l95(g).
"Anode bake plant" means a facility
which produces carbon anodes for use
in a primary aluminum reduction plant.
"Potroom" means a building unit
which houses a group of electrolytic
cells in which aluminum is produced.
"Potroom group" means an
uncontrolled potroom: a potroom which
is controlled individually, or a group of
potrooms or potroom segments ducted to
a common control system.
"Primary aluminum reduction plant"
means any facility manufacturing
aluminum by electrolytic reduction.
"Primary control system" means an
air pollution control system designed to
remove gaseous and.particulate
flourides from exhaust gases which are
captured at the cell.
"Roof monitor" means that portion of
the roof of a potroom where gases not
captured at the cell exit from the
potroom.
"Total fluorides" means elemental
fluorine and all fluoride compounds as
measured by reference methods
specified in | 60.195 or by equivalent or
alternative methods (see § 60.8(b)).
§ 60. 1 82 Standards for fluorides.1 M
(a) On and after the date on which the
initial performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere from
any affected facility any gases
containing total fluorides, as measured
according to i 60.8 above, in excess of:
(1) 1.0 kg/Mg (2.0 Ib/ton) of aluminum
produced for potroom groups at
Soderberg plants: except that emissions
between 1.0 kg/Mg and 1.3 kg/Mg (2.6
Ib/ton) will be considered in compliance
if the owner or operator demonstrates
that exemplary operation and
maintenance procedures were used with
respect to the emission control system
and that proper control equipment was
operating at the affected facility during
the performance tests:
(2) 0.95 kg/Mg (1.9 Ib/ton) of
aluminum produced for potroom groups
at prebake plants; except that emissions
between 0.95 kg/Mg and 1.25 kg/Mg (2.5
Ib/ton) will be considered in compliance
if the owner or operator demonstrates
that exemplary operation and
maintenance procedures were used with
respect to the emission control system
and that proper control equipment was
operating at the affected facility during
the performance test: and
(3) 0.05 kg/Mg (0.1 Ib/ton) of
aluminum equivalent for anode bake
plants.
(b) Within 30 days of any performance
test which reveals emissions which fall
between the 1.0 kg/Mg and 1.3 kg/Mg
levels in paragraph (a)(l) of this section
or between the 0.95 kg/Mg and 1.25 kg/
Mg levels in paragraph (a)(2) of this
section, the owner or operator shall
submit a report indicating whether all
necessary control devices were on-line
and operating properly during the
performance test, describing the
operating and maintenance procedures
followed, and setting forth any
explanation for the excess emissions, to
the Director of the Enforcement Division
of the appropriate EPA Regional Office.
§ SO. 193 Standard Sor visible emissions."4
(a) On and after the date on which the
performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere:
(1) From any potroom group any gases
which exhibit 10 percent opacity or
greater, or
(2) From any anode bake plant any
gases which exhibit 20 percent opacity
or greater.
§ 60.194 Monitoring of operations.114
(a) The owner or operator of any
affected facility subject to the provisions
of this subpart shall install, calibrate.
maintain, and operate monitoring
devices which can be ised to determine
daily the weight of aluminum and anode
produced. The weighing devices shall
have an accuracy of ± 5 percent over
their operating range.
(b) The owner or operator of any-
affected facility shall maintain a record
of daily production rates of aluminum
and anodes, raw material feed rates.
and cell or potline voltages.
(Section 114 of the Clean Air Act as amended
(42 U.S.C. 7414))
§ SO. 195 7
-------
(2) For sampling emissions from roof
monitors not employing stacks or
pollutant collection systems:
(i) Method 1 for sample and velocity
traverses.
(ii) Method 2 and Method 14 for
velocity and volumetric flow rate.
(iii) Method 3 for gas analysis, and
(iv) Method 14 for the concentration of
total fluorides and associated moisture
content.
(3) For sampling emissions from roof
monitors not employing stacks but
equipped with pollutant collection
systems, the procedures under § 60.8(b)
shall be followed. .
(d) For Method 13A or 13B. the
sampling time for each run shall be at
least 8 hours for any potroom sample
and at least 4 hours for any anode bake
plant sample, and the minimum sample
volume shall be 6.8 dscm (240 dscf) for
any potroom sample and 3.4 dscm (120
dscf) for any anode bake plant sample
except that shorter sampling times or
smaller volumes, when necessitated by
process variables or other factors, may
be approved by the Administrator.
(e) The air pollution control system for
each affected facility shall be
constructed so that volumetric flow
rates and total fluoride emissions can be
accurately determined using applicable
methods specified under paragraph (c)
of this section.
(f) The rate of aluminum production is
determined by dividing 720 hours into
the weight of aluminum tapped from the
affected facility during a period of 30
days prior to and including the final run
of a performance test.
(g) For anode bake plants, the
aluminum equivalent for anodes
produced shall be determined as
follows:
(1) Determine the average weight (Mg)
of anode produced in anode bake plant
during a representative oven cycle using
•=i monitoring device which meets the
requirements of § 60.194(a).
(2) Determine the average rate of
anode production by dividing the total
weight of anodes produced during the
representative oven cycle by the length
of the cycle in hours.
(3) Calculate the aluminum equivalent
for anodes produced by multiplying the
average rate of anode production by
two. (Note: An owner or operator may
establish a different multiplication
factor by submitting production records
of the Mg of aluminum produced and the
concurrent Mg of anode consumed by
potrooms.)
(h) For each run, potroom group
emissions expressed in kg/Mg of
aluminum produced shall be determined
using the following equation:
(CsOsMO'-ttCsOsliKT*
Epg-
M
Where:
Epg = potroom group emissions of total
fluorides in kg/Mg of aluminum
produced.
Cs = concentration of total fluorides in mg/
dscm as determined by'Method 13A or
13B, or by Method 14. as applicable.
Qs = volumetric flow rate of the effluent
gas stream in dscm/hr as determined by
Method 2 and/or Method 14, as
applicable.
10 ~6= con version factor from mg to kg.
M = rate of aluminum production in Mg/hr
as determined by § 60.195(f).
(CsQs), = product of Cs and Qs for
measurements of primary control system
effluent gas streams.
(CsQs)> = product of Cs and Qs for
measurements of secondary control
system or roof monitor effluent gas
streams.
Where an alternative testing requirement has
been established for the primary control
system, the calculated value (CsQs) , from
the most recent performance test will be
used.
(i) For each run, as applicable, anode
bake plant emissions expressed in kg/
Mg of aluminum equivalent shall be
determined using the following equation:
Ebp=
CsOs 10
Where:
Ebp = anode bake plant emissions of total
fluorides in kg/Mg of aluminum
equivalent.
Cs = concentration of total fluorides in
mg/dscm as determined by Method 13A
or 13B.
Qs = volumetric flow rate of the effluent
gas stream in dscm/hr as determined by
Method 2.
10 "• = conversion factor from mg to kg.
Me = aluminum equivalent for anodes
produced by anode bake plants in Mg/hr
as determined by § 60.195(g).
(Section 114 of the Clean Air Act as* amended
(42 U.S.C. 7414))
Proposed/effecti ve
39 FR 37730, 10/23/74
Promulgated
41 FR 3825, 1/26/76 (27)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
45 FR 44202, 6/30/80 (114)
46 FR 61125, 12/15/81 (134)
111-61
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Subpart T—Standards of Performance for
the Phosphate Fertilizer Industry: Wet-
Process Phosphoric Acid Plants "
160.200 Applicability and designation
of affected facility. 64
(a) The affected facility to which the
provisions of this subpart apply is each
wet-process phosphoric acid plant. For
the purpose of this subpart, the affected
facility includes any combination of:
reactors, filters, evaporators, and hot-
wells.
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after October
22, 1974, is subject to the requirements
of this subpart.
§ 60.201 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them In the Act and in Subpart A
of this part.
(a) "Wet-process phosphoric acid
plant" means any facility manufactur-
ing phosphoric acid by reacting phos-
phate rock and acid.
(b) "Total fluorides" means elemental
fluorine and all fluoride compounds as
measured by reference methods specified
in § 60.204, or equivalent or alternative
methods.
(c) "Equivalent PZO. feed" means the
quantity of phosphorus, expressed as
phosphorous pentoxide, fed to the proc-
ess.
§ 60.202 Standard for fluorides.
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any affected
facility any gases which contain total
fluorides In excess of 10.0 g/metric ton
of equivalent P:O5 feed (0.020 Ib/ton).
§ 60.203 Monitoring of operations.
(a) The owner or operator of any wet-
process phosphoric acid plant subject to
the provisions of this subpart shall in-
stall, calibrate, maintain, and operate a
monitoring device which can be used to
determine the mass flow of phosphorus-
bearing feed material to the process. The
monitoring device shall have an accu-
racy of ±5 percent over its operating
range.
(b) The owner or operator of any wet-
process phosphoric acid plant shall
maintain a daily record of equivalent
P,OS feed by first determining the total
mass rate in metric ton/hr of phosphorus
bearing feed using a monitoring device
for measuring mass flowrate which meets
the requirements of paragraph (a) of
this section and then by proceeding ac-
cording to § 60.204(d) (2).
(c) The owner or operator of any wet-
process phosphoric acid subject to the
provisions of this part shall install, cali-
brate, maintain, and operate a monitor-
ing device which continuously measures
and permanently records the total pres-
sure drop across the process scrubbing
system. The monitoring device shall have
an accuracy of ±5 percent over Its op-
erating range.
(Sec. 114. Clean Air Act I* amended (42
U.S.C. 7414».68'83
§ 60.204 Test methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided in § 60.8
(b), shall be used to determine compli-
ance with the standard prescribed hi
S 60.202 as follows:
(1) Method 13A or 13B for the concen-
tration of total fluorides and the asso-
ciated moisture content,
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and vol-
umetric flow rate, and
(4) Method 3 for gas analysis.
(b) For Method 13A or 13B, the sam-
pling time for each run shall be at least
60 minutes and the minimum sample
volume shall be 0.85 dscm (30 dscf) ex-
cept that shorter sampling times or
smaller volumes, when necessitated by
process variables or other factors, may
be approved by the Administrator.
(c) The air pollution control system
for the affected facility shall be con-
structed so that volumetric flow rates
and total fluoride emissions can be ac-
curately determined by applicable test
methods and procedures.
(d) Equivalent P,O« feed shall be de-
termined as follows:
(1) Determine the total mass rate In
metric ton/hr of phosphorus-bearing
feed during each run using a flow
monitoring device meeting the require-
ments of § 60.203(a).
(2) Calculate the equivalent P-On feed
by multiplying the percentage PiO» con-
tent, as measured by the spectrophoto-
metric molybdovanadophosphate method
(AOAC Method 9), times the total mass
rate of phosphorus-bearing feed. AOAC
Method 9 is published in the Official
Methods of Analysis of the Association
of Official Analytical Chemists, llth edi-
tion, 1970, pp. 11-12. Other methods may
be approved by the Administrator.
(e) For each run, emissions expressed
in g/metric ton of equivalent P-jO, feed
shall be determined using the following
equation:
„ «?.s feed In metric
ton/hr as determined by I 60.-
204(d).
(Sec. 114. Clean Air Act to amended (
UJS.C. 7414».68-83
where:
E=Emissions of total fluorides In g/
metric ton of equivalent P2O,
feed.
C,=Concentration of total fluorides In
mg/dscm as determined by
Method ISA or 13B.
Q,=Volume trio flow rate of the effluent
gas stream In dscm/hr as deter-
mined by Method 2.
10-«=Conversion factor for mg to g.
Proposed/effective
39 FR 37602, 10/22/74
Promulgated
40 FR 33152, 8/6/75 (14)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-62
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Subpart U—Standards of Performance for
the Phosphate Fertilizer Industry: Super-
phosphoric Acid Plants M
§ 60.210 Applicability and designation
of affected facility.64
(a) The affected facility to which the
provisions of this subpart apply is each
superphosphoric acid plant. For the
purpose of this subpart, the affected
facility includes any combination of:
evaporators, hot wells, acid sumps, and
cooling tanks.
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after October
22, 1974, is subject to the requirements
of this suboart.
§60.211 Definitions.
As used in this subpart, all terms not
denned herein shall have the meaning
given them in the Act and in subpart A
of this part.
(a) "Superphosphoric acid plant"
means any facility which concentrates
wet-process phosphoric acid to 66 per-
cent or greater PjOB content by weight
for eventual consumption .as a fertilizer.
(b) "Total fluorides" means elemen-
tal fluorine and all fluoride compounds
as measured by reference methods spe-
cified in § 60.21,4, or equivalent or alter-
native methods.
(c) "Equivalent P2OS feed" means the
quantity of phosphorus, expressed as
phosphorous pentoxide, fed to the
process.
f 60.212 Standard for fluorides.
(a) On and after the date on which
the performance test required to be con-
ducted by I 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any affected
facility any gases which contain total
fluorides in excess of 5.0 g/metric ton of
equivalent PiOB feed (0.010 Ib/ton).
f 60.213 Monitoring of operations.
(a) The owner or operator of any
superphosphoric acid plant subject to
the provisions of this subpart shall in-
stall, calibrate, maintain, and operate
a flow monitoring device which can be
used to determine the mass flow of
phosphorus-bearing feed material to the
process. The flow monitoring device shall
have an accuracy of ± 5 percent over its
operating range.
(b) The owner or operator of any
superphosphoric acid plant shall main-
tain a daily record of equivalent P£>>
feed by first determining the total mass
rate in metric ton/hr of phosphorus-
bearing feed using a flow monitoring, de-
vice meeting the requirements of para-
graph (a) of this section and then by
proceeding according to 8 60.214(d) (2).
(c) The owner or operator of any
superphosphoric acid plant subject to the
provisions of this part shall install, cali-
brate, maintain, and operate a monitor-
Ing device which continuously measures
and permanently records the total pres •
sure drop across the process scrubbing
system. The monitoring device shall have
.an accuracy of ± 5 percent over its
operating range.
(Sec. 114. Clean Air Act U amended (42
U.S.C. 7414)).68'83
§ 60.214 Test methods and procedures.
(a^ Reference methods in Appendix
A of this part, except as provided In
8 60.8(b), shall be used to determine
compliance with the standard prescribed
In i 60.212 as follows:
(1) Method ISA or 13B for the concen-
tration of total fluorides and the asso-
ciated moisture content.
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and volu-
metric flow rate, and
(4) Method 3 for gas analysis.
(b) For Method ISA or 138, the sam-
pling time for each run shall be at least
60 minutes and the minimum sample
volume shall be at least 0.85 dscm (30
dscf) except that shorter sampling times
or smaller volumes, when necessitated by
process variables or other factors, may
be approved by the Administrator.
(c) The air pollution control system
for the affected facility shall be con-
structed so that volumetric flow rates and
total fluoride emissions can be accurately
determined by applicable test methods
and procedures.
(d) Equivalent P^Os feed shall be deter-
mined as follows:
(1) Determine the total mass rate in
metric ton/hr of phosphorus-bearing
feed during each run using a flow moni-
toring device meeting the requirements
of § 60.213(a).
(2) Calculate the equivalent P»O; feed
by multiplying the percentage PzOj con-
tent, as measured by the spectrophoto-
metric molybdovanadophosphate method
(AOAC Method 9), times the total mass
rate of phosphorus-rbearing feed. AOAC
Method 9 is published in the Official
Methods of Analysis of the Association of
Official Analytical Chemists, llth edition,
1970, pp. 11-12. Other methods may be
approved by the Administrator.
(e) For each run, emissions expressed
to g/metric ton of equivalent P:OS feed,
•hall be determined using the following
equation:
,-, (C.Q.) 10-'
where:
E = Emissions of total fluorides In g/
metric ton of equivalent JP.O;
feed.
C, — Concentration of total fluorides In
mg/dscm as determined by
Method ISA or 13B.
Q, = Volumetric flow rate of the effluent
gas stream 'in dscm/hr as deter-
mined by Method 2.
10-3=Con version factor for mg to g.
Jfiy>;= Equivalent ff>^ feed In metric
ton/hr as determined by \ 60.-
314(d).
(Sec. 114. Clean Air Act U amended (42
U.S.C. 7414)). 48, 83
Proposed/effective
39 FR 37602, 10/22/74
Promulgated
40 FR 33152, 8/6/75 (14)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-63
-------
Subpart V—Standards of Performance for
the Phosphate Fertilizer Industry: Diam-
monium Phosphate Plants '4
§ 60.220 Applicability and designation
of affected facility. »4
(a) The affected facility to which the
provisions of this subpart apply is each
granular drammonium phosphate plant.
For the purpose of this subpart, the af-
fected facility Includes any combination
of: reactors, granulators. dryers, coolers,
screens, and mills.
(b> Any facility under paragraph (a)
of this section that commences construc-
tion or modification after October 22,
197t, is subject to the requirements of
this subpart.
§ 60.221 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
(a) "Granular diammonium phos-
phate plant" - means any plant manu-
facturing granular diammonium phos-
phate by reacting phosphoric acid with
ammonia.
(b) "Total fluorides" means elemental
fluorine and all fluoride compounds as
measured by reference methods speci-
fied in I 60.224, or equivalent or alter-
native methods.
(c) "Equivalent P2O5 feed" means the
quantity of phosphorus, expressed as
phosphorous pentoxide, fed to the proc-
ess. .
f 60.222 Standard for fluorides.
(a) On and after the date on which
the performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
Into the atmosphere from any affected
facility any gases which contain total
fluorides in excess of 30 g/metric ton of
•quivalent P.-Os feed (0.060 Ib/ton).
f 60.223 Monitoring of operations.
(a) The.owner or operator of any
granular diammonium phosphate plant
subject to the provisions of this subpart
shall install, calibrate, maintain, and
operate a flow monitoring device which
can be used to determine the mass flow
of phosphorus-bearing feed material to
the process. The flow monitoring device
shall have an accuracy of ±5 percent
over its operating range.
(b) The owner or operator of any
granular diammonium phosphate plant
shall maintain a daily record of equiv-
alent P2Oj feed by first determining the
total mass rate in metric ton/hr of phos-
phorus-bearing feed using a flow moni-
toring device meeting the requirements
of paragraph (a) of this section and then
by proceeding according to I 60.224(d)
.(2).
(c) The owner or operator of any
granular diammonium phosphate plant
subject to the provisions of this part shall
install, calibrate, maintain, and operate
a monitoring device which continuously
measures and permanently records the
total pressure drop across the scrubbing
system. The monitoring device shall have
•n accuracy of ±5 percent over its op-
erating range.
(Sec. 114. Clean Air Act to amended (42
U.S.C. 7414)).68'83
§ 60.224 Test methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided for in
I 60.8 (b), shall be used to determine com-
pliance with the standard prescribed in
f 60.222 as follows:
. (1) Method ISA or 13B for the con-
centration of total fluorides and the as-
sociated moisture content,
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and volu-
metric flow rate, and
(4) Method 3 for gas analysis.
(b) For Method ISA or 13B, the
sampling time for each run shall be at
least 60 minutes and the minimum
sample volume shall be at least 0.85 dscm
(30 dscf) except that shorter sampling
times or'smaller volumes when, neces-
sitated by process variables or other
factors, may be approved by the Ad-
ministrator.
(c) The air pollution control system
for the affected facility shall be con-
structed so that volumetric flow rates
and total fluoride emissions can be ac-
curately determined by applicable test
methods and procedures.
(d) Equivalent P20, feed shall be de-
termined as follows:
(1) Determine the total mass rate in
metric ton/hr of phosphorus-bearing
feed during each run using a flow moni-
toring device meeting the requirements
of §60.223(a).
(2) Calculate the equivalent PsO, feed
by multiplying the percentage Pad con-
tent, as measured by the spectrophoto-
metric molybdovanadophosphate method
(AOAC Method 9), times the total mass
rate of phosphorus-bearing feed. AOAC
Method 9 is published in the Official
Methods of Analysis of the Association
of Official Analytical Chemists, llth edi-
tion, 1970, pp. 11-12. Other methods may
be approved by the Administrator.
(e) For each run, emissions expressed
In g/metric ton of equivalent P»0f feed
shall be determined using the following
equation:
„ (C.Q.) 10-'
M rto,= Equivalent P,O, feed In metric
ton/hr a* determined by 1 60.-
(Sec. 114. Clean Air Act U amended (42
U.S.C. 7414)).
where:
E=Emissions of total fluorides in g/
metric ton at equivalent P,O,.
C( = Concentration of total fluorides In
mg/dscm as determined by
Method 13A or 13B,
-------
Subpart W—Standards o? Performance) tfor
the Phosphate Fertilizer industry: Triple
Superphosphate Plants M
§ 60.230 Applicability and designation!
of affrcted facility.64
(ai The affected facility to which the
provisions of this subpart apply Is each
triple superphosphate plant. For the pur-
pose of this subpart, the affected facility
includes any combination of: mixers,
curing belts (dens), reactors, granula-
tors, dryers, cookers, screens, mills, and
facilities which store run-of-pile triple
superphosphate.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after October 22.
1974, is subject to the requiremente of
this subpart.
In metric ton/hr of phosphorus-bearing
feed using a now monitoring device meet-
ing the requirements of paragraph (a)
of this (section ond then by proceeding
according to 0 S0.234(d) (2).
(c) The owner or operator of any triple
superphosphate plant subject to the pro=
visions of this part shall install, calibrate,
maintain, and operate a monitoring de-
vice which continuously measures and
permanently records the total pressure
drop across the process scrubbing system.
The monitoring device shall have an ac-
curacy of ±5 percent over Its operating
range.
(Sec. 114. Clean Air Act is amended (42
U.S.C. 7414)). 68, 83
§ 60.231. Befinitiono.
As used in this subpart, all terms not
denned herein shall have the meaning
given them in the Act and in subpart A
of this part.
(a) "Triple superphosphate plant"
means any facility manufacturing triple
superphosphate by reacting phosphate
rock with phosphoric acid. A rule-of-pile
triple superphosphate plant includes
curing and storing.
(b) "Run-of-pile triple superphos-
phate" means any triple superphosphate
that has not been processed in & granu-
lator and is composed of particles at
least 25 percent by weight of which
(when not caked) will pass through a J8
mesh screen,
(c) "Total fluorides" means ele-
mental fluorine and all fluoride com-
pounds as measured by reference
methods specified in § 60.234, or equiva-
lent or alternative methods.
(d) "Equivalent P,O5 feed" means the
quantity of phosphorus, expressed sss
phosphorus pentoxide, fed to the process.
| 6®.232 Standard fop flnorides.
(a) On and after the date on which the
performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any affected
facility any gases which contain total
fluorides in excess of 100 g/metric ton of
equivalent PjO, feed (0.20 Ib/ton).
(§ (£0.233 Moraitoinng oS OjjteFoliona.
(a) The owner or operator of any triple
superphosphate plant subject to the pro-
visions of this subpart shall install, cali-
brate, maintain, and operate a flow moni-
toring device which can be used to deter-
mine the mass flow of phosphorus-bear-
ing feed material to the process. The flow
monitoring device shall have an accuracy
of ±5 percent over its operating range.
(b) The owner or operator of any
triple superphosphate plant shall main-
tain a daily record of equivalent P>OB feed
by first determining the total mass rate
C0 = Concentration of total Suortdea la
ms/dacm as determined by
" Method 13A or 13B.
^z Volumetric flow rate of the effluent
gas stream la dscm/hr os deter-
mined by Method 3.
10-"= Conversion /actor for mg to g.
if,P,O.=Equivalent pao, feed In metric
ton/hr co determined by D 80.-
234(d).
(Sec. 114. Clean Air Act Is amended (42
U.S.C. 7414)).68. 83
g 60.234 Test methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided for in
§ 60.8 Method 3 for gas analysis.
(b) For Method 13A or 13B, the sam=
pling time for each run shall be at least
60 minutes and the -minimum sample
volume shall be at least 0.85 dscm (30
dscf ) except that shorter sampling times
or smaller volumes, when necessitated by
process variables or other factors, may
be approved by the Administrator.
(c) The ah* pollution control system
for the affected facility shall be con-
structed so that volumetric flow rates
and total 'fluoride emissions can be ac-
curately determined by applicable test
methods and procedures.
(d) Equivalent P,O» feed shall be deter-
mined as follows:
(1) Determine the total mass rate in
metric ton/hr of phosphorus-bearing
feed during each run using a flow moni-
toring device meeting the requirements
of § 60.233 (a).
(2) Calculate the equivalent P=O8 feed
by multiplying the percentage PaO0 con-
tent, as measured by the spectrophoto-
metric molybdovanadophosphate method
(AOAC Method 9), tiroes the total mass
rate of phosphorus-bearing feed. AOAC
Method 9 is published in the Official
Methods of Analysis of the Association of
Official Analytical Chemists, llth edition,
1970, pp. 11-12. Other methods may be
approved by the Administrator.
(e) For each run, emissions expressed
in g/metric ton of equivalent P.O0 feed
shall be determined using the following
equation:
(C.Q.) 10-°
where:
E= Emissions of total fluorides In g/
metric ton of equivalent PaO.
feed.
Proposed/effective
39 FR 37602, 10/24/74
Promulgated
40 FR 33152, 8/6/75 (14)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
II.I-C.5
-------
Subpart X—Standards of Performance for.
the Phosphate Fertilizer Industry: Gran-
ular Triple Superphosphate Storage Fa-
cilities "<
§60.240 Applicability and designation
of affected facility.<>4
(a) The affected facility to which the
provisions of this subpart apply is each
granular triple superphosphate storage
facility. For ttie purpose of this subpart,
the affected facility includes any combi-
nation of: storage or curing piles, con-
veyors, elevators, screens, and mills.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after October 22,
1974, is subject to the requirements of
this subpart.
§ 60.241 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part
(a) "Granular triple superphosphate
storage facility" means any facility cur-
Ing or storing granular triple superphos-
phate.
(b) "Total fluorides" means elemental
fluorine and all fluoride compounds as
measured by reference methods specified
in S 60.244, or equivalent or alternative
methods.
(c) "Equivalent P=O5 stored" means
the quantity of phosphorus, expressed as
phosphorus pentoxide, being cured or
stored In the affected facility.
(d) "Fresh granular triple superphos-
phate" means granular triple superphos-
phate produced no more than 10 days
prior to the date of the performance lest.
§ 60.242 Standard for fluoride*.
(a) On and after the date on which the
performance test required to be con-
ducted by i 60.8 Is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere from any affected
facility any gases which contain total
fluorides In excess of 0.25 g/hr/metric
ton of equivalent PiO, stored (5.0 z 10-*
Ib/hr/ton of equivalent P,O, stored).
§60.243 Monitoring of operations.
(a) The owner or operator of any
granular triple superphosphate storage
facility subject to the provisions of this
subpart shall maintain an accurate ac-
count of triple superphosphate In storage
to permit the determination of the
amount of equivalent P«O» stored,
(b) The owner or operator of any
granular triple superphosphate storage
facility shall maintain.a daily record of
total equivalent P.O. stored by multiply-
ing the percentage P.O. content, as
determined by § 60.244(f)(2>. times the
total'mass of granular triple superphos-
phate stored.
(c) The owner or operator of any
granular triple superphosphate storage
•facility subject to the provisions of this
part shall install, calibrate, maintain,
and operate a monitoring device which
continuously measures and permanently
.records the total pressure drop across the
process scrubbing sytem. The monitoring
device shall have an accuracy of ±5 per-
cent over its operating range.
(Sec. 114, Clean Air Act is amended (42
U.S.C. 7414 ».*»•83
in g/hr/metric ton of equivalent P-O,
stored shall be determined using the fol-
lowing equation:
(C.Q.) IP''
•§ 60.244 Tert methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided for In
I 60.8(b), shall be used to determine
compliance with the standard prescribed
in § 60.242 as follows:
(l) Method 13A or 13B for the con-
centration of total fluorides and the as-
sociated moisture content,
(2) Method 1 for sample and velocity
traverses,
<3) Method 2 for velocity and volu-
metric flow rate, and
(4) Method 3 for gas analysis.
f the build-
ing capacity.
(2) Fresh granular triple superphos-
phate—at least 20 percent of the amount
of triple superphosphate in the building.
,o,=Equlvalent P,O, feed In metric
tons as measured by i 60.244(d).
(Sec. 114, Clean Air Act Is amended (42
U.S.C. 7414)). 68, 83
Proposed/effective
39 FR 37602, 10/24/74
Promulgated
40 FR 33152, 8/6/75 (14)
Revised
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-66
-------
BMfcpari V—SJandoi^s of Performance to
<3®al Preparation Ftento 26»'"
§ Sffl.gS© AjjupUeoWIiOy and
off affected facility.64
(a) The provisions of thts subpart are
applicable to any of the following af-
fected facilities in coal preparation
plants which process more than 200 tons
par day: thermal dryers, pneumatic ccal-
cleaning equipment (air tables), coal
processing and conveying equipment (in-
cluding breakers and crushers), coal
storage systems, end coal transfer and
loading systems.
(b) Any facility under paragraph (a)
of this section that commences construe-
6toa or modification after October 24,
\fflQ. {g sffifojGcfe to QMS Fsquiremento of
.71
As used in this subpart, all terms not
defined herein have the meaning given
them in the Act and in subpart A of this
part
(a) "Coal preparation plant" means
any facility (excluding underground
mining operations) which prepares ccai
by one or more of the following proc-
esses: breaking, crushing, screening, wefe
or dry cleaning, and thermal drying.
Ob) "Bituminous coal" means solid fca=
oil fuel classified as bituminous coal toy
A.B.TM. Designation X>-38M6.
(c) "Coal" means all solid fossil fuels
classified as anthracite, bituminous, craEt=
bituminous, or Jlgnlts by AS.TM. Bsa=
agnation X>-388-fl6.
(d) "Cyclonic flow" means a spiralSng
movement of exhaust gases within e, fiasfi
or stack.
(e) "Thermal «S?yer" means any to=
effllty in which Qie moisture eonteaft ®3
bituminous ©oal to rsducsd fe? ©oatesO
•\jltfa a heated gas stream which is ex-
feausted to the atmosphere.
, ' (f) "Pneumatic eoal-cleaning equip-
ment" means any facility which classifies
Bituminous coal by size or separates bi-
tuminous coal from refuse by application
b£ air stream(s).
! (g) "Coal processing and conveying
equipment" means any machinery used
%o reduce the size of coal or to separate
feoal from refuse, and the equipment used
§o convey coal to or remove coal and
Refuse from the machinery. This in-
cludes, but is not limited to, breakers,
crushers, screens, and conveyor belts.
(h) "Coal storage system" means any
facility used to store coal except for open
.storage piles.
: (1) "Transfer and loading system"
means any facility used to transfer and
toad coal for shipment.
Q
-------
Subpart Z—Standards of Performance for
Ferroalloy Production Facilttie*33-3*
§ 60.260 Applicability and designation
of affected facility/*
(a) The provisions of this subpart are
applicable to the following affected fa-
cilities: electric submerged arc furnaces
which produce silicon metal, ferrosilicon,
calcium silicon, sillcomanganese zircon-
ium, ferrochrome silicon, silvery
iron, high-carbon ferrochrome, charge
chrome, standard ferromanganese, sill-
comanganese, ferromanganese silicon, or
calcium cattolde; and dust-handling
equipment35
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after October 21,
1974, is subject to the requirements of
this subpart.
§ 60,261 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
(a) "Electric submerged arc furnace"
means any furnace wherein electrical
energy is converted to heat energy by
transmission of current "between elec-
trodes partially subm:rged in the furnace
charge.
(b) "Furnace charge" me?ns any ma-
terial introduced into the electric,sub-
merged arc furnace and may consist of,
but. is not limited to, orss, slag, carbo-
naceous material, and limestone.
(c> "Product change" means any
change in the composition of ths furnace
charge that would cause the electric sub-
merged arc furnace to become subject
to a different mass standard applicable
under this subpart.
(d) "Slag" means the more or less
completely fused and vitrified matter
separated during the reduction of a
metal from its ore.
(e) "Tapping" means the removal of
slag or product from the electric sub-
merged arc furnace under normal op-
erating conditions such as removal of
metal under normal pressure and move-
ment by gravity down the spout Into the
ladle.
(f) "Tapping period" means the time
duration from initiation of the process
of opening the tap hole until plugging of
the tap hole Is complete.
(g) "Furnace cycle" means the time
period from completion of a furnace
product tap to the completion of the next
consecutive product tap.
(h) "Tapping station" means that
general area where molten product or
•lag is removed from the electric sub-
merged arc furnace.
(i) "Blowing tap" means any tap in
which an evolution of gas forces or pro-
jects jets of Same or matal sparks be-..
yond the ladle, runner, or collection hood.
(J) "Furnace power Input" means the
resistive electrical power consumption of
an electric submerged arc furnace as
measured in kilowatts.
(k) "Dust-handling equipment" means
any equipment used to handle partlcu-
lite matter collected by th: air pollution
control device (and located at or near
•uch device) serving any electric sub-
merged arc furnace subject to this sub-
part.
<1) "Control device'" means the air
pollution control equipment used to re-
Move partlculate matter generated by an
electric submerged arc furnace from an
effluent gas stream.
(m) "Capture 'system" means the
equipment (Including hoods, ducts, fans,
dampers, etc.) used to capture or trans-
port particulate matter generated by an
affected electric submerged arc furnace
to the control device.
(n) "Standard ferromanganese" means
that alloy as defined by A.S.T.M. desig-
nation A99-66.
(o) "Sillcomanganese" means that
alloy as defined by A.S.T.M. designation
A483-66.
(p) "Calcium carbide" means material
containing 70 to 85 percent calcium car-
bide by weight.
(q) "High-carbon ferrochrome" means
that alloy as denned by A.S.T.M. desig-
nation A101-66 grades HC1 through HC6.
(r) "Charge chrome" means that alloy
containing 52 So 70 percent by weight
chrcmium, 5 to 8 percent by weight car-
ban, and 3 to 6 percent by weight silicon.
(s). "Silvery iron" means any f erro-
silicon, as defined by A.S.T.M. designa-
tion 100-69, which contains Isss than
30 percent silicon.
(t) "Ferrochrome silicon" means that
alloy as defined by A.S.T.M. designation
A482-66.
(u) "Eilicomanganess zirconium"
means that alloy containing 60 to 65 per-
cent by weight silicon, 1.5 to 2.5 percent
by weight calcium, 5 to 7 percent by
weight zirconium, 0.75 to 1.25 percent by
wci;ht aluminum, 5 to 7 percent by
weight manganese, and 2 to 3 percent by
weight barium.
(v) "Calcium silicon" means that
alloy as defined by A.S.T.M. designation
A495-G4.
(w) "Ferrosilicon" means that alloy as
defined by A.S.T.M. designation A100-69
grades A, B, C, D, and E which contains
60 or more percent by weight silicon.
(x) "Silicon metal" means any silicon
alloy containing more than 96 percent
silicon by weight.
(y) "Ferromanganese silicon" means
that alloy containing 63 to 66 percent by
weight manganese, 28 to 32 percent by
weight silicon, and a maximum of 0.08
percent by weight carbon.
g 60.262 Standard for particulate mat-
ter.
(a) On and after the date on which the
performance test required to be con-
ducted by § 60.8 is completed, no owner
or operator subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere .from any electric
submerged arc furnace any gases which:
(1) Exit frorr. a control device and con-
tain particulate matter in excess of 0.45
kg/MW-hr (0.99 Ib/MW-hr) while sili-
con metal, ferrosilicon, calcium silicon,
or sillcomanganese zirconium is being
produced.
(2) Exit from a control device and con-
tain particulate matter in excess of 0.23
kg/MW-hr (0.51 Ib/MW-hr) while high-\
carbon ferrochrome, charge chrome,
standard ferromanganese, silicomanga-
nese, calcium carbide, ferrochrome sill- /
con, ferromanganese silicon, or silvery '
Iron is being produced.
(3) Exit from a control device and ex-
hibit IS percent opacity or greater.
(4) Exit from an electric submerged
arc furnace and escape the capture sys-
tem and are visible without the aid of
Instruments. The requirements under
I this subparagraph apply only during pe-
riods when flow rates are being estab-
lished under ! 60.265(d).
«) Escape the capture system at the
tapping station and are visible without
the aid of instruments for more than 40
percent of each tapping period. There are
no limitations on visible emissions under
this subiaragraph when a blowing tap
occurs. The requirements under this sub-
paragraph apply only during periods
when flow rates are being established
under 560.265(d).
The owner or operator subject to
the provisions of this subpart shall in-
stall, calibrate, maintain and operate a
continuous monitoring system for meas-
urement of the opacity of emissions dis-
charged into the atmosphere from the
control device (s).
(b) For the purpose of .reports re-
quired under § 60.7(c), the owner or op-
erator shall report as excess emissions
all six-minute periods in which the av-
erage onacity is 15 percent or greater.
(c) The owner or operator subiect to
the provisions of this subnart shall sub-
mit a written report of any product
change to the Administrator. Reports of
product changes must be postmarked
not later than 30 days after implemen-
tation of the product change.
(Sec. 114. Clean Air Act is amended (42
U.S.C. 7414».68'83
£ 60.265 Monitoring of operation*.
(a) The owner or operator of any elec-
tric submerged arc furnace subject to the
provisions of this subpart shall main-
-63
-------
tain daily records of the following in-
formation:
(1) Product being produced.
(2) Description of constituents of fur-
aace charge. Including the quantity, by
weight.
(3) Time and duration of each tap-
ping period and the identification of ma-
terial tapped (slag or product.)
(4) All furnace power input data ob-
onder paragraph (b) of this sec-
AH fiorr rote data, obtained under
f®) us this section or oil faa
swraer consumption and pressure
(flrop data obtained under paragraph (e)'
®3 this section.
svred in kilowatts), and
(2) Install, calibrate, maintain, and
operate a device to continuously meas-
ure ?nd re-ord the pressure droo across
the fan. The fan rower consumption and
pressure dron measurements must be
synchronised to allo-' real time comnar-
i'ons cf the data. The monitoring de-
vices must hnve an accuracy of ±5 per-
cent over the'r normal operating ranges.
(f) The volumetric flow rate through
each fnn of the capture svstem must be
determined from the fan power con-
sumntlon, fan pressure drop, and fan
performance curve fnecif ed under para-
prar-h (e) of thh section, during anv per-
formance test required under § 60.8 of
this p'rt to demonstrate compMpnce with
the standards under §§ 60.262(a) (4) and
(5). The O"'ner or operator shall deter-
mine the volumetric flow rate at a repre-
sentative temnerature for furnace power
input leve's of 50 and 100 percent of the
nominal rated capacity of the electric
submerged arc furnace. At all times the
e'ectric .submerged arc furnace is op-
erated, the owner or operator shall main-
tain the fan power consumption and fan
pressure drop at leve's such that the vol-
umetn'c flow rat° is at or above the levels
established during the most recent per-
formonce te*t for that furnace poxver in-
put level. If emissions due to tapping are
captured and ducted separately from
emissions of the electric mbmerged arc
furnace, during each tapping period the
owner or operator shall maintain the fan
power consumption and fan pressure
drop at levels such that the volumetric
flow rate is at or above the levels estab-
lished during the most recent perform-
ance test. Operation at lower flow rates
mav be considered bv the Administrator
to be unacceptable operation and main-
tenance of the affected facility. The own-
er or operator may request tint these
flow rates be reestablished by conducting
new performs nee tests under 8 60.8 of
this part. The Administrator may require
the owner or operator to verify the fan
performance curve by monitoring neces-
sary fan operating parameters and de-
termining the gas volume moved relative
to Methods 1 and 2 of Appendix A to this
part.
(g) AH monitoring devices required
under paragraphs (c) and (e) of this
cection are to be checked for calibration
annually in accordance with the proce-
dures under G@0.13(b>.
(Sec. 114, Clean Air Act i£ amended (42
U.S.C. 7414)). 48, 83
g 60.266 Test methods on<8 jirocedorea.
, shell be used to determine compli-
ance with the standards prescribed in
060.262 and §30.263 as follows:
(1) Method 5 for the concentration of
particulate matter and the associated
moisture content except that the heating
systems specified in paragraphs 2.1.2 and
2.1.4 of Method 5 are not to be used when
the carbon monoxide content of the gas
stream exceeds 10 percent by volume,
dry basis.
(2) Method 1 for sample and velocity
traverses.
(3) Method 2 for velosity and volumet-
ric flow rate.
(4) Method 3 for gas analysis, includ-
ing carbon monoxide.
(b) For Method 5, the sampling time
for each run is to Include an integral
number of furnace cycles. The sampling
time for each run must be at least 60
minutes and the minimum sample vol-
ume must be 1.8 dscm (64 dscf) when
sampling emissions from open electric
submerged arc furnaces with wet scrub-
ber control devices, sealed electric sub-
merged arc furnaces, or semi-enclosed
electric submerged arc furnaces. When
sampling emissions from other types of
installations, the sampling time for each
run must be at leist 200 minutes and the
minimum sample volume must be 5.7
dscm (200 dscf). Shorter sampling times
or smaller sampling volumes, when ne-
cessitated by process variables or other
factors, may be approved by the Admin-
istrator.
(c) During the performance test, the
owner or operator shall record the maxi-
mum open hood area (in hoods with
segmented or otherwise nioveable sides)
under which the process is expected to
be operated and remain Incompliance
with all standards. Any future operation
of the hooding system with open areas in
excess of the maximum is not permitted.
(d> The owner or operator shall con-
struct the control device so that volu-
metric flow rates and particulate matter
emissions can be accurately determined
by applicable test methods and proce-
dures.
(e) During any performance' test re-
quired under § 60.8 of this part, the
owner or operator shall not allow gaseous
diluents to be added to the effluent gas
stream after the fabric in an open pres-
surized fabric filter collector unless the
111-69
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total gas volume flow from the collector
is accurately determined and considered
In the determination of emissions.
(f ) When compliance with 5 60.263 is
to be attained by combusting the gas
stream in a flare, the location of the
sampling site for partlculate matter is
to be upstream of the flare.
(g) For each run, partlculate matter
emissions, expressed in kg/hi (Ib/hr),
must be determined for each exhaust
stream at which emissions are quantified
using the following equation:
where:
£„= Emissions of partlculate matter In
kg/hr (Ib/hr).
C. =Con:entr»tlon of partlculate matter In
kg/dscm (ib/dscf) as determined by.
Method 5.
For Method 5. partlculate matter
emissions from the affected facility, ex-
pressed in kg/MW-hr (Ib/MW-hr) must
be determined for each run using the
following equation:
35
where:
• £ = Emissions of partlculate from the af-
fected facility,' In kg/MW-hr (lb/
MW-hr).
//=Total number of exhaust streams at
which emissions are quantified.
£»=Emission of partlculate matter from
each exhaust stream In kg/hr (lb/
hr). as determined In paragraph (g)
of this section.
p=Average furnace power Input during
the sampling period. In megawatts
as determined according to I 80.26}
(Sec. 114. Clean Air Act
U.S.C. 7414)).68'83
U amended (43
Proposed/effecti ve
39 FR 37922. 10/24/74
Promulgated
41 FR 18498, 5/4/76 (33)
Revised
41 FR 20659, 5/20/76 (35)
42 FR 37936, 7/25/77 (64)
42 FR 41424, 8/17/77 (68)
43 FR 8800, 3/3/78 (83)
111-70
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gubpfipj AA — Standards of Performance
fer Stool Hants: Electric Are Fumooso '
of offecaedl facility.
(s) The provisions of this subpart OFQ
applicable to the following affected fa-
cilities in steel plants: electric arc fur-
naces and dust-handling equipment.
(b) Any facility under paragraph (a)
of this section that commences construc-
tion or modification after October 21,
1074, is subject to tfes requlremente of
0 60.271
As used to this subpart, aU te'rms nofe
defined herein shall have the meaning
given them in the Act and in subpart A
o£ this part.
(a) "Electric arc furnace* CEAF)
means any furnace that produces molten
ateel and beats the charge materials
with electric arcs from carbon electrodes.
Furnaces from which the molten steel ts
cast into the shape of finished products,
such as in a foundry, are not affected fa-
cilities included within the scope of this
definition. Furnaces which, as the pri-
mary source of iron, continuously feed
prereduced ore pellets are not affected
faculties •within the scope of this
definition. .„
fb) "Dust-handling equipment" meaao
any equipment used to handle partice-
late matter collected by the control de-
vice and located at or near the control
device for an SAP subject to this sub-
8»art..
"Control device" means Qie ofc>
pollution control equipment, used to K>=
move participate matter generated by
an EAP(s) from the effluent gas stream.
(d) "Capture system" means the
equipment (including ducts, hoods, fans,
dampers, etc.) used to capture or trans-
port particulate matter generated by an
EAF to the air pollution control device.
(e) "Charge" means, the addition of
iron and steel scrap or other materials
into the top of an electric arc furnace.
£ emissleas toot® t&s chop
.fafcea to accordance with Method e of
Appendix A of this part for the applica-
ble time periods.
(1) "Heat time" means the period
commencing when scrap is charged to an
esipty SAP and terminating when the
BAP tap is completed.
percent, may
{recur during tapping periods.
(iii) Opacity standards under para-
graph (c.) (3) of this section shall apply
only during periods when flow rates and
pressures are being established under
<5 60.274 Xc) and (f ) .
(iv) Where the capture system is op-
erated such that the roof of the shop is
closed during the charge and the tap,
end emissions to the atmosphere are pre-
vented until tiie roof is opened after
completion of the charge or tap, the shop
opacity standards under paragraph (a)
(3) of this section shall apply when the
roof is opened and shall continue to ap-
ply for the length of time defined by the
charging and/or tapping periods.
(b) On and after the date on which the
performance test required to be con-
ducted by B 60.8 Is completed, no owner
relative to Methods 1 and 2 of Appendix
A of this part.
(c) When the owner or operator of
an EAF is required to demonstrate com-
pliance with the standard under § 60.272
(a) (3) and at any other time the Ad-
ministrator may require (under section
ilfl of the Act, as amended), the volu-
metric flow rate through each separately
ducted hood shall be determined during
all periods in which the hood is operated
for the purpose, of capturing emissions
from the EAF using the monitoring de-
vice under paragraph (b) of this section.
The owner or operator may petition the
Administrator for reestablishment of
these flow rates whenever the owner or
operator can demonstrate to the Admin-
istrator's satisfaction that the EAF oper-
ating conditions upon which the flow
rates were previously established are no
longer applicable. The flow rates deter-
mined during the most recent demon-
stration" of compliance shall be main-
tained (or may be exceeded) at the ap-
propriate level for each applicable period.
Operation at lower flow rates may be
considered by the Administrator to be
unacceptable operation and maintenance
of the affected facility.
(d) The owner or operator may peti-
tion the Administrator to approve any
alternative method that will provide a
continuous .record of operation of each
emission capture system.
(e) Where emissions during any phase
of the heat time are controlled by use
of a direct shell evacuation system, the
111-71
-------
owner or operator shall Install, calibrate,
and maintain a monitoring device that
continuously records the pressure in the
free space inside the EAF. The pressure
shall be recorded as 15-minute inte-
grated averages. The monitoring device
may be installed in any appropriate lo-
cation in the EAT such that reproduc-
ible results will be obtained. The pres-
sure monitoring device shall have an ac-
curacy of ±5 mm of water gauge over
its normal operating range and shall be
calibrated according to the manufac-
turer's Instructions.
(f) When the owner or operator of an
EAF is required to demonstrate compli-
ance with the standard under i 60.272
(a) (3) and at any other time the Ad-
ministrator may require (under section
114 of the Act, as amended), the pressure
in the free space inside the furnace shall
be determined during the meltdown and
reflning period(s) using the monitoring
device under paragraph (e) of this sec-
tion. The owner or operator may peti-
tion the Administrator for reestablish -
ment of the 15-minute Integrated aver-
age pressure whenever the owner or
operator can demonstrate to the Admin-
istrator's satisfaction that the EAP op-
erating conditions upon which the pres-
sures were previously established are no
longer applicable. The pressure deter-
mined during the.most recent demon-
stration of compliance shall be main-
tained at all times the EAF is operating
In a meltdown and reflning period. Op-
eration at -higher pressures may be con-
sidered by the Administrator to be un-
acceptable operation and maintenance
of the affected facility.
(g) Where the capture system is de-
signed and operated such that all emis-
sions are captured and ducted to a con-
trol device, the owner or operator shall
not be subject to the requirements of this
section.
(Sec. 114. Clean Air Act Is amended (42
U.S.C. 7414».68 83
§ 60.275 Test methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided under
§60.8(b), shall be used to determine
compliance with the standards pre-
scribed under § 60.272 as follows:
(1) Method 5 for concentration of par-
ticulate matter and associated moisture
content;
(2) Method 1 for sample and velocity
traverses;
(3) Method 2 for velocity and volu-
metric flow rate; and
(4) Method 3 for gas analysis.
(b) For Method 5, the sampling time
for each run shall be at least four hours.
When a single EAF is sampled, the sam-
pling time for each run shall also in-
clude an integral number of heats.
Shorter sampling times, when necessi-
tated by process variables or other fac-
tors, may be approved by the Admin-
istrator. The minimum sample volume
shall be 4.5 dscm (160 dscf).
(c) For the purpose of this subpart.
the owner or operator shall conduct the
demonstration of compliance with 60.-
272(a)(3> and furnish the Adminis-
trator a written report of the results of
the test.
(d) During any performance test re-
quired under § 60.8 of this part, no gase-
ous diluents may be added to the
•effluent gas stream after 'the fabric in
any pressurized fabric filter collector.
unless the amount .of dilution! Is sepa-
rately determined and considered in the
determination of emissions.
(e) When more than one control de-
vice serves the EAF(s) being tested, the
concentration of particulate matter shall
be determined using the followim
equation:
C.=
£}(«.).
where:
C.=-concentration of parttcnlate matw
In mg/dscm (gr/dsef) as determine*
, by method 5.
AT= total number of control devices
tested.
-------
Subpart M—Slandardi of Performance lor
Kraft Pulp Mills 82
60.280 Applicability and designation of af-
fected facility.
(a) The provisions of this subpart
are applicable to the following affect-
ed facilities in kraft pulp mills: digest-
er system, brown stock washer system,
multiple-effect evaporator system,
black liquor oxidation system, recov-
ery furnace, smelt dissolving tank,
lime kiln, and condensate stripper
system. In pulp mills where kraft
pulping is combined with neutral sul-
fite semichemical pulping, the provi-
sions of this subpart are applicable
when any portion of the material
charged to an affected facility is pro-
duced by the kraft pulping operation.
(b) Any facility under paragraph (a)
of this section that commences con-
struction or modification after Sep-
tember 24, 1976, is subject to the re-
quirements of this subpart.
§ 60.281 Definitions.
As used in this subpart, all terms not
defined herein shall have the same
meaning given them in the Act and in
Subpart A.
(a) "Kraft pulp mill" means any sta-
tionary source which produces pulp
from wood by cooking (digesting)
wood chips in a water solution of
sodium hydroxide and sodium sulfide
(white liquor) at high temperature
and pressure. Regeneration " of the
cooking chemicals through a recovery
process is also considered part of the
kraft pulp mill.
(b) "Neutral sulfite semichemical
pulping operation" means any oper-
ation in which pulp is produced from
wood by cooking (digesting) wood
chips in a solution of sodium sulfite
and sodium bicarbonate, followed by
mechanical defibrating (grinding).
(c) "Total reduced sulfur (TRS)"
means the sum of the sulfur com-
pounds hydrogen sulfide, methyl mer-
cap tan, dimethyl sulfide, and dimethyl
disulfide, that are released during the
kraft pulping operation and measured
by Reference Method 16.
(d) "Digester system" means each
continuous digester or each batch di-
gester used for the cooking of wood in
white liquor, and associated flash
tank(s), below tank(s), chip steamer(s),
and condenser(s).
(e) "Brown stock washer system"
means brown stock washers and associ-
ated knotters, vacuum pumps, and fil-
trate tanks used to wash the pulp fol-
lowing the digester system.
(f) "Multiple-effect evaporator
system" means the multiple-effect
evaporators and associated
condenser(s) and hotwell(s) used to
concentrate the spent cooking liquid
that is separated from the pulp (black
liquor).
(g) "Black liquor oxidation system"
means the vessels used to oxidize, with
air or oxygen, the black liquor, and as-
sociated storage tank(s).
(h) "Recovery furnace" means either
a straight kraft recovery furnace or a
cross recovery furnace, and includes
the direct-contact evaporator for a
direct-contact furnace.
(i) "Straight kraft recovery furnace"
means a furnace used to recover
chemicals consisting primarily of
sodium and sulfur compounds by
burning black liquor which on a quar-
terly basis contains 7 weight percent
or less of the total pulp solids from
the neutral sulfite semichemical pro-
cess or has green liquor sulfidity of 28
percent or less.
(J) "Cross recovery furnace" means a
furnace used to recover chemicals con-
sisting primarily of sodium and sulfur
compounds by burning black liquor
which on a quarterly basis contains
more than 7 weight percent of the
total pulp solids from the neutral sul-
fite semichemical process and has a
green liquor sulfidity of more than 28
percent.
(k) "Black liquor solids" means the
dry' weight of the solids which enter
the recovery furnace in the black
liquor.
(1) "Green liquor sulfidity" means
the sulfidity of the liquor which leaves
the smelt dissolving tank.
(m) "Smelt dissolving tank" means a
vessel used for dissolving the smelt
collected from the recovery furnace.
(n) "Lime kiln" means a unit used to
calcine lime mud, which consists pri-
marily of calcium carbonate, into
quicklime, which is calcium oxide.
(o) "Condensate stripper system"
means a column, and associated con-
densers, used to strip, with air or
steam, TRS compounds from conden-
sate streams from various processes
within a kraft pulp mill.
§ 60.282 Standard for paniculate matter.
(a) On and after the date on which
the performance test required to be
conducted by §60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere:
(1) From any recovery furnace any
gases which:
(i) Contain participate matter in
excess of 0.10 g/dscm (0.044 gr/dscf)
corrected to 8 percent oxygen.
(ii) Exhibit 35 percent opacity or
greater.
(2) From any smelt dissolving tank
any gases which contain participate
matter in excess of 0.1 g/kg black
liquor solids (dry weight)[0.2 Ib/ton
black liquor solids (dry weight)].
(3) From any lime kiln any gases
which contain participate matter in
excess of:
(i) 0.15 g/dscm (0.067 gr/dscf) cor-
rected to 10 percent oxygen, when gas-
eous fossil fuel is burned.
(ii) 0.30 g/dscm (0.13 gr/dscf) cor-
rected to 10 percent oxygen, when
liquid fossil fuel is burned.
§60.283 Standard for total reduced sulfur
(TRS).
(a) On and after the date on which
the performance test required to be
conducted by §60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere:
(1) From any digester system, brown
stock washer system, multiple-effect
evaporator system, black liquor oxida-
tion system, or condensate stripper
system any gases which contain TRS
In excess of 5 ppm by volume on a dry
basis, corrected to 10 percent oxygen.
unless the following conditions are
met:
(i) The gases are combusted in a lime
kiln subject to the provisions of para-
graph (a)(5) of this section; or
(ii) The gases are combusted In a re-
covery furnace subject to the provi-
sions of paragraphs (a)(2) or (a)(3) of
this section; or
(iii) The gases are combusted with
other waste gases in an incinerator or
other device, or combusted in a lime
kiln or recovery furnace not subject to
the provisions of this subpart, and are
subjected to a minimum temperature
of 1200* F. for at least 0.5 second; or
(iv) It has been demonstrated to the
Administrator's satisfaction by the
owner or operator that incinerating
the exhaust gases from a new, modi-
fied, or reconstructed black liquor oxi-
dation system or brown stock washer
system in an existing facility is tech-
nologically or economically not feasi-
ble. Any exempt system will become
subject to the provisions of this sub-
part if the facility is changed so that
the gases can be incinerated.
(v) The gases from the digester
system, brown stock washer system,
condensate stripper system, or black
liquor oxidation system are controlled
by a means other than combustion. In
this case, these systems shall not dis-
charge any gases to the atmosphere
which contain TRS in excess of 5 ppm
by volume on a dry basis, corrected to
the actual oxygen content of the un-
treated gas stream.9'
(2) From any straight kraft recovery
furnace any gases which contain TRS
in excess of 5 ppm by volume on a dry
basis, corrected to 8 percent oxygen.
(3) From any cross recovery furnace
any gases which contain TRS in excess
of 25 ppm by volume on a dry basis,
corrected to 8 percent oxygen.
(4) From any smelt dissolving tank
any gases which contain TRS in excess
of 0.0084 g/kg black liquor solids (dry
weight) [0.0168 Ib/ton liquor solids
(dry weight)].
(5) From any lime kiln any gases
which contain TRS in excess of 8 ppm
by volume on a dry basis, corrected to
10 percent oxygen.
Ill-73
-------
f M.284- Monitoring of emissions and op-
erations.
(a) Any owner or operator subject to
the provisions of this subpart shall in-
stall, calibrate, maintain, and operate
the following .continuous monitoring
systems:
(DA continuous monitoring system
to monitor and record the opacity of
the gases discharged into the atmos-
phere from any recovery furnace. The
•pan of this system shall be set at 70
percent opacity.
(2) Continuous monitoring systems
to monitor and record the concentra-
tion of TRS emissions on a dry basis
and the percent of oxygen by volume
on a dry basis In the gases discharged
into the atmosphere from any lime
kiln, recovery furnace, digester
system, brown stock washer system,
multiple-effect evaporator system,
black liquor oxidation system, or con-
densate stripper system, except where
the provisions of 860.283(a)(l) (ill) or
(iv) apply. These systems shall be lo-
cated downstream of the control
device(s) and the span(s) of these con-
tinuous monitoring system(s) shall be
set:
(i) At a TRS concentration of 30
ppm for the TRS continuous monitor-
ing system, except that for any cross
recovery furnace the span shall be set
at SO ppm.
(11) At 20 percent oxygen for the
continuous oxygen monitoring system.
(b) Any owner or operator subject to
the provisions of this subpart shall in-
stall, calibrate, maintain, and operate
the following continuous monitoring
devices:
(DA monitoring device which mea-
sures the combustion temperature at
the point of incineration of effluent
gases which are emitted from any di-
gester system, brown stock washer
system, multiple-effect evaporator
system, black liquor oxidation system,
or condensate stripper system where
the provisions of §60.283(a)(l)(Ui)
apply. The monitoring device is to be
certified by the manufacturer to be ac-
curate within ±1 percent of the tem-
perature being measured.
(2) For any lime kiln or smelt dis-
solving tank using a scrubber emission
control device:
(1) A monitoring device for the con-
tinuous measurement of the pressure
loss of the gas stream through the
control equipment. The monitoring
device is to be certified by the manu-
facturer to be accurate to within a
gage pressure of ±500 pascals (ca. ±2
Inches water gage pressure).
(11) A monitoring device for the con-
tinuous measurement of the scrubbing
liquid supply pressure to the control
equipment. The monitoring device is
to be certified by the manufacturer to
be accurate within ±15 percent of
design scrubbing liquid supply pres-
sure. The pressure sensor or tap is to
be located close to the scrubber liquid
discharge point. The Administrator
may be consulted for approval of alter-
native locations.
(c) Any owner or operator subject to
the provisions of this subpart shall,
except where the provisions of
§60.283(a)(l)(iv) or §60.283(a)(4)
apply.
(1) Calculate and record on a daily
basis 12-hour average TRS concentra-
tions for the two consecutive periods
of each operating day. Each 12-hour
average shall be determined as the
arithmetic mean of the appropriate 12
contiguous 1-hour average total re-
duced sulfur concentrations provided
by each continuous monitoring system
installed under paragraph (a)(2) of
this section.
(2) Calculate and record on a daily
basis 12-hour average oxygen concen-
trations for the two consecutive peri-
ods of each operating day for the re-
covery furnace and lime kiln. These
12-hour averages shall correspond to
the 12-hour average TRS concentra-
tions under paragraph (c)(l) of this
section and shall be determined as an
arithmetic mean of the appropriate 12
contiguous 1-hour average oxygen con-
centrations provided by 'each continu-
ous monitoring system installed under
paragraph (a)(2) of this section.
(3) Correct all 12-hour average TRS
concentrations to 10 volume percent
oxygen, except that all 12-hour aver-
age TRS concentration from a recov-
ery furnace shall be corrected to -8
volume percent using the following
equation:
where:
C««T=the concentration corrected for
oxygen.
C^^the concentration uncorrected for
oxygen.
X=the volumetric oxygen concentration In
percentage to be corrected to (8 percent
for recovery furnaces and 10 percent for
lime kilns, incinerators, or other de-
. vices).
y=the measured 12-hour average volumet-
ric oxygen concentration.
(d) For the purpose of reports re-
quired under §60.7(c), any owner or
operator subject to the provisions of
this subpart shall report periods of
excess emissions as follows:
(1) For emissions from any recovery
furnace periods of excess emissions
are:
(i) All 12-hour averages of TRS con-
centrations above 5 ppm by volume for
straight kraft recovery furnaces and
above 25 ppm by volume for cross re-
covery furnaces.
(11) All 6-minute average opacities
that exceed 35 percent.
(2) For emissions from any lime kiln,
periods of excess emissions are all 12-
hour average TRS concentration
above 8 ppm by volume.
(3) For emissions from any digester
system, brown stock washer system,
multiple-effect evaporator system,
black liquor oxidation system, or con-
densate stripper system periods of
excess emissions are:
(i) All 12-hour average TRS concen-
trations above 5 ppm by volume unless
the provisions of §60.283(a)(l) (i), (ii),
or (iv) apply; or
(ii) All periods in excess of 5 minutes
and their duration during which the
combustion temperature at the point
of incineration is less than 1200° F.
where the provisions of
§ 60.283(a)(l)(ii) apply.
(e) The Administrator will not con-
sider periods of excess emissions re-
ported under paragraph (d) of this sec-
tion to be indicative of a violation of
§ 60.11(d) provided that:
(1) The percent of the total number
of possible contiguous periods of
excess emissions in a quarter (exclud-
ing periods of startup, ~shutdown, or
malfunction and periods when the fa-
cility is not operating) during which
excess emissions occur does not
exceed:
(i) One percent for TRS emissions
from recovery furnaces.
(ii) Six percent for average opacities
from recovery furnaces.
(2) The Administrator determines
that the affected facility, including air
pollution control equipment, is main-
tained and operated in a manner
which is consistent with good air pol-
lution control practice for minimizing
emissions during periods of excess
emissions.
§ 60.285 Test methods and procedures.
(a) Reference methods in Appendix
A of this part, except as provided
under § 60.8(b), shall be used to deter-
mine compliance with §60.282(a) as
follows:
(1) Method 5 for the concentration
of particulate matter and the associat-
ed moisture content,
(2) Method 1 for sample and velocity
traverses,
(3) When determining compliance
with § 60.282(a)(2), Method 2 for veloc-
ity and volumetric flow rate,
(4) Method 3 for gas analysis, and
(5) Method 9 for visible emissions.
(b) For Method 5, the sampling time
for each run shall be at least 60 min-
utes and the sampling rate shall be at
least 0.85 dscm/hr (0.53 dscf/min)
except that shorter sampling times,
when necessitated by process variables
or other factors, may be approved by
the Administrator. Water shall be
used as the cleanup solvent instead of
acetone in the sample recovery proce-
dure outlined in Method 5.
(c) Method 17 (in-stack filtration)
may be used as an alternate method
for Method 5 for determining compli-
ance with §60.282(a)(l)(i): Provided,
That a constant value of 0.009 g/dscm
(0.004 gr/dscf) is added to the results
of Method 17 and the stack tempera-
111-74
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ture is no greater than 205' C (ca. 400°
F). Water shall be used as the cleanup
solvent instead of acetone in the
sample recovery procedure outlined in
Method 17.
(d) For the purpose of determining
compliance with §60.283(a) (1), (2),
(3), (4), and (5), the following refer-
ence methods shall be used:
(1) Method 16 for the concentration
of TRS,
(2) Method 3 for gas analysis, and
(3) When determining compliance
with §60.283(a)(4), use the results of
Method 2, Method 16, and the black
liquor solids feed rate in the following
equation to determine the TRS emis-
sion rate.
Where:
f •= mass of TRS emitted per unity of black
liquor solids (g/kg) (Ib/ton)
Cm = average concentration of hydrogen
sulfide (ELS) during the test period,
PPM.
CK.IH = average concentration of methyl
mercaptan (MeSH) during the test
period. PPM.
average concentration of dimethyl
sulfide (DMS) during the test period,
PPM.
= average concentration of dimethyl
disulfide (DMDS) during the test period.
PPM.
Ftm = 0.001417 g/m1 PPM for metric unite
= 0.08844 Ib/ft' PPM for English units
FUOB = 0.00200 g/m1 PPM for metric units
- 0.1248 Ib/ft1 PPM for English unite
fma = 0.002583 g/m* PPM for metric unite
«= 0.1612 lb/ff PPM for English unite
Fuax = 0.003917 g/m' PPM for metric unite
= 0.2445 lb/ff PPM for English unite
Q* — dry volumetric stack gas flow rate cor-
rected to standard conditions, dscm/hr
(dscf/hr)
BLS = black liquor solids feed rate, kg/hr
(Ib/hr)
(4) When determining whether a
furnace is straight kraft recovery fur-
nace or a cross recovery furnace,
TAPPI Method T.624 shall be used to
determine sodium sulfide, sodium hy-
droxide and sodium carbonate. These
'determinations shall be made three
times daily from the green liquor and
the daily average values shall be con-
verted to sodium oxide (Na,O) and
substituted into the following equa-
tion to determine the green liquor sul-
fidity:
OLS - 100 Cfc.VC.w'
Where:
OLS = percent green liquor sulf idity
Curt! = average concentration of No* ex-
pressed as Na,O (mg/1)
C».OH = average concentration of NaOH
expressed as Na,O (mg/1)
CfcjCOi = average concentration of Na,CO,
expressed as Na,O (mg/1)
(e) All concentrations of particular
matter and TRS required to be mea-
sured by this section from lime kilns
or incinerators shall be corrected 10
volume percent oxygen and those con-
centrations from recovery furnaces
shall be corrected to 8 volume percent
oxygen. These corrections shall be
made in the manner specified in
S 60.284(0(3).
Proposed/effective
41 FR 42012, 9/24/76
Promulgated
43 FR 7568. 2/23/78 (82)
Revised
43 FR 34784, 8/7/78 (91)
111-75
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Subpart CC—Standards of
Pvrformanc* for Glass Manufacturing
Plants118
860.290 Applicability and designation of
affected faculty.
(a) Each glass melting furnace is an
affected facility to which the provisions
of this subpart apply.
(b) Any facility under paragraph (a) of
this section that commences
construction or modification after June
15,1979, is subject to the requirements
of this subpart.
(c) This subpart does not apply to
hand glass melting furnaces, glass
melting furnaces designed to produce
less than 4,550 kilograms of glass per
day and all-electric melters.
{60.291 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them In the Act and in Subpart A
of this part unless otherwise required
by the context
"All-electric melter" means a glass
melting furnace in which all the heat
required for melting is provided by
electric current from electrodes
submerged in the molten glass, although
some fossil fuel may be charged to the
furnace as raw material only.
"Borosilicate Recipe" means raw
material formulation of the following
approximately weight proportions: 72
percent silica; 7 percent nepheline
syenite; 13 percent anhydrous borax; 8
percent boric acid; and 0.1 percent
misellaneous materials.
"Container glass" means glass made
of soda-lime recipe, clear or colored,
which is pressed and/or blown into
bottles, jars, ampoules, and other
products listed in Standard Industrial
Classification 3221 (SIC 3221).
"Flat glass" means glass made of
soda-lime recipe and produced into
continuous flat sheets and other
products listed in SIC 3211.
"Glass melting furnace" means a unit
comprising a refractory vessel in which
raw materials are charged, melted at
high temperature, refined, and
conditioned to produce molten glass.
The unit includes foundations,
superstructure and retaining walls, raw
material charger systems, heat
exchangers, melter cooling system,
exhaust system, refractory brick work,
fuel supply and electrical boosting
equipment, integral control systems and
instrumentation, and appendages for
conditioning ahd distributing molten
glass to forming apparatuses. The
forming apparatuses, including the float
bath used in flat glass manufacturing.
are not considered part of the glass
melting furnace.
"Glass produced" means the weight of
the glass pulled from the glass molting
furnace.
"Har.J glass melting furnace" means ;i
glass melting furnace where the molten
glass is removed from the furnace by a
glassworker using a blowpipe or a
pontil.
"Lead recipe" means raw material
formulation of the following
approximate weight proportions: 56
percent silica; 8 percent potassium
carbonate; and 36 percent red lead.
"Pressed and blown glass" means
glass which is pressed, blown, or both.
including textile fiberglass,
noncontinuous flat glass, noncontainer
glass, and other products listed in SIC
3229. It is separated into:
(1) Glass of borosilicate recipe.
(2) Glass of soda-lime and lead
recipes.
(3) Glass of opal, fluoride, and other
recipes.
"Rebricking" means cold replacement
of damaged or worn refractory parts of
the glass melting furnace. Rebricking
includes replacement of the refractories
comprising the bottom, sidewalls, or
roof of the melting vessel; replacement
of refractory work in the heat
exchanger; replacment of refractory
portions of the glass conditioning and
distribution system.
"Soda-lime recipe" means raw
material formulation of the following
approximate weight proportions: 72
percent silica; 15 percent soda; 10
percent lime and magnesia; 2 percent
alumina; and 1 percent miscellaneous
materials (including sodium sulfuto).
"Wool fiberglass" means fibrous gl.iss
of random texture, including fiberglass
insulation, and other products listed in
SIC 3296.
§ 60.292 Standards for participate matter.
(a) On and after the date on which Ihc
performance test required to be
conducted by § 60.8 is completed, no
owner or operator of a glass melting
furnace subject to the provisions of this
subpart shall cause to be discharged
into the atmosphere—
(1) From any glass melting furnace
fired exclusively with either a gaseous
fuel or a liquid fuel, particulate matter at
emission rates exceeding those specified
in Table CC-1, Column 2 and Column 3.
respectively, or
(2) From any glass melting furnace,
Tired simultaneously with gaseous and
liquid fuels, particulate matter at
emission rates exceeding STD as
specified by the following equation:
STD=X [1.3(Y)+(Z)J
Where:
STD = Particulate matter emission limit, g of
particulate/kg of glass produced.
X = Emission rate specified in Table CC-1 for
furnaces fired with gaseous fuel (Column
2).
Y = Decimal percent of liquid fuel heating
value to total (gaseous and liquid) fuel
heating value fired in the glass melting
furnaces as determined in § 60.296(f).
(joules/joules).
Z = (1-Y).
(b) Conversion of a glass melting
furnace to the use of liquid fuel is not
considered a modification for the
purposes of § 60.14.
(c) Rebricking and the cost of
rebricking is not considered a
reconstruction for the purposes of
§ 60.15.
Table CC-11.—Emission Rates
(g of particulate/kg of glass produced]
Col. 1 —Glass manufacturing plant
industry segment
Col.
2— »
Fur-
nace
fired
with
Col.
3—
Fur-
race
fired
with
ecus
fuel
liquid
fuel
Container glass 0.1 0.13
Pressed and blown glass
(ai Borosilicate Recipes 0.5 0.6S
(b) Soda-Lime and Lead Recipes 0.1 0.13
(c) Other-Than Sorosilicate. Soda-
Lime, and Lead Recipes (includ-
ing opal, fluoride, and other rec-
ipes) 0.25 0.325
Wool fiberglass 0.25 0.325
Fiat glass 0.225 0.225
§§ 60.293-60.295 [Reserved]
§ 60.296 Test methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided under
§ 60.8(b), shall be used to determine
compliance with § 60.292 as follows:
(1) Method 1 shall be used for sample
and velocity traverses, and
(2) Method 2 shall be used to
determine velocity and volumetric flow
rate.
(3) Method 3 shall be used for gas
analysis.
(4) Method 5 shall be used to
determine the concentration of
particulate matter and the associated
moisture content.
(b) For Method 5, the probe and filter
holder heating systen in the sampling
train shall be set to provide a gas
temperature no greater than 177° C. The
sampling time for each run shall be at
least 60 minutes and the collected
particulate shall weigh at least 50 mg.
(c) The particulate emission rate, E,
shall be computed as follows:
E=QxC
Where:
(1) E is the particulate emission rate (g/hr)
(2) Q is the average volumetric flow rate
(dscm/hr) as found from Method 2
(3) C is the average concentration (g/dscm) o
111-76
-------
participate matter as found from .the
modified Method 5
(d) The rate of glass produced, P (kg/
hr), shall be determined by dividing the
weight of glass pulled in kilograms (kg)
from the affected facility during the
performance test by the number of hours
(hr) taken to perform the performance
test. The glass pulled, in kilograms, shall
be determined by direct measurement or
computed from materials balance by
good engineering practice.
(e) For the purposes of these
standards the furnace emission rate
shall be computed as follows:
R=E-A~P
Where:
(1) R is the furnace emission rate (g/kg)
(2) E is the participate emission rate (g/hr)
from (c) above
(3) A is the zero production rate correction;
A is 227 g/hr for container glass, pressed
and blown (soda-lime and lead) glass,
and pressed and blown (other-'than
borosilicate, soda-lime, and lead) glass
A is 454 g/hr for pressed and blown
(borosilicate) glass, wool fiberglass, and
flat glass
(4) P is the rate of glass production (kg/hr)
from (d) above
(f) When gaseous and liquid fuels are
fired simultaneously in a glass melting
furnace, the heat input of each fuel,
expressed in joules, is determined
during each testing period by
multiplying the gross calorific value of
each fuel fired (in joules/kilogram) by
the rate of each fuel fired (in kilograms/
second) to the glass melting furnaces.
The decimal percent of liquid fuel
heating value to total fuel heating value
is determined by dividing the heat input
of the liquid fuels by the sum of the heat
input for the liquid fuels and the gaseous
fuels. Gross calorific values are
determined in accordance with
American Society of Testing and
Materials (A.S.T.M.) Method D 240-
64(73) (liquid fuels) and D 1826-64(7)
(gaseous fuels), as applicable. The
owner or operator shall determine the
rate of fuels burned during each testing
period by suitable methods and shall
confirm the rate by a material balance
over the glass melting system.
[Section 114 of Clean Air Act, as amended (42
U.S.C. 7414))
Proposed/effective
44 FR 34840, 6/15/79
Promulgated
45 FR 66742, 10/7/80 (118)
111-77
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Subpart DD—Standard* of
Performance for Grain Elevators 90
§60.300 Applicability and designation of
affected facility.
(a) The provisions of this subpart
apply to each affected facility at any
grain terminal elevator or any grain
storage elevator, except as provided
under §60.304(b). The affected facili-
ties are each truck unloading station,
truck loading station, barge and ship
unloading station, barge and ship load-
ing station, railcar loading station,
railcar unloading station, grain dryer,
and all grain handling operations.
(b) Any facility under paragraph (a)
of this section which commences con-
struction, modification, or reconstruc-
tion after (date of reinstatement of
proposal) is subject to the require-
ments of this part.
{60.301 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the act and in subpart A
of this part.
(a) "Grain" means corn, wheat, sor-
ghum, rice, rye, oats, barley, and soy-
beans.
(b) "Grain elevator" means any
plant or installation at which grain is
unloaded, handled, cleaned, dried,
stored, or loaded.
(c) "Grain terminal elevator" means
any grain elevator which has a perma-
nent storage capacity of more than
88,100 ms (ca. 2.5 million U.S. bushels),
except those located at animal food
manufacturers, pet food manufactur-
ers, cereal manufacturers, breweries,
and livestock f eedlots.
(d) "Permanent storage capacity"
means grain storage capacity which is
inside a building, bin, or silo.
(e) "Railcar" means railroad hopper
car or boxcar.
(f) "Grain storage elevator" means
any grain elevator located at any
wheat flour mill, wet corn mill, dry
corn mill (human consumption), rice
mill, or soybean oil extraction plant
which has a permanent grain storage
capacity of 35,200 m9 (ca. 1 million
bushels).
(g) "Process emission" means the
particulate matter which is collected
by a capture system.
(h) "Fugitive emission" means the
particulate matter which is not collect-
ed by a capture system and is released
directly into the atmosphere from an
affected facility at a grain elevator.
(i) "Capture system" means the
equipment such as sheds, hoods, ducts,
fans, dampers, etc. used to collect par-
ticulate matter generated by an affect-
ed facility at a grain elevator.
(j) "Grain unloading station" means
that portion of a grain elevator where
the grain is transferred from a truck,
railcar, barge, or ship to a receiving
hopper.
(k) "Grain loading station" means
that portion of a grain elevator where
the grain is transferred from the ele-
vator to a truck, railcar, barge, or ship.
(1) "Grain handling operations" in-
clude bucket elevators or legs (exclud-
ing legs used to unload barges or
ships), scale hoppers and surge bins
(garners), turn heads, scalpers, clean-
ers, trippers, and the headhouse and
other such structures.
(m) "Column dryer" means any
equipment used to reduce the mois-
ture content of grain in which the
grain flows from the top to the bottom
In one or more continuous packed col-
umns between two perforated metal
sheets.
(n) "Rack dryer" means any equip-
ment used to reduce the moisture con-
tent of grain in which the grain flows
from the top to the bottom in a cas-
cading flow around rows of baffles
(racks).
(o) "Unloading leg" means a device
which includes a bucket-type elevator
which is used to remove grain from a
barge or ship.
§ 60.302 Standard for particulate matter.
(a) On and after the 60th day of
achieving the maximum production
rate at which the affected facility will
be operated, but no later than 180
days after initial startup, no owner or
operator subject to the provisions of
this subpart shall cause to be dis-
charged into the atmosphere any
gases which exhibit greater than 0
percent opacity from any:
(1) Column dryer with column plate
perforation exceeding 2.4 mm diame-
ter (ca. 0.094 inch).
(2) Rack dryer in which exhaust
gases pass through a screen filter
coarser than 50 mesh.
(b) On and after the date on which
the performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere from
any affected facility except a grain
dryer any process emission which:
(1) Contains particulate matter in
excess of 0.023 g/dscm (ca. 0.01 gr/
dscf).
(2) Exhibits greater than 0 percent
opacity.
(c) On and after the 60th day of
achieving the maximum production
rate at which the affected facility will
be operated, but no later than 180
days after initial startup, no owner or
operator subject to the provisions of
this subpart shall cause to be dis-
charged into the atmosphere any fugi-
tive emission from:
(1) Any individual truck unloading
station, railcar unloading station, or
railcar loading station, which exhibits
greater than 5 percent opacity.
(2) Any grain handling operation
which exhibits greater than 0 percent
opacity.
(3) Any truck loading station which
exhibits greater than 10 percent opac-
ity.
(4) Any barge or ship loading station
which exhibits greater than 20 percent
opacity.
(d) The owner or operator of any
barge or ship unloading station shall
operate as follows:
(1) The unloading leg shall be en-
closed from the top (including the re-
ceiving hopper) to the center line of
the bottom pulley and ventilation to a
control device shall be maintained on
both sides of the leg and the grain re-
ceiving hopper.
(2) The total rate of air ventilated
shall be at least 32.1 actual cubic
meters per cubic meter of grain han-
dling capacity (ca. 40 ft'/bu).
(3) Rather than meet the require-
ments of subparagraphs (1) and (2), of
this paragraph the owner or operator
may use other methods of emission
control if it is demonstrated to the Ad-
ministrator's satisfaction that they
would reduce emissions of particulate
matter to the same level or less.
§ 60.303 Test methods and procedures.
(a) Reference methods in appendix
A of this part, except as provided
under §60.8(b), shall be used to deter-
mine compliance with the standards
prescribed under § 60.302 as follows:
(1) Method 5 or method 17 for con-
centration of particulate matter and
associated moisture content;
(2) Method 1 for sample and velocity
traverses;
(3) Method 2 for velocity and volu-
metric flow rate;
(4) Method 3 for gas analysis; and
(5) Method 9 for visible emissions.
(b) For method 5, the sampling
probe and filter holder shall be operat-
ed without heaters. The sampling time
for each run, using method 5 or
method 17, shall be at least 60 min-
utes. The minimum sample volume
shall be 1.7 dscm (ca. 60 dscf).
(Sec. 114, Clean Air Act, as amended (42
U.S.C. 7414).)
§60.304 Modifications.
(a) The factor 6.5 shall be used in
place of "annual asset guidelines
repair allowance percentage," to deter-
mine whether a capital expenditure as
defined by § 60.2(bb) has been made to
an existing facility.
(b) The following physical changes
or changes in the method of operation
shall not by themselves be considered
a modification of any existing facility:
(1) The addition of gravity loadout
spouts to existing grain storage or
grain transfer bins.
(2) The installation of automatic
grain weighing scales.
(3) Replacement of motor and drive
units driving existing grain handling
equipment.
111-78
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(4) The installation of permanent
storage capacity with no increase in
iourly grain handling capacity.
Proposed/effective
43 FR 34349, 8/3/78
Promulgated
43 FR 34340, 8/3/78 (90)
111-79
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Subpart GG—Standards of
Performance for Stationary Gas
Turbines'01
S 60.330 Applicability and designation of
affected facility.
The provisions of this subpart are
applicable to the following affected
facilities: all stationary gas turbines
with a heat input at peak load equal to
or greater than 10.7 gigajoules per hour,
based on the lower heating value of the
fuel fired.
560.331 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in subpart A
of this part.
(a) "Stationary gas turbine" means
any simple cycle gas turbine,
regenerative cycle gas turbine or any
gas turbine portion of a combined cycle
steam/electric generating system that is
not self propelled. It may, however, be
mounted on a vehicle for portability.
(b) "Simple cycle gas turbine" means
any stationary gas turbine which does
not recover heat from the gas turbine
exhaust gases to preheat the inlet
combustion air to the gas turbine, or
which does not recover heat from the
gas turbine exhaust gases to heat water
or generate steam.
{c) "Regenerative cycle gas turbine"
means any stationary gas turbine which
recovers heat from the gas turbine
exhaust gases to preheat the inlet
combustion air to the gas turbine.
(d) "Combined cycle gas turbine"
means any stationary gas turbine which
recovers heat from the gas turbine
exhaust gases to heat water or generate
steam.
(e) "Emergency gas turbine" means
any stationary gas turbine which
operates as a mechanical or electrical
power source only when the primary
power source for a facility has been
rendered inoperable by an emergency
situation.
(f) "Ice fog" means an atmospheric
suspension of highly reflective ke
crystals.
(g) "ISO standard day conditions"
means 288 degrees Kelvin, 60 percent
relative humidity and 101.3 kilopascals
pressure.
(h) "Efficiency" means the gas turbine
manufacturer's rated heat rate at peak
load in terms of heat input per unit of
power output based on the lower
heating value of the fuel
(i) "Peak load" means 100 percent of
the manufacturer's design capacity of
the gas turbine at ISO standard day
conditions.
(j) "Base load" means the load level at
which a gas turbine is normally
operated.
(k) "Fire-fighting turbine" means any
stationary gas turbine that is used solely
to pump water for extinguishing Ores.
(1) "Turbines employed in oil/gas
production or oil/gas transportation"
means any stationary gas turbine used
to provide power to extract crude oil/
natural gas from the earth or to move
crude oil/natural gas, or products
refined from these substances through
pipelines.
(m) A "Metropolitan Statistical Area"
or "MSA" as defined by the Department
of Commerce.
(n) "Offshore platform gas turbines"
means any stationary gas turbine
located on a platform in an ocean.
(o) "Garrison facility" means any
permanent military installation.
(p) "Gas turbine model" means a
group of gas turbines having the same
nominal air flow, combuster inlet
pressure, combuster inlet temperature,
firing temperature, turbine inlet
temperature and turbine inlet pressure.
(q) "Electric utility stationary gas
turbine" means any stationary gas
turbine constructed for the purpose of
supplying more than one-third of its
potential electric output capacity to any
utility power distribution system for
(r) "Emergency fuel" is a fuel fired by
a gas turbine only during circumstances,
such as natural gas supply curtailment
or breakdown of delivery system, that
make it impossible to fire natural gas in
the gas turbine.142
(s) "Regenerative cycle gas turbine"
means any stationary gas turbine that
recovers thermal energy from the
exhaust gases and utilizes the thermal
energy to preheat air prior to entering
the combustor.
§60332 Standard tor nRrogen
(a) On and after the date of the
performance test required by J 60.8 is
completed, every owner or operator
subject to the provisions of this snbpart
as specified in paragraphs (b), (c), and
(d) of this section shall comply with one
of the following, except as provided in
paragraphs (e), (f), (g), (h), (i), (J). {k}, and
(1) of this section. '«
(I) No owner or 'operator subject to
the provisions of this subpart shall
cause to be discharged into the
atmosphere from any stationary gas
turbine, any gases which contain
nitrogen oxides in excess of:
(14 4)
STD = 0.0075 v + F
32
where:
STD = allowable NO, emissions (percent by
volume at 15 percent oxygen and on a
dry basis).
Y = manufacturer's rated heat rate at
manufacturer's rated load (kilojoules per
watt hour) or, actual measured heat rate
based on lower heating value of fuel as
measured at actual peak load for the
facility. The value of Y shall not exceed
14.4 kilojoules per watt hour.
F=NO, emission allowance for fuel-bound
nitrogen as defined in part (3) of this
paragraph.
• (2) No owner or operator subject to the
provisions of this subpart shall cause to be
discharged into the atmosphere from any
stationary gas turbine, any gases which
contain nitrogen oxides in excess of:
STD = 0.0150
where:
STD=allcrwable NO, emissions (percent by
Toiume at 15 percent oxygen and on a
dry basis).
Y = manufacturer's rated heat rate at .
manufacturer's rated peak load
(kilojoules per watt hour), or actual
measured heat rate based on lower
heating value of fuel as measured at
actual peak load for the facility. The
value of Y shall not exceed 14.4
kilojoules per watt hour.
F=NO, emission allowance for fuel-bound
nitrogen as defined in part (3} of mis
paragraph.
(3) F shall be defined according to the
nitrogen content of the fuel as follows:
Fuel-Bound Nltrogwi F
(percent by weight) (NO^ percent by volume)
II c 0.015 0
0.015 < N « 0.1
O.I « N . 0.26
H > 0.2S
0.01(N)
0.004 * 0.0067(N-0.))
0.005
where:
N = the nitrogen content of tb* fuel (percent
by weight).
or.
Manufacturers may develop custom
fuel-bound nitrogen allowances for each
gas turbine model they manufacture.
These fuel-bound nitrogen allowances
shall be substantiated with data and
must be approved for use by the
Administrator before the initial
performance test required by § 60.8.
Notices of approval of custom fuel-
bound nitrogen allowances will be
published in the Federal Register.
(b) Electric utility stationary gas
turbines with a heat input at peak load
greater than 107.2 gigajoules per hour
(100 million Btu/honr) based on the
lower heating value of the fuel fired
111-80
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•haD comply with the provisions of
I 80332(a)(l).M2
(c) Stationary gat turbines with a heat
input at peak load equal to or greater
than 10.7 gigajoules per hour (10 million
Btu/hour) but less than or equal to 107.2
gigajoules per hour (100 million Btu/
hour) based on the lower heating value
of the fuel fired, shall comply with the
provisions of § 60.332(a)(2).
(id) Stationary gas turbines with a
manufacturer's rated base load at ISO
conditions of 30 megawatts or less
except as provided in 9 60-332(b) shall
comply with S 6O332(aH2).t42
(e) Stationary gas turbines with a heat
input at peak load equal to or greater
than 10.7 gigajoules per hour (10 million
Btu/hour) but less than or equal to 107.2
gigajoules per hour (100 million Btu/
hour) based on the lower heating value
of the fuel fired and that have
commenced construction prior to
October 3.1962 are exempt from
paragraph (a) of this section.
(f) Stationary gas turbines using water
or steam injection for control of NO,
emissions are exempt from paragraph
(a) when ice fog is deemed a traffic
hazard by the owner or operator of the
gas turbine.
(g) Emergency gas turbines, military
gas turbines for use in other than a
garrison facility, military gas turbines
installed for use as military training
facilities, and fire fighting gas turbines
are exempt from paragraph (a) of this
section.
(h) Stationary gas turbines engaged by
manufacturers in research and
development of equipment for bothgas
turbine emission control techniques and
gas turbine efficiency improvements are
exempt from paragraph fa) on a case-by-
case basis as determined by the
Administrator.
(i) Exemptions from the requirements
of paragraph (a) of this section will be
granted on a case-by-case basis as
determined by the Administrator in
specific geographical areas where
mandatory water restrictions are
required by governmental agencies
because of drought conditions. These
exemptions will be allowed only while'
the mandatory water restrictions are in
effect.
(j) Stationary gaa turbines with a heat
input at peak load greater than 107.2
gigajoules per hour that commenced
construction, modification, or
reconstruction between the dates of
October 3,1977, and January 27.1982,
and were required in the September 10,
1979, Federal Register (44 FR 52792) to
comply with 5 60.332fa)(l). except
electric utility stationary gas turbines,
are exempt from paragraph (a) of this
section.'42
(k) Stationary gaa turbines with a heat
input greater than or equal to 10.7
gigajoules per hour (10 million Btu/hour)
when fired with natural gas are exempt
from paragraph (a)(2) of this section
when being fired with an emergency
fuel.1'2
(1) Regenerative cycle gas turbines
with a heat input less than or equal to
107.2 gigajoules per hour (100 million
Btu/hour) are exempt from paragraph
(a) of this section.14/
§ 60.333 Standard for sulfur dioxide.
On and after the date on which the
performance test required to be .
conducted by § 60.8* is completed, every
owner or operator subject to the
provision of this subpart shall comply
with one or the other of the following
conditions:
(a) No owner or operator subject to
the provisions of this subpart shall
cause to be discharged into the
atmosphere from any stationary gas
turbine any gases which contain sulfur
dioxide in excess of 0.015 percent by
volume at 15 percent oxygen and on a
dry basis.
(b) No owner or operator subject to
the provisions of this subpart shall burn
in any stationary gas turbine any fuel
which contains sulfur in excess of 0.8
percent by weight.
§ 60.334 Monitoring of operations.
(a) The owner or operator of an"
stationary gas turbine subject to (he
provisions of this subpart and using
water injection to control NO, emissions
shall install and operate a continuous
monitoring system to monitor and record
the fuel consumption and the ratio of
water to fuel being fired in the turbine.
This system shall be accurate to within
±5.0 percent and shall be approved by
the Administrator.
(b) The owner or operator of any
.stationary gas turbine subject to the
provisions of this subpart shall monitor
sulfur content and nitrogen content of
the fuel being fired in the turbine. The
frequency of determination of these
values shall be as follows:
(1) If the turbine is supplied its fuel
from a bulk storage tank, the values
shall be determined on each occasion
that fuel is transferred to the storage
tank from any other source.
(2) If the turbine is supplied its fuel
without intermediate bulk storage the
values shall be determined and recorded
daily. Owners, operators or fuel vendors
may develop custom schedules for
determination of the values based on the
design and operation of the affected
facility and the characteristics of the
fuel supply. These custom schedules
shall be substantiated with data and
must be approved by the Administrator
before they can be used to comply with
paragraph (b) of this section.
(c) For the purpose of reports required
under § 60.7(c), periods of excess
emissions that shall be reported are
defined as follows:
(1) Nitrogen oxides. Any one-hour
period during which the average water-
to-fuel ratio, as measured by the
continuous monitoring system, falls
below the water-to-fuel ratio determined
to demonstrate compliance with § 60.332
by the performance test required in .
S 60.8 or any period during which the
fuel-bound nitrogen of the fuel is greater
than the maximum nitrogen content
allowed by the fuel-bound nitrogen
allowance used during the performance
test required in § 60.8. Each report shall
include the average water-to-fuel ratio,
average fuel consumption, ambient
conditions, gas turbine load, and
nitrogen content of the fuel during the
period of excess emissions, and the
graphs or figures developed under
§ 60.335(a).
(2) Sulfur dioxide. Any daily period
during which the sulfur content of the-
fuel being fired in the gas turbine
exceeds 0.8 percent.
(3) Ice fog. Each period during which
an exemption provided in § 60.332(g) is
in effect shall be reported in writing to
the Administrator quarterly. For each
period the ambient conditions existing
during the period, the date and time the
air pollution control system was
deactivated, and the date and time the
air pollution control system was
reactivated shall be reported. All
quarterly reports shall be postmarked by
the 30th day following the end'of each
calendar quarter.
(4) Emergency fuel. Each period
during which an exemption provided in
§ 60.332(k) is in effect shall be included
in the report required in § 60.7(c). For
each period, the type, reasons, and
duration of the firing of the emergency
fuel shall be reported.142
(Sec. 114 of the Clean Air Act •• amended (42
U.S.C. 18570-9))
{ 60.335 Test methods and procedures.
(a) The reference methods in
Appendix A to this part, except as
provided in § 60.8(b), shall be used to
determine compliance with the
standards prescribed in § 60.332 as
follows:
(1) Reference Method 20 for the
concentration of nitrogen oxides and
oxygen. For affected facilities under this
subpart, the span value shall be 300
parts per million of nitrogen oxides.
(i) The nitrogen oxides emission level
measured by Reference Method 20 shall
be adjured to ISO standard day
111-81
-------
conditions by the following ambient
condition correction factor
e19(H
where:
NO.=emissions of NO. at IS percent oxygen
and ISO standard ambient conditions.
NOEOhl°= measured NO. emissions at 15
percent oxygen, ppmv.
Pnf=reference combuster inlet absolute
pressure at 101.3 kilopascals ambient
pressure.
POM=measured combustor inlet absolute
pressure at test ambient pressure.
HOH=specific humidity of ambient air at test
e=transcendental constant (2.718).
TAIH=temperature of ambient air at test
The adjusted NO, emission level shall
be used to determine compliance with
S 60.332.
(ii) Manufacturers may develop
custom ambient condition correction
factors for each gas turbine model they
manufacture in terms of combustor inlet
pressure, ambient air pressure, ambient
air humidity and ambient air
temperature to adjust the nitrogen
oxides emission level measured by the
performance test as provided for in
S 60.8 to ISO standard day conditions.
These ambient condition correction
factors shall be substantiated with data
and must be approved for use by. the
Administrator before the initial
performance test required by S 60.8.
Notices of approval of custom ambient
condition correction factors will be
published in the Federal Register.
(iii) The water-to-fuel ratio necessary
to comply with § 60.332 will be
determined during the initial
performance test by measuring NO. ' '
fnission using Reference Method 20 and
obs
the water-to-fuel ratio necessary to
comply with { 60.332 at 30,50,75, and
100 percent of peak load or at four
points in the normal operating range of
the gas turbine, including the minimum
point in the range and peak load. All
loads shall be corrected to ISO
conditions using the appropriate
equations supplied by the manufacturer.
(2) The analytical methods and
procedures employed to determine the
nitrogen content of the fuel being Bred
shall be approved by the Administrator
and shall be accurate to within ±5
percent.
(b) The method for determining
compliance with { 60.333, except as
provided in { 60.8(b), shall be as
follows:
(1) Reference Method 20 for the
concentration of sulfur dioxide and
oxygen or
(2) ASTM D2B80-71 for the sulfur
' content of liquid fuels and ASTM
D1072-70 for the sulfur content of
gaseous fuels. These methods shall also
be used to comply with S 60.334(b). •
(c) Analysis for the purpose of
determining the sulfur content and the
nitrogen content of the fuel as required
by { 60.334(b), this subpart, maybe
performed by the owner/operator, a
service contractor retained by the
owner/operator, the fuel vendor, or any
other qualified agency provided that the
analytical methods employed by these
Agencies comply with the applicable
paragraphs of this section.
(Sec. 114 of the Clean Air Act as amended [42
U.S.C. 18570-01]).
Proposed/effective
42 FR 53782, 10/3/77
Promulgated'
44 FR 52792, 9/10/79 (101)
Revised
4TTF3767. 1/27/82 (142)
111-82
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MIHI —
raeinea fer iirae
Plaints 85
§ 60.340 Applicability end designation of
affected facility.
(a) The provisions of this subpart
are applicable to the following affect-
ed facilities used in the manufacture1
of lime: rotary lime kilns and lime hy-
drators.
(b) The provisions of this subpart
are not applicable to facilities used in
the manufacture of lime at kraft pulp
mills.
(c) Any facility under paragraph (a)
of this section that commences con-
struction or modification after May 3,
1977, is subject to the requirements of
this part.
§60.341 Definitions.
As used in this subpart, all terms not
defined herein shall have the same
meaning given them in the Act and in
subpart A of this part.
(a) "Lime manufacturing plant" in-
cludes any plant which produces a
lime product from limestone by calci-
nation. Hydration of the lime product
is also considered to be part of the
source.
(b) "Lime product" means the prod-
uct of the calcination process includ-
ing, but not limited to, calcitic lime,
dolomitic lime, and dead-burned dolo-
mite.
(c) "Rotary lime kiln" means a unit
with an inclined rotating drum which
is used to produce a lime product from
limestone by calcination.
(d) "Lime hydrator" means a unit
used to produce hydrated lime prod-
uct.
§ 60.342 Standard for particulate matter.
(a) On and after the date on which
the performance test required to be
conducted by §60.8 is completed, no
owner or operator subject to the provi-
sions of this subpart shall cause to be
discharged into the atmosphere:
(1) Prom any rotary lime kiln any
gases which:
(i) Contain participate matter in
excess of 0.15 kilogram per megagram
of limestone feed (0.30 Ib/ton).
(ii) Exhibit 10 percent opacity or
greater.
(2) Prom any lime hydrator any
gases which contain particulate matter
in excess of 0.075 kilogram per mega-
gram of lime feed (0.15 Ib/ton).
§ 60.343 Monitoring of emissions end op-
erations.
(a) The owner or operator subject to
the provisions of this subpart shall in-
stall, calibrate, maintain, and operate
a continuous monitoring system,
except as provided in paragraph (b) of
this section, to monitor and record the
opacity of a representative portion of
the gases discharged into the atmos-
phere from any rotary lime kiln. The
span of this system shall be set at 40
percent opacity.
(b) The owner or operator of any
rotary lime kiln using a wet scrubbing
emission control device subject to the
provisions of this subpart shall not be
required to monitor the opacity of the
gases discharged as required in para-
graph (a) of this section, but shall in-
stall, calibrate, maintain, and operate
the following continuous monitoring
devices:
(DA monitoring device for the con-
tinuous measurement of the pressure
loss of the gas stream through the
scrubber. The monitoring device must
be accurate within ±250 pascals (one
inch of water).
(2) A monitoring device for the con-
tinuous measurement of the scrubbing
liquid supply pressure to the control
device. The monitoring device must be
accurate within ±5 percent of design
scrubbing liquid supply pressure.
(c) The owner or operator of any
lime hydrator using a wet scrubbing
emission control device subject to the
provisions of this subpart shall install,
calibrate, maintain, and operate the
following continuous monitoring de-
vices:
(DA monitoring device for the con-
tinuous measuring of the scrubbing
liquid flow rate. The monitoring
device must be accurate within ±5 per-
cent of design scrubbing liquid flow
rate.
(2) A monitoring device for the con-
. tinuous measurement of the electric
current, in amperes, used by the scrub-
ber. The monitoring device must be ac-
curate within ±10 percent over its
normal operating range.
(d) For the purpose of conducting &
performance test under §60.8, the
owner or operator of any lime manu-
facturing plant subject to the provi-
sions of this subpart shall install, cali-
brate, maintain, and operate a device
for measuring the mass rate of lime-
stone feed to any affected rotary lime
kiln and the mass rate of lime feed to
any affected lime hydrator. The mea-
suring device used must be accurate to
within ±5 percent of the mass rate
over its operating range.
(e) For the purpose of reports re-
quired under §60.7(c), periods of
excess emissions that shall be reported
ore defined as all six-minute periods
during which the average opacity of
the plume from any lime kiln subject
to paragraph (a) of this subpart is 10
percent or greater.
(Sec. 114 of the Clean Air Act. as amended
(42 UJ3.C. 7414).)
g 50.344 Test methods and procedures.
(a) Reference methods in Appendix
A of this part, except as provided
under §60.8(b), shall be used to deter-
mine compliance with §80.322(a) as
follows:
(1) Method 5 for the measurement
of particulate matter,
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and volu-
metric flow rate,
(4) Method 3 for gas analysis,
(5) Method 4 for stack gas moisture,
and
(6) Method 9 for visible emissions.
(b) For Method 5, the sampling time
for each run shall be at least 60 min-
utes and the sampling rate shall be at
least 0.85 std m'/h, dry basis (0.53
dscf/min), except that shorter sam-
pling times, when necessitated by pro-
cess variables or other factors, may be
approved by the Administrator.
(c) Because of the high moisture
content «!0 to 85 percent by volume)
of the exhaust gases from hydretors,
the Method 5 sample train may be
modified to include a calibrated orifice
Immediately following the sample
nozzle when testing lime hydrators. In
this configuration, the sampling rate
necessary for maintaining isokinetic
conditions can be directly related to
exhaust gas velocity without a correc-
tion for moisture content. Extra care
should be exercised when cleaning the
sample train with the orifice in this
position following the test runs.
(Sec. 114 of the Clean Air Act. as amended
(42 UJS.C. 7414).)
Proposed/effecti ve
42 FR 22506, 5/3/77
Promulgated
43 FR 9452, 3/7/78 (85)
111-83
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Subpart KK—Standards of
Performance for Lead-Add Battery
Manufacturing Plants <45
560.370 Applicability and designation of
affected facility.
(a) The provisions of this subpart are
applicable to the affected facilities listed
in paragraph (b) of this section at any
lead-acid battery manufacturing plant
that produces or has the design capacity
to produce in one day (24 hours)
batteries containing an amount of lead
equal to or greater than 5.9 Mg (6.5 tons).
(b) The provisions of this subpart are
applicable to the following affected
facilities used in the manufacture of
lead-acid storage batteries:
(1) Grid casting facility.
(2) Paste mixing facility.
(3) Three-process operation facility.
(4) Lead oxide manufacturing facility.
(5) Lead reclamation facility.
(6) Other lead-emitting operations.
(c) Any facility under paragraph (b) of
this section the construction or
modification of which is commenced
after January 14,1980, is subject to the
requirements'of this subpart.
J 60.371 Definition*.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart A
of this part.
(a) "Grid casting facility" means the
facility which includes all lead melting
pots and machines used for casting the
grid used in battery manufacturing.
(b) "Lead-acid battery manufacturing
plant" means any plant that produces a
storage battery using lead and lead
compounds for the plates and sulfuric
acid for the electrolyte.
(c) "Lead oxide manufacturing
facility" means a facility that produces
lead oxide from lead, including product
recovery.
(d) "Lead reclamation facility" means
the facility that remelts lead scrap and
casts it into lead ingots for use in the
battery manufacturing process, and
which is not a furnace affected under
Sub; ..rt L of this part.
(e) "Other lead-emitting operation"
means any lead-acid battery
manufacturing plant operation from
which lead emissions are collected and
ducted to the atmosphere and which is
not part of a grid casting, lead oxide
manufacturing, lead reclamation, paste
mixing, or three-process operation
facility, or a furnace affected under
Subpart L of this part.
(f) "Paste mixing facility" means the
facility including lead oxide storage,
conveying, weighing, metering, and
charging operations; paste blending,
handling, and cooling operations; and
plate pasting, takeoff, cooling, and
drying operations.
(g) "Three-process operation facility"
means the facility including those
processes involved with plate stacking,
burning or strap casting, and assembly
of elements into the battery case.
860.372 Standards for toad.
(a) On and after the date on which the
performance test required to be
conducted by S 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere:
(1) From any grid casting facility any
gases that contain lead in excess of 0.40
milligram of lead per dry standard cubic
meter of exhaust (0.000176 gr/dscf).
(2) From any paste mixing facility any
gases that contain in excess of 1.00
milligram of lead per dry standard cubic
meter of exhaust (0.00044 gr/dscf).
(3) From any three-process operation
facility any gases that contain in excess
of 1.00 milligram of lead per dry
standard cubic meter of exhaust (0.00044
gr/dscf).
(4) From any lead oxide
manufacturing facility any gases that
contain in excess of 5.0 milligrams of
lead per kilogram of lead feed (0.010 lb/
ton).
(5) From any lead reclamation facility
any gases that contain in excess of 4.50
milligrams of lead per dry standard
cubic meter of exhaust (0.00198 gr/dscf).
(6) From any other lead-emitting
operation any gases that contain in
excess of 1.00 milligram per dry
standard cubic meter of exhaust (0.00044
gr/dscf).
[7] From any affected facility other
than a lead reclamation facility any
gases with greater than 0 percent
opacity (measured according to Method
9 and rounded to the nearest whole
percentage).
(8) From any lead reclamation facility
any gases with greater than 5 percent
opacity (measured according to Method
9 and rounded to the nearest whole
percentage).
(b) When two or more facilities at the
same plant (except the lead oxide
manufacturing facility) are ducted to a
common control device, an equivalent
standard for the total exhaust from the
commonly controlled facilities shall be
determined as follows:
s.=
Where:
S«=is the equivalent standard for the total
exhaust stream.
S.=is the actual standard for each exhaust
stream ducted to the control device.
N=is the total number of exhaust streams
ducted to the control device.
Q,4.=ls the dry standard volumetric flow
rate of the effluent gas stream from each
facility ducted to the control device.
QnT = is the total dry standard volumetric
flow rate of all effluent gas streams
ducted to the control device.
§60.373 Monitoring of emiaakm* and
operation*.
The owner or operator of any lead-
acid battery manufacturing facility
subject to the provisions of this subpart
and controlled by a scrubbing system^)
shall install, calibrate, maintain, and
operate a monitoring device(s) that
measures and records the pressure drop
across the scrubbing system(s) at least
once every 15 minutes. The monitoring
device shall have an accuracy of ±5
percent over its opera ting .range.
(Sec. 114 of the Clean Air Act as amended (42
U.S.C. 7414))
§60.374 T««t methods and procedure*.
(a) Reference methods in Appendix A
of this part, except as provided under
§ 60.8(b), shall be used to determine
compliance according to § 60.8 as
follows:
(1) Method 12 for the measurement of
lead concentrations,
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and
volumetric flow rate, and
(4) Method 4 for stack gas moisture.
(b) For Method 12, the sampling time
for each run shall be at least 60 minutes
and the sampling rate shall be at least
0.85 dscm/h (0.53 dscf/min), except that
shorter sampling times, when
necessitated by process variables or
other factors, may be approved by the
Administrator.
(c) When different operations in a
three-process operation facility are
ducted to separate control devices, the
lead emission concentration from the
facility shall be determined using the
equation:
Cm
a=l
a=l
Where:
CpB,.=is the facility emission concentration
for the entire facility.
N=is the number of control devices to which
separate operations in the facility are
ducted.
Cn>=is the emission concentration from
'each control device.
111-84
-------
0.^=18 the dry standard* volumetric flow
rate of the effluent gas stream from each
control device.
0^=18 the total dry standard vohunetric
flow rate from all of the control devices.
(d) For lead oxide manufacturing
facilities, the average lead feed rate to a
facility, expressed in kilograms per hour,
shall be determined for each test run as
follows:
(1) Calculate the total amount of lead
charged to the facility during the run by
multiplying the number of lead pigs
(ingots) charged during the run by the
average mass of a pig in kilograms or by
another suitable method.
(2) Divide the total amount of lead
charged to the facility during the run by
the duration of the run in hours.
(e) Lead emissions from lead oxide
manufacturing facilities, expressed In
milligrams per kilogram of lead charged.
shall be determined using the following
equation:
Wnere:
E,» -is the lead emission rate from the
facility in milligrams per kilogram of lead
charged.
Cn = is the concentration of lead in the
exhaust stream in milligrams per dry
standard cubic meter as determined
according to paragraph (a)(lj of this
section.
Q«i = iB the dry standard volumetric flow rate
in dry standard cubic meters per hour as
determined according to paragraph (a)(3)
of this section.
F = is the lead feed rate to the facility in
kilograms per hour as determined
according to paragraph (d) of this
section.
(Sec. 114 of the Clean Air Act as amended (42
U.S.C. 7414))
Proposed/effective
45 FR 2790, 1/14/80
Promulgated
47 FR 16564, 4/16/82 (145)
111-85
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Subpart MM—Standards of
Performance for Automobile and Light
Duty Truck Surface Coating
Operations 124
5 60.390 Applicability and designation of
aftoctod facility.
(a) The provisions of this subpart
apply to the following affected facilities
in an automobile or light-duty truck
assembly plant: each prime coat
operation, each guide coat operation,
and each topcoat operation.
(b) Exempted from the provisions of
this subpart are operations used to coat
plastic body components or all-plastic
automobile or light-duty truck bodies on
separate coating lines. The attachment
of plastic body parts to a metal body
before the body is coated does not cause
the metal body coating operation to be
exempted.
(c) The provisions of this subpart
apply to any affected facility identified
in paragraph (a) of this section that
begins construction, reconstruction, or
modification after October 5,1979.
§ 60.391 Defintttona.
(a) All terms used in this subpart that
are not defined below have the meaning
given to them in the Act and in Subpart
A of this part.
"Applied coating solids" means the
volume of dried or cured coating solids
which is deposited and remains on the
surface of the automobile or light-duty
truck body.
"Automobile" means a motor vehicle
capable of carrying no more than 12
passengers.
"Automobile and light-duty truck
body" means the exterior surface of an
automobile or light-duty truck including
hoods, fenders, cargo boxes, doors, and
grill opening panels.
"Bake oven" means a device that uses
heat to dry or cure coatings.
"Electrodeposition (EDP)" means a
method of applying a prime coat by
which the automobile or light-duty truck
body is submerged in a tank filled with
coating material and an electrical field
is used to effect the deposition of the
coating material on the body.
"Electrostatic spray application"
means a spray application method that
uses an electrical potential to increase
the transfer efficiency of the coating
solids. Electrostatic spray application
can be used for prime coat, guide coat,
or topcoat operations.
"Flash-off area" means the structure
on automobile and light-duty truck
assembly lines between the coating
application system (dip tank or spray
booth) and the bake oven.
"Guide coat operation" means the
guide coat spray booth, flash-off area
and bake oven(s) which are used to
apply and dry or cure a surface coating
between the prime coat and topcoat
operation on the components of
automobile and light-duty truck bodies.
"Light-duty truck" means any motor
vehicle rated at 3,850 kilograms gross
vehicle weight or less, designed mainly
to transport property.
"Plastic body" means an automobile
or light-duty truck body constructed of
synthetic organic material.
"Plastic body component" means any
component of an automobile or light-
duty truck exterior surface constructed
of synthetic organic material.
"Prime coat operation" means the
prime coat spray booth or dip tank,
flash-off area, and bake oven(s) which
are used to apply and dry or cure the
initial coating on components of
automobile or light-duty truck bodies.
"Purge" or "line purge" means the
coating material expelled from the spray
system when clearing it.
"Solvent-borne" means a coating
which contains five percent or less
water by weight in its volatile fraction.
"Spray application" means a method
of applying coatings by atomizing the
coating material and directing the
atomized material toward the part to be
coated. Spray applications can be used
for prime coat, guide coat, and topcoat
operations.
"Spray booth" means a structure
housing automatic or manual spray
application equipment where prime
coat, guide coat, or topcoat is applied to
components of automobile or light-duty
truck bodies.
"Surface coating operation" means
any prime coat, guide coat, or topcoat
operation on an automobile or light-duty
truck surface coating line.
"Topcoat operation" means the
topcoat spray booth, flash-off area, and
bake oven(s) which are used to apply
and dry or cure the final coating(s) on
components of automobile and light-
duty truck bodies.
"Transfer efficiency" means the ratio
of the amount of coating solids
transferred onto the surface of a part or
product to the total amount of coating
solids used.
"VOC content" means all volatile
organic compounds that are in a coating
expressed as kilograms of VOC per liter
of coating solids.
"Waterborne" or "water reducible"
means a coating which contains more
than five weight percent water in its
volatile fraction.
(b) The nomenclature used in this
subpart has the following meanings:
C.j = concentration of VOC (as carbon) in the
effluent gas flowing through stack (j)
leaving the control device (parts per million
by volume).
Cb, = concentration of VOC (as carbon) in the
effluent gas flowing through stack (ij
entering the control device (parts per
million by volume),
Cm = concentration of VOC (as carbon) in the
effluent gas flowing through exhaust stack
(k) not entering the control device (parts
per million by volume),
Dc, = density of each coating (i) as received
(kilograms per liter),
Daj = density of each type VOC dilution
solvent (j) added to the coatings, as
received (kilograms per liter),
Dr=density of VOC recovered from an
affected facility (kilograms per liter),
E = VOC destruction efficiency of the control
device,
F=fraction of total VOC which is emitted by
an affected facility that enters the control
device,
G = volume weighted average mass of VOC
per volume of applied solids (kilograms per
liter),
Le, = volume of each coating (i) consumed, as
received (liters),
Ui'/=volume of each coating (i) consumed by
each application method (1), as received
liters),
Ljj = volume of each type VOC dilution
solvent (j) added to the coatings, as
received (liters),
L, = volume of VOC recovered from an
affected facility (liters),
L, = volume of solids in coatings consumed
(liters),
Ma = total mass of VOC in dilution solvent
(kilograms),
Mo = total mass of VOC in coatings as
received (kilograms).
M, = total mass of VOC recovered from an
affected facility (kilograms),
N-volume weighted average mass of VOC
per volume of applfed coating solids after
the control device
kilograms of VOC
Her of applied solids
Q.J = volumetric flow rate of the effluent gas
flowing through stack (j) leaving the control
device (dry standard cubic meters per
hour),
Qbl = volumetric flow rate of the effluent gas
flowing through stack (i) entering the
control device (dry standard cubic meters
per hour).
Qfk = volumetric flow rate of the effluent gas
flowing through exhaust stack (k) not
entering the control device (dry standard
cubic meters per hour).
T = overall transfer efficiency.
T, = transfer efficiency for application method
111-86
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,i = proportion of solids by volume in each
coating (i) as received
6 liter solids^
iter coatingy ,
Wo,=proportion of VOC by weight in each
coating (i), as received
kilograms VOC
dlograms coating
§ 60.392 Standards for volatile organic
compounds
On and after the date on which the
initial performance test required by
§ 60.8 is completed, no owner or
operator subject to the provisions of this
subpart shall discharge or cause the
discharge into the atmosphere from any
affected facility VOC emissions in
excess of:
(a) 0.16 kilograms o' VOC per liter of
applied coating solids from each prime
coat operation.
(b) 1.40 kilograms of VOC per liter of
applied coating solids from each guide
coat operation.
(c) 1.47 kilograms of VOC per liter of
applied coating solids from each topcoat
operation.
§ 60.393 Performance test and compliance
provisions.
(a) Sections 60.8 (d) and (f) do not
apply to the performance test
procedures required by this section.
(b) The owner or operator of an
affected facility shall conduct an initial
performance test in accordance with
§ 60.8(a) and thereafter for each
calendar month for each affected facility
according to the procedures in this
section.
(c) The owner or operator shall use
the following procedures for determining
the monthly volume weighted average
mass of VOC emitted per volume of
applied coating solids.
(1) The owner or operator shall use
the following procedures for each
affected facility which does not use a
capture system and a control device to
comply with the applicable emission
limit specified under § 60.392.
(i) Calculate the volume weighted
average mass of VOC per volume of
applied coating solids for each calendar
month for each affected facility. The
owner or operator shall determine the
composition of the coatings by
formulation data supplied by the
manufacturer of the coating or from data
determined by an analysis of each
coating, as received, by Reference
Method 24. The Administrator may
require the owner or operator who uses
formulation data supplied by the
manufacturer of the coating to
determine data used in the calculation
of the VOC content of coatings by
Reference Method 24 or an equivalent or
alternative method. The owner or
operator shall determine from company
records on a monthly basis the volume
of coating consumed, as received, and
the mass of solvent used for thinning
purposes. The volume weighted average
of the total mass of VOC per volume of
coating solids used each calendar month
will be determined by the following
procedures.
(A) Calculate the mass of VOC used
in each calendar month for each
affected facility by the following
equation where "n" is the total number
of coatings used and "m" is the total
number of VOC solvents used:
Dd
m
+ I
j«l
[2 L.U Da will be zero if no VOC solvent
is added to the coatings, as received].
(b) Calculate the total volume of
coating solids used in each calendar
month for each affected facility by the
following equation where "n" is the total
number of coatings used:
Ls =
n
I I
ci
'si
(c) Select the appropriate transfer
efficiency (T) from the following tables
for each surface coating operation:
Application Method
Transfer
efficiency
An Atomized Spray (watertxxne coating)
Air Atomized Spray (solvent-borne coating)...
Manual Electrostatic Spray
Automatic Electrostatic Spray
Electrodeposrtion
0.39
0.50
0.75
0.95
1.00
The values in the table above represent
an overall system efficiency which
includes a total capture of purge. If a
spray system uses line purging after
each vehicle and does not collect any of
the purge material, the following table
shall be used:
Application Method
Transfer
efficiency
Air Atomized Spray (waterbome coating)
Air Atomized Spray (solvent-borne coating)
Manual Electrostatic Spray
Automatic Electrostatic Spray...
0.30
0.40
0.62
0.75
If the owner or operator can justify to
the Administrator's satisfaction that
other values for transfer efficiencies are
appropriate, the Administrator will
approve their use on a case-by-case
basis.
(1) When more than one application
method (/) is used on an individual
surface coating operation, the owner or
operator shall perform an analysis to
determine an average transfer efficiency
by the following equation where "n" is
the total number of coatings used and
"p" is the total number of application
methods:
n p
i i
i=l £=1
si
(D) Calculate the volume weighted
average mass of VOC per volume of
applied coating solids (G) during each
calendar month for each affected facility
by the following equation:
G =
LsT
(ii) If the volume weighted average
mass of VOC per volume of applied
coating solids (G), calculated on a
calendar month basis, is less than or
equal to the applicable emission limit
specified in § 60.392, the affected facility
is in compliance. Each monthly
calculation is a performance test for the
purpose of this subpart.
111-87
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(2) The owner or operator shall use
the following procedures for each
affected facility which uses a capture
system and a control device that
destroys VOC (e.g., incinerator) to
comply with the applicable emission
limit specified under § 60.392.
(i) Calculate the volume weighted
average mass of VOC per volume of
applied coating solids (C) during each
calendar month for each affected facility
as described under § 60.393(c)(l)(i).
(ii) Calculate the volume weighted
average mass of VOC per volume of
applied solids emitted after the control
device, by the following equation:
N = G[1-FE)
(A) Determine the fraction of total
VOC which is emitted by an affected
facility that enters the control device by
using the following equation where "n"
is the total number of stacks entering the
control device and "p" is the total
number of stacks not connected to the
control device:
F =
1=1
k=l
If the owner can justify to the
Administrator's satisfaction that another
method will give comparable results, the
Administrator will approve its use on a
case-by-case basis.
(1) In subsequent months, the owner
or operator shall use the most recently
determined capture fraction for the
performance test.
(B) Determines the destruction
efficiency of the control device using
values of the volumetric flow rate of the
gas streams and the VOC content (as
carbon) of each of the gas streams in
and out of the device by the following
equation where "n" is the total number
of stacks entering the control device and
"m" is the total number of stacks leaving
the control device:
E=
m
i Cbi -j Caj
(7) In subsequent months, the owner
or operator shall use the most recently
determined VOC destruction efficiency
for the performance test.
(C) If an emission control device
controls the emissions from more than
one affected facility, the owner or
operator shall measure the VOC
concentration (Cbi) in the effluent gas
entering the control device (in parts per
million by volume) and the volumetric
flow rate (Qbi) of the effluent gas (in dry
standard cubic meters per hour) entering
the device through each stack. The
destruction or removal efficiency
determined using these data shall be
applied to each affected facility served
by the control device.
(iii) If the volume weighted average
mass of VOC per volume of applied
solids emitted after the control device
(N) calculated on a calendar month
basis is less than or equal to the
applicable emission limit specified in
§ 60.392, the affected facility is in
compliance. Each monthly calculation is
a performance test for the purposes of
this subpart.
(3) The owner or operator shall use
the following procedures for each
affected facility which uses a capture
system and a control device that
recovers the VOC (e.g., carbon
adsorber) to comply with the applicable
emission limit specified under § 60.392.
(i) Calculate the mass of VOC
(M0-(-Md) used during each calendar
month for each affected facility as
described under § 60.393(c)(l)(i).
(ii) Calculate the total volume of
coating solids (Ls) used in each calendar
month for each affected facility as
described under § 60.393(c)(l)(i).
(iii) Calculate the mass of VOC
recovered (Mr) each calendar month for
each affected facility by the following
equation: Mr = LrDr
(iv) Calculate the volume weighted
average mass of VOC per volume of
applied coating solids emitted after the
control device during a calendar month
by the following equation:
N =
"o + Md - Mr
LsT
(v) If the volume weighted average
mass of VOC per volume of applied
solids emitted after the control device
(N) calculated on a calendar month
basis is less than or equal to the
applicable emission limit specified in
§ 60.392. the affected facility is in
compliance. Each monthly calculation is
a performance test for the purposes of
this subpart.
§ 60.394 Monitoring of emissions and
operations.
The owner or operator of an affected
facility which uses an incinerator to
comply with the emission limits
specified under § 60.392 shall install,
calibrate, maintain, and operate
temperature measurement devices as
prescribed below:
(a) Where thermal incineration is
used, a temperature measurement
device shall be installed in the firebox.
Where catalytic incineration is used, a
temperature measurement device shall
be installed in the gas stream
immediately before and after the
catalyst bed.
(b) Each temperature measurement
device shall be installed, calibrated, and
maintained according to accepted
practice and the manufacturer's
specifications. The device shall have an
accuracy of the greater of ±0.75 percent
of the temperature being measured
expressed in degrees Celsius or ±2.5° C.
(c) Each temperature measurement
device shall be equipped with a
recording device so that a permanent
record is produced.
(Section 114 of the Clean Air Act as amended
(42 U.S.C. 74140))
§ 60.395 Reporting and recordkeeplng
requirements.
(a) Each owner or operator of an
affected facility shall include the data
outlined in subparagraphs (1) and (2) in
the initial compliance report required by
§60.8.
(1) The owner or operator shall report
the volume weighted average mass of
VOC per volume of applied coating
solids for each affected facility.
(2) Where compliance is achieved
through the use of incineration, the
owner or operator shall include the
following additional data in the control
device initial performance test requried
by | 60.8(a) or subsequent performance
tests at which destruction efficiency is
determined: the combustion temperature
(or the gas temperature upstream and
downstream of the catalyst bed), the
total mass of VOC per volume of
applied coating solids before and after
the incinerator, capture efficiency, the
destruction efficiency of the incinerator
used to attain compliance with the
applicable emission limit specified in
§ 60.392 and a description of the method
used to establish the fraction of VOC
captured and sent to the control device.
111-88
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(b) Following the initial report, each
owner or operator shall report the
volume weighted average mass of VOC
per volume of applied coating solids for
each affected facility during each
calendar month in which the affected
facility is not in compliance with the
applicable emission limit specified in
§ 60.392. This report shall be
postmarked not later than ten days after
the end of the calendar month that the
affected facility is not in compliance.
Where compliance is achieved through
the use of a capture system and control
device, the volume weighted average
after the control device should be
reported.
(c) Where compliance with § 60.392 is
achieved through the use of incineration,
the owner or operator shall continuously
record the incinerator combustion
temperature during coating operations
for thermal incineration or the gas
temperature upstream and downstream
of the incinerator catalyst bed during
coating operations for catalytic
incineration. The owner or operator
shall report quarterly as defined below.
(1) For thermal incinerators, every
three-hour period shall be reported
during which the average temperature
measured is more than 28°C less than
the average temperature during the most
recent control device performance test
at which the destruction efficiency was
determined as specified under § 60.393.
(2) For catalytic incinerators, every
three-hour period shall be reported
during which the average temperature
immediately before the catalyst bed,
when the coating system is operational,
is more than 28" C less than the average
temperature immediately before the
catalyst bed during the most recent
control device performance test at
which destruction efficiency was
determined as specified under § 60.393.
In addition, every three-hour period
shall be reported each quarter during
which the average temperature
difference across the catalyst bed when
the coating system is operational is less
than 80 percent of the average
temperature difference of the device
during the most recent control device
performance test at which destruction
efficiency was determined as specified
under § 60.393.
(3) For thermal and catalytic
incinerators, if no such periods occur,
the owner or operator shall submit a
negative report.
(d) The owner or operator shall notify
the Administrator 30 days in advance of
any test by Reference Method 25.
(Section 114 of the Clean Air Act as amended
(42 U.S.C. 7414))
§ 60.396 Reference methods and
procedure*.
(a) The reference methods in
Appendix A to this part, except as
provided in § 60.8 shall be used to
conduct performance tests.
(1) Reference Method 24 or an
equivalent or alternative method
approved by the Administrator shall be
used for the determination of the data
used in the calculation of the VOC
content of the coatings used for each
affected facility. Manufacturers'
formulation data is approved by the
Administrator as an alternative method
to Method 24. In the event of dispute.
Reference Method 24 shall be the referee
method.
(2) Reference Method 25 or an
equivalent or alternative method
approved by the Administrator shall be
used for the determination of the VOC
concentration in the effluent gas
entering and leaving the emission
control device for each stack equipped
with an emission control device and in
the effluent gas leaving each stack not
equipped with a control device.
(3) The following methods shall be
used to determine the volumetric flow
rate in the effluent gas in a stack:
(i) Method 1 for sample and velocity
traverses,
(ii) Method 2 for velocity and
volumetric flow rate,
(iii) Method 3 for gas analysis, and
(iv) Method 4 for stack gas moisture.
(b) For Reference Method 24, the
coating sample must be a 1-liter sample
taken in a 1-liter container.
(c) For Reference Method 25, the
sampling time for each of three runs
must be at least one hour. The minimum
sample volume must be 0.003 dscm
except that shorter sampling times or
smaller volumes, when necessitated by
process variables or other factors, may
be approved by the Administrator. The
Administrator will approve the sampling
of representative stacks on a case-by-
case basis if the owner or operator can
demonstrate to the satisfaction of the
Administrator that the testing of
representative stacks would yield
results comparable to those that would
be obtained by testing all stacks.
(Sec. 114 of the Clean Air Act as amended (42
U.S.C. 7414))
§ 60.397 Modifications.
The following physical or operational
changes are not, by themselves,
considered modifications of existing
facilities:
(1) Changes as a result of model year
• changeovers or switches to larger cars.
(2) Changes in the application of the
coatings to increase coating film
thickness.
Proposed/effective
44 FR 57792, 10/5/79
Promulgated
45 KR 85410, 12/24/80 (124)
111-89
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Subpart NN—Standards of
Performance for Phosphate Rock
Plants 146
§ 60.400 Applicability and designation of
affected facility.
(a) The provisions of this subpart are
applicable to the following affected
facilities used in phosphate rock plants
which have a maximum plant
production capacity greater than 3.6
megagrams per hour (4 tons/hr): dryers,
calciners, grinders, and ground rock
handling and storage facilities, except
those facilities producing or preparing
phosphate rock solely for consumption
in elemental phosphorus production.
(b) Any facility under paragraph (a) of
this section which commences
construction, modification, or
reconstruction after September 21,1979,
is subject to the requirements of this
part.
§ 60.401 Definitions.
(a) "Phosphate rock plant" means any
plant which produces or prepares
phosphate rock product by any or all of
the following processes: Mining,
beneficiation, crushing, screening,
cleaning, drying, calcining, and grinding.
(b) "Phosphate rock feed" means all
material entering the process unit
including, moisture and extraneous
material as well as the following ore
minerals: Fluorapatite, hydroxylapatite,
chlorapatite, and carbonateapatite.
(c) "Dryer" means a unit in which the
moisture content of phosphate rock is
reduced by contact with a heated gas
stream.
(d) "Calciner" means a unit in which
the moisture and organic matter of
phosphate rock is reduced within a
combustion chamber.
(e) "Grinder" means a unit which is
used to pulverize dry phosphate rock to
the final product size used in the
manufacture of phosphate fertilizer and
does not include crushing devices used
in mining.
(f) "Ground phosphate rock handling
and storage system" means a system
which is used for the conveyance and
storage of ground phosphate rock from
grinders at phosphate rock plants.
(g) "Beneficiation" means the process
of washing the rock to remove
impurities or to separate size fractions.
§ 60.402 Standard for partlculate matter.
(a) On and after the date on which the
performance test required to be
conducted by § 60.8 is completed, no
owner or operator subject to the
provisions of this subpart shall cause to
be discharged into the atmosphere:
(1) From any phosphate rock dryer
any gases which:
(i) Contain particulate matter in
excess of 0.030 kilogram per megagram
of phosphate rock feed (0.06 Ib/ton), or
(ii) Exhibit greater than 10-percent
opacity.
(2) prom any phosphate rock calciner
processing unbeneficiated rock or
blends of beneficiated and
unbeneficiated rock, any gases which:
(i) Contains particulate matter in
excess of 0.12 kilogram per megagram of
phosphate jock feed (0.23 Ib/ton), or
(ii) Exhibit greater than 10-percent
opacity,
(3) From any phosphate rock calciner
processing beneficiated rock any gases
which:
(i) Contain particulate matter in
excess of 0.055 kilogram per megagram
of phosphate rock feed (0.11 Ib/ton), or
(ii) Exhibit greater than 10-percent
opacity.
(4) From any phosphate rock grinder
any gases which:
(i) Contain particulate matter in
excess of 0.006 kilogram per megagram
of phosphate rock feed (0.012 Ib/ton), or
(ii) Exhibit greater than zero-percent
opacity.
(5) From any ground phosphate rock
handling and storage system any gases
which exhibit greater than zero-percent
opacity.
§ 60.403 Monitoring of emissions and
operations.
(a) Any owner or operator subject to
the provisions of this subpart shall
install, calibrate, maintain, and operate
a continuous monitoring system, except
as provided in paragraphs (b) and (c) of
this section, to monitor and record the
opacity of the gases discharged into the
atmosphere from any phosphate rock
dryer, calciner, or grinder. The span of
this system shall be set at 40-percent
opacity.
(b) For ground phosphate rock storage
and handling systems, continuous
monitoring systems for measuring
opacity are not required.
(c) The owner or operator of any
affected phosphate rock facility using a
wet scrubbing emission control device
shall not be subject to the requirements
in paragraph (a) of this section, but shall
install, calibrate, maintain, and operate
the following continuous monitoring
devices:
(1) A monitoring device for the
continuous measurement of trie pressure
loss of the gas stream through the
scrubber. The monitoring device must be
certified by the manufacturer to be
accurate within ±250 pascals (±1 inch
water) gauge pressure.
(2) A monitoring device for the
continuous measurement of the
scrubbing liquid supply pressure to the
control device. The monitoring device
must be accurate within ±5 percent of
design scrubbing liquid supply pressure.
(d) For the purpose of conducting a
performance test under 5 60.8, the owner
or operator of any phosphate rock plant
subject to the provisions of this subpart
shall install, calibrate, maintain, and
operate a device for measuring the
phosphate rock feed to any affected
dryer, calciner, or grinder. The
measuring device used must be accurate
to within ±5 percent of the mass rate
over its operating range.
(e) For the purpose of reports required
under § 60.7(c), periods of excess
emissions that shall be reported are
defined as all 6-minute periods during
which the average opacity of the plume
from any phosphate rock dryer, calciner.
or grinder subject to paragraph (a) of
this section exceeds the applicable
opacity limit.
(f) Any owner or operator subject to
the requirements under paragraph (c) of
this section shall report for each
calendar quarter all measurement
results that are less than 90 percent of
the average levels maintained during the
most recent performance test conducted
under J 60.8 in which the affected
facility demonstrated compliance with
the standard under S 60.402.
(Sec. 114. Clean Air Act as amended (42
U.S.C. 7414)) |
§ 60.404 Test methods and procedures.
(a) Reference methods in Appendix A
of this part, except as provided under
,§ 60.8(b), shall be used to determine
compliance with § 60.402 as follows:
(1) Method 5 for die measurement of
particulate matter and associated
moisture content
(2) Method 1 for sample and velocity
traverses,
(3) Method 2 for velocity and
volumetric flow rates,
(4) Method 3 for gas analysis, and
(5) Method 9 for the measurement of
the opacity of emissions.
(b) For Method 5, the sampling time
for each run shall be at least 60 minutes
and have a minimum sampled volume of
0.84 dscm (30 dscf). However, shorter
sampling times and smaller sample
volumes, when necessitated by process
variables or other factors, may be
approved by the Administrator.
(c) For each run, the average
phosphate rock feed rate in megagrams
per hour shall be determined using a
device meeting the requirements of
§ 60.403(d).
(d) For each run, emissions expressed
in kilograms per megagram of pKosphate
111-90
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rock feed shall be determined using the
following equation:
M
where. E= Emissions of particulates in kg/Mg
of phosphate rock feed.
Cs = Concentration of particulates in mg/
dscm as measured by Method 5.
Qs — Volumetric flow rate in dscm/hr as
determined by Method 2.
10" •= Conversion factor for milligrams to
kilograms.
M = Average phosphate rock feed rate in mg/
hr.
Note. — The reporting and recordkeeping
requirements in this section are not subject to
Section 3507 of the Paperwork Reduction Act
of 1980, 44 U.S.C. 3507, because these
requirements are expected to apply to fewer
than 10. persons by 1985.
(Sec. 114. Clean Air Act, as amended (42
U.S.C. 7414))
Proposed/effectlve
44 FR 54970, 9/21/79
Promulgated
47 FR T6b82, 4/16/82 (146)
111-91
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119
§ 80.420 Applicability and designation ®J
aWocted facility.
(a) The affected facility to which the
provisions of this subpart apply is each
ammonium sulfate dryer within an
ammonium sulfate manufacturing plant
in the caprolactam by-product,
synthetic, and coke oven by-product
sectors of the ammonium sulfate
industry,
(b) Any facility under paragraph (a) of
this section that commences
construction or modification after
February 4,1980, is subject to the
requirements of this subpart.
§ 50.421 Definitions.
As used in this subpart, all terms not
defined herein shall have the meaning
given them in the Act and in Subpart A.
''Ammonium sulfate dryer" means a
unit or vessel into which ammonium
sulfate is charged for the purpose of
reducing the moisture content of the
product using a heated gas stream. The
unit includes foundations,
superstructure, material charger
systems, exhaust systems, and integral
control systems and instrumentation.
"Ammonium sulfate feed material
streams" means the sulfuric acid feed
stream to the reactor/crystallizer for
synthetic and coke oven by-product
ammonium sulfate manufacturing
plants; and means the total or combined
feed streams (the oximation ammonium
sulfate stream and the rearrangement
reaction ammonium sulfate stream) to
the crystallizer stage, prior to any
recycle streams.
"Ammonium sulfate manufacturing
plant" means any plant which produces
ammonium sulfate.
"Caprolactam by-product ammonium
sulfate manufacturing plant" means any
plant which produces ammonium sulfate
as a by-product from process streams
generated during caprolactam
manufacture.
"Coke oven by-product ammonium
sulfate manufacturing plant" means any
plant which produces ammonium sulfate
by reacting sulfuric acid with ammonia
recovered as a by-product from the
manufacture of coke.
"Synthetic ammonium sulfate
manufacturing plant" means any plant
which produces ammonium sulfate by
direct combination of ammonia and
sulfuric acid.
§ 60.432 Standards for partlculoto mattes'.
On or after the date on which the
performance test required to be
conducted by § 60.8 is completed, no
owner or operator of an ammonium
sulfate dryer subject to the provisions of
this subpart shall cause to be discharged
into the atmosphere*, from any
ammonium sulfate dryer, particulate
matter at an emission rate exceeding
0.15 kilogram of particulate per
me'gagram of ammonium sulfate
produced (0.30 pound of particulate per
ton of ammonium sulfate produced) and
exhaust gases with greater than 15 •
percent opacity.
§ 60.023 Monitoring ol ofsoraMefso.
(a) The owner or operator of any
ammonium sulfate manufacturing plant
subject to the provisions of this subpart
shall install, calibrate, maintain, and
operate flow monitoring devices which
can be used to determine the mass flow
of ammonium sulfate feed material
streams to the process. The flow
monitoring device shall have an
accuracy of ± 5 percent over its range.
However, if the plant uses weigh scales
of the same accuracy to directly
measure production rate of ammonium
sulfate, the use of flow monitoring
devices is not required.
(b) The owner or operator of any
ammonium sulfate manufacturing plant
subject to the provisions of this subpart
shall install, calibrate, maintain, and
operate a monitoring device which
continuously measures and permanently
records the total pressure drop across
the emission control system. The
monitoring device shall have an
accuracy of ± 5 percent over its
operating range.
(Section 114 of the Clean Air Act as amended
(42 U.S.C. 7414))
§ 60.424 Test methods and procedures
(a) Reference methods in Appendix A
of this part, except as provided in
§ 60.8(b), shall be used to determine
compliance with § 60.422 as follows:
(1) Method 5 for the concentration of
particulate matter.
(2) Method 1 for sample and velocity
traverses.
(3) Method 2 for velocity and
volumetric flow rate.
(4) Method 3 for gas analysis.
(b) For Method 5, the sampling time
for each run shall be at least 60 minutes
and the volume shall be at least 1.50 dry
standard cubic meters (53'dry standard
cubic feet).
(c) For each run, the particulate
emission rate, E, shall be computed as
follows:
E=Q«xC.-i-10CO
(1) E is the particulate emission rate
(kg/h).
(2) Qsd is the average volumetric flow
rate (dscm/h) as determined by Method
2; and
(3) C, is the average concentration (g/
dscm) of paniculate matter as
determined by Method 5.
(d) For each run, the rate of
ammonium sulfate production, P (Mg/h),
shall be determined by direct
measurement using product weigh
scales or computed from a material
balance. If production rate is determined
by material balance, the following
equations shall be used.
(1) For synthetic and coke oven by-
product ammonium sulfate plants, the
ammonium sulfate production rate shall
be determined using the following
equation:
P=AxBxCx0.0808
where:
P = Ammonium sulfate production rate in
megagrams per hour.
A = Sulfuric acid flow rate to the reactor/
crystallizer in liters per minute averaged
over the time period taken to conduct the
run.
B = Acid density (a function of acid strength
and temperature) in grams per cubic
centimeter.
C = Percent acid strength in decimal form.
0.0808 = Physical constant for conversion of
time, volume, and mass units.
(2) For caprolactam by-product
ammonium sulfate plants the ammonium
sulfate production rate shall be
determined using the following equation:
H = DxExFx(6.0xiO-5)
where:
P= Production rate of caprolactam by-
product ammonium sulfate in megagrams
per hour.
D = Total combined feed stream flow rate to
the ammonium sulfate crystallizer before
the point where any recycle streams
enter the stream, in liters per minute
averaged over the time period taken to
conduct the test run.
E = Density of the process stream solution in
grams per liter.
F = Percent mass of ammonium sulfate in the
process solution in decimal form.
6.0xlO"5= Physical constant for conversion
of time ai.d mass units.
(e) For each run, the dryer emission
rate shall be computed as follows:
where:
(1) R is the dryer emission rate (kg/Mg):
(2) E is the particulate emission rate (ky/hj
from \c) above; and
(3) P is the rate of ammonium sulfate
production (Mg/h) from (d) above.
(Section 114 of the Clean Air Act as amended
(42 U.S.C. 7414))
Proposed/effective
45 FR 7758, 2/4/80
Promulgated
45 FR 74846, 11/12/80 (119)
111-92
-------
Appendix A—Reference Methods1
.Tim reference methods in this appendli tar referred to
in J60.8 (Performance Tests) and 180.11 (Compliance
With Standards and Maintenance Requirements) of 40
CFR Part 60, Suhpart A (General Provisions). Specific
uses of these reference methods are described In the
standards of performance contained In the SubparU,
beginning with Buhpart D..
Within each standard of performance, a section titled
"Test Methods anil Procedures" Is provided to (1)
identify the lest methods applicable to the facility
subject to the respective standard and (2) Identify toy
special Instructions or conditions to be followed when
applying a method to the respective facility. Such In-
structions (for example, establish sampling rates, vol-
umes, or temperatures) are to be used either In addition
to, or as a substitute for procedures In a reference method.
Similarly, tor sources subject to emission monitoring
requirement*, specific Instructions pertaining to tny us*
•I a reference method are provided In (he aibfwrt or la
Append)] B.
Inclusion of methods In this appendix Is not Intended
M MI endorsement or denial of their applicability to
•duress that we not subject to standards of performance.
The methods m potentially, applicable to other source*;
however, applicability should be confirmed by careful
and appropriate evaluation of the conditions prevalent
»t such sources.
The approach followed in the formulation of the. n-f-
erence methods Involves specifics!inns for equipment.
procedures, and performance. In concept, a performance
specification approach would be preferable in oil methods
because this allows the greatest flexibility to the user.
In practice, however, this approach Is impractical in most
cases because performance specifications cnnnot be
established. Most of the methods described herein,
Iherefore, involve specific equipment si>cciflcations and
procedures, and only a few methods in this appendix rely
on |>ei formancc criteria.
Minor changes in llic reference methods should not
necessarily affect Hie validity of the results and it Is
recounted that, alternative and equivalent methods
exist. Section fiO.H provides authority for the. Administra-
tor to specify or approve (1) equivalent methods, (2)
alternative methods, and (3) minor chances in the
methodology of the reference, methods. It should he
clearly understood that unless otherwise identified all
such methods and changes must have prior approval of
the Administrator. An owner employing such methods or
deviations from the reference methods \vithoulobtaining
prior approval does so nt the risk of subsequent disap*
proval and relesiing with approved methods.
Within the reference methods, certain specific equip-
ment or procedures are recognized as being acceptable
or potentially acceptable and are s|>ei ilically identified
In the methods. Tne items identified as acceptable op-
tions may be used wit.hout approval but m»ist l*e identi-
fied in the test report. Tho potentially approvnlilc op-
tions are cited as "subject to the approval of the
Administrator'' or as "or equivalent." Such potentially
approvable techniques or alternatives may beused at the
discretion of the owner without prior approval, llowevnr,
detailed descriptions for applying these potentially
approvalOe techniques or alternatives are not provided
In the reference methods. Also, the potentially approv-
»ble options are not necessarily acceptable in all applica-
tions. Therefore, an owner electing to use such po-
tentially approvable techniques or alternatives is re-
sponsible for: (1) assuring that the techniques or
alternatives are in tact applicable and are proiierly
executed; (2) Including a written description of the
alternative method in the test report (the written
method must be clear and must be capable of being per-
formed without additional instruction, and the degree
of detail should be similar to the detail contained in the
reference methods); and (3) providing any rationale or
supporting data necessary to show the validity of th«
alternative in the particular application. Failure to
meet these requirements can result In the Adminis-
trator's disapproval of the alternative.
69
MF.TITOD 1-SAMPLE AND VELOCITY TFAVKR.«K« FOR
STATIOXART SOI-RC.F.S 69
50
0.5
DUCT DIAMETERS UPSTREAM FROM FLOW DISTURBANCE (DISTANCE A)
1.0 1.5 2.0
2.5
40
O
0.
Ul
C/)
ec
UJ
20
* 10
I
\
T
A
i
\
J
I-,
|
1
^
'DISTURBANCE
MEASUREMENT
£- SITE
DISTURBANCE
* FROM POINT OF ANY TYPE OF
DISTURBANCE (BEND, EXPANSION, CONTRACTION, ETC.)
3456789
•x
DUCT DIAMETERS DOWNSTREAM FROM FLOW DISTURBANCE (DISTANCE B)
Figure 1-1. Minimum number of traverse points for particulate traverses.
10
Ill-Appendix A-l
-------
1. /Vinrijrf' awl .t/ip/icaWMi/
1.1 Principle. To aid in the representative measure-
ment of pollutant emissions and/or total volumetric flow
rate from a stationary source, a measurement site where
the effluent stream is flowing in a known direction is
sv-lected, and the cross-section of the *tack is divided into
n number of eonal areas. A traverse point is thru located
within each of these equal areas.
1.2 Applicability. This method is applicable to flow-
ing gas streams in ducts, stacks, and flues. The method
cannot be used when: (1) flow is cyclonic or swirling (see
flection 2.4), (2) a stack is smaller than about 0.30 meter
(12 in.) in diameter, or 0.071 m1 (113 in.') in cross-sec-
tional area, or (3) the measurement file is less than two
stack or duct diameters downstream or loss th.in a half
diameter upstream from a flow disturbance.
The requirements of this method must be considered
before construction of a new facility from which emissions
will be measured; failure to do so may require subsequent
alterations to the stack or deviation from the standard
procedure. Cases Involving variants are subject to ap-
proval by the ' Administrator. U.P. Environmental
Protection Agency.
2. Prottdvrt
2.! Selection of Measurement Site. Sampling or
velocity measurement is performed at a File located at
least eight stack or duct diameters downstream and two
diameters upstream from any flow disturbance such as
a bond, expansion, or contraction in the stack, or from a
visible flame. If necessary, an alternative location may
be selected, at a position at least two stack or duct di-
ameters downstream and a half diameter upstream from
any flow disturbance. For a rectangular cross section,
an equivalent diameter (7>.) shall be calculated from the
following equation, to determine the upstream and
downstream distances:
„ 2iir
where £=length and JK=width.
2.2 Determining the Number of Traverse Points.
2.2.1 Paniculate Traverses. When the eight- and
two-diameter criterion can be met, the minimum number
of traverse points shall be: (1) twelve, for circular or
rectangular stacks with diameters (or equivalent di-
ameters) greater than 0.61 meter (24 in.); (2) eight, for
circular stacks with diameters between 0.30 and 0.61
meter (12-24 in.); (3) nine, for rectangular stacks with
equivalent diameters between 0.30 and 0.61 meter (12-24
in.).
When the eight- and two-diameter criterion cannot be
met, the minimum number of traverse points is deter-
mined from Figure 1-1. Before referring to the figure,
however, determine the distances from the chosen meas-
urement site to the nearest upstream and downstream
disturbances, and divide each distance by the stack
diameter or equivalent diameter, to determine the
distance in terms of the number of duct diameters. Then,
determine from Figure 1-1 the minimum number of
traverse points that corresponds: (1) to the number of
duct diameters upstream; and (2) to the number of
diameters downstream. Select the higher of the two
minimum numbers of traverse points, or a greater value,
so that for circular stacks the number is a multiple of 4,
and for rectangular stacks, the number is one bf those
shown in Table 1-1.
TAT-.T.E 1-1. Croti-scctional layout for rcttangirtar alaeti
dumber of
Ma-
trix
tracerst ixiii
..87
'L+W
12..
16..
20-..
25..
30..
38..
42..
49..
out
3x3
4x3
4x4
5x4
5x5
6x5
6x«
7x6
7x7
2.2.2 Velocity (Non-Particulate) Traverses. When
velocity or volumetric flow rate is to be determined (but
not particulat* matter), the same procedure as that for
paniculate traverses (Section 2.2.1) is followed, except
that Figure 1-2 may be used instead of Figure 1-1.
2.3 Cross-Sectional Layout and Location of Traverse
Points.
2.3.1 Circular Stacks. Locate the traverse points on
two perpendicular diamctersaccording to Table 1-2 and
the example shown in Figure 1-3. Any equation (for
examples, see Citations 2 and 3 In the Bibliography) that
gives the same values.as those in Table 1-2 may be used
In lieu of Table 1-2.^™
For participate traverses, one of the diameters must be
in a plane containing the greatest expected concentration
variation, e.g., after bends, one diameter shall be in the
plane of the bend. This requirement becomes less critical
as the distance from the disturbance increases; therefore,
•ther diameter locations may be used, subject to approval
of the Administrator.
In addition, for stacks having diameters greater than
0.61 m (24 in.) no traverse points shall be located within
2.5 centimeters (1.00 in.) of the stack walls; and for stack
diameters equal to or less than 0.61 m (24 in.), no traverse
points shall be located within 1.3 cm (0.50 in.) of the stack
walls. To meet these criteria, observe the procedures
given below.
2.3.1.1 Stacks With Diameters Greater Than 0.61 m
(24 in.). When any of the traverse points as located in
Section 2.3.1 fallwithin2.5cm (1.00 in.) of the stack walls,
relocate them away from the stack walls to: (1) a distance
of 2.5 cm (i.oo in.); or (2) a distance equal to the nozzle
Inside diameter, whichever Is larger. These relocated
traverse points (on each end of a diameter) shall be the
"adjusted" traverse points.
Whenever two successive traverse points are combined
to form a single adjusted traverse point, treat the ad-
justed poiM as two separate traverse points, both in the
sampling (or velocity measurement) procedure, and in
recording the data.
DUCT DIAMETERS UPSTREAM FROM FLOW DISTURBANCE (DISTANCE A)
0.5 1.0 1.5 2.0
2.5
50
40
O
a.
LU
u.
O
30
20
* 10
5
I
I
I
T
A
B
1
MEASUREMENT
h >- SITE
DISTURBANCE
DISTURBANCE
I
I
34 5 6 7 8 9
DUCT DIAMETERS DOWNSTREAM FROM FLOW DISTURBANCE (DISTANCE B)
10
Figure 1-2. Minimum number of traverse points for velocity (nonparticulate) traverses.
^II-Appendix A-2
-------
TRAVERSE
POINT
1
2
3
4
5
6
Figure 1-3. Example showing circular stack cross section divided into
12 equal areas, with location of traverse points indicated.
Table 1-2. LOCATION OF TRAVERSE POINTS IN CIRCULAR STACKS
(Percent of stack diameter from Inside wall to traverse point)
Traverse
point
number
on a .
diameter
1
2
3
«!
5'
6
7
8
9
10
11
«l
13
14
15
16
17
18
19
20!
21
22
23
24
Number of traverse points on a diameter
2
14.6
85.4
4
6.7
25.0
75.0
93.3
6
4.4
14.6
29.6
70.4
85.4
95.6
8
3.2
10.5
19.4
32.3
67.7
80.6
89.5
96.8
10
2.6
8.2
14.6
22.6
34.2
65.8
77.4
85.4
91.8
97.4
12
2.1
6.7
11.8
17.7
25.0
35 ..6
64.4
75.0
82.3
88.2
93.3
97.9
14
1.8
5.7
9.9
14.6
20.1
26.9
36.6.
63.4
73.1
79.9
85.4
90.1
94.3
98.2
16
1.6
4.9
8.5
12.5
16.9
22.0
28.3.
37.5
62.5
71.7
78.0
83.1
87.5
91.5
95'. 1
98.4
18
1.4
4.4
7.5
10.9
14.6
18.8
23.6
29.6
38.2
61.8
70.4
76.4
31.2
85.4
89.1
92.5
95.6
98.6
20
1.3
3.9
•6.7
.9.7
12.9
16.5
20.4
25.0
30.6
38.8
61.2
69.4
75.0
79.6
83.5
87.1
90.3
93.3
96.1
98.7
22
1.1
3.5
6.0
8.7
11.6
14.6
18.0
21.8
26.2
31.5
39.3
60.7
68.5
73.8
78.2
82.0
85.4
88.4
91.3
94.0
96.5
98.9
24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
.39.8
60.2
67.7
72.8
77.0
80.6
83,. 9
86.8
89.5
92.1
94.5
96.8
98.9
"minimum number of points" matrix were
expanded to 36 points, the final matrix
could be 9x4 or 12x3. and would not neces-
sarily have to be 6x6. After constructing the
final matrix, divide the stack cross-section
into as many equal rectangular, elemental
areas as traverse points, and locate a tra-
verse point at the centroid of each equal
area.8'
The situation of traverse points being too close to the
stack walls is not expected to arise with rectangular
stacks. If this problem should eTer arise, the Adminis-
trator must be contacted for resolution of the matter.
2.4 Verification of Absence of Cyclonic Plow. In most
stationary sources, the direction of stack ga» flow Is
essentially parallel, to the stack walls. However,
cyclonic flow mar exist (1) after such devices as cyclones
and Inertial demisters following rental scrubbers, or
0) in (tacks baring Ui^enUal Inlets or other duct eon-
flxantlou which tend to Induce swirling; In these
Instances, the presence or absence of cyclonic flow at
the sampling location must be determined. Tbe following
techniques are acceptable for this determination.
I
Figure 1-4. Example showing rectangular stack cross
section divided into 12 equal areas, with a traverse
point at centroid of each area.
Level and zero the manometer. Connect a Type 8
pilot tube to the manometer. Position the Type 8 pilot
tube at each traverse point, in succession, so that the
planes of the face openings of the pilot tube are perpendic-
ular to the stack cross-sectional plane: when the Type 8
pilot tube is in this position, it is at "0° reference." Note
the differential pressure (Ap) reading at each traverse
point. U a null (zero) pilot reading is obtained at
-------
METHOD 2—DETERMINATION OF STACK OAS VELOCITY
AND VOLUMBTBIC FLOW RATE (TYPE S PITOT TUBE) °v
1. Principle and Applicability
1.1 Principle. The average gas velocity in a stack is
determined from the gas density and from measurement
of the average velocity head with a Type S (Stausscheibe
or reverse type) pitot tube.
1.2 Applicability. This method is applicable for
measurement of the average velocity of a gas stream and
for quantifying gas flow.
This procedure is not applicable at measurement sites
which fail to meet the criteria of Method 1, Section 2.1.
Also, the method cannot be used for direct measurement
in cyclonic or swirling gas streams; Section 2.4 of Method
1 shows how to determine cyclonic or swirling flow con-
ditions. When unacceptable conditions exist, alternative
procedures, subject to the approval of the Administrator,
U.S. Environmental Protection Agency, must be em-
ployed to make accurate Bow rate determinations:
examples of such alternative procedures are: (1) to install
straightening vanes; (2) to calculate the total volumetric
flow rate stoichiometrically, or (3) to move to another
measurement site at which the flow is acceptable.
2. Apparatus
Specifications for the apparatus are given below. Any
other apparatus that has been demonstrated (subject to
approval of the Administrator) to be capable of meeting
the specifications will be considered acceptable.
2.1 Type S Pitot Tube. The Type B pitot tab*
(Figure 2-1) shall be made of metal tubing (e.g., stain-
less steel). It is recommended that the external tubing
diameter (dimension D,, Figure 2-2b) be between 0.48
and 0.96 centimeters (M« and M inch). There shall be
-an equal distance from the base ol each leg of the pitot
lube to its face-opening plane (dimensions PA and Pt,
Figure 2-2b); it is recommended that this distance b»
between 1.06 and 1.60 times tbe external tubing diameter.
The face openings of the pitot tube shall, preferably, b*
aligned as shown In Figure 2-2; however, alight misalign-
ments of the openings are permissible (see Figure 2-3).
Tbe Type 8 pitot tube shall have a known coefficient,
determined as outlined in Section 4. An identification
number shall be assigned to the pitot tube; this number
nail be permanently marked or engraved on the body
1.9 0-2.54 cm*
(0.75 -1.0 in.)
L_Q.
tm""- j*:'v-^-"--" "^
I 7.62 cm (3 in.)*
TEMPERATURE SENSOR
LEAK-FREE
CONNECTIONS
MANOMETER
SUGGESTED (INTERFERENCE FREE)
PITOT TUBE • THERMOCOUPLE SPACING
Figure 2-1. Type S pitot tube manometer assembly.
Ill-Appendix A-4
-------
TRANSVERSE
TUBE AXIS
\
FACE
•OPENING
PLANES
(a)
A SIDE PLANE
J
LONGITUDINAL 7 Dt
TUBE AXIS *~ \ .*
. ,!.-
s "7
*
-------
TRANSVERSE
TUBE AXIS
LONGITUDINAL
TUBE AXIS—
Figure 2-3. Types of face-opening misalignment that can result from field use or Im-
proper construction of Type S pi tot tubes. These will not affect the baseline value
of E?p(s) so long as ai and a2 < 10°, 01 and 02 < 5°. z < 0.32 cm (1/8 In.) and w <
0.08 cm (1/32 in.) (citation 11 in Section 6).
Ill-Appendix A-6
-------
A standard pilot tube may be nsed Instead of a Type 9,
provided that it meets the spocificationj of Sections 2.7
and 4.2; note, however, that the static and Impact
pressure holes of standard pilot tubes are susceptible to
plugging in particuloto-lftden gas streams. Therefore,
whenever a standard pilot tube is used lo perform a
traverse adequate proof must be furnished that the
openings of the pilot tube have not plugged up during the
traverse period: this ran be done by talcing a velocity
head (Ap) rending at the dual traverse point, eleanmg out
I lie impact and slatic holes of the standard pitol lube by
"back-pursing" with pressurized air. and then taking
another i;> reading. If the Ap readings made before and
after the air puree urethe same (±5 percent!. the traverse
is acceptable Otherwise, reject t!ie run. Note that if Ap
at the final traverse point is unsuitably low, another
point may be selected. If "back-purging" at regular
intervals is part of the procedure, then comparative Ap
readings shall be taken, as above, for the last two back™
purges at which suitably high Ap readings are observed.0'
•> -2 Differential Pressure dauge. An inclined manom-
eter or equivalent device is used. Most sampling trains
are equipped with a 10-in. (water column) inclined-
vertical manometer, having 0.01-in. H,O divisions on the
0- to 1-in. inclined scale, and 0.1-in. HjO divisions on the
1- to in-in. vertical scale. This type of manometer (or
other gauge of equivalent sensitivity) is satisfactory for
the measurement of Ap values as low as 1.3 mm (0.05 in.)
HjO. However, a differential pressure gauge of greater
sensitivity shall be used (subject to the approval of the
Administrator), if any of the following is fonnd to be
true: (1) the arithmetic average of all Ap readings at the
traverse points in the stack is less than 1.3 mm (0.08 In.)
H-0- (2) for traverses of 12 or more points, more than 10
percent of the individual Ap readings are below L3 mm
(0.05 in.) H.O; (3) for traverses of fewer than 12 points,
more than one Ap reading is below 1.3 mm (0.06m.) H:O.
Citalion 18 in Section 6 describes commercially available
instrumenlalion for the measurement of tow-range gas
V
-------
PLANT.
DATE.
RUN NO.
STACK DIAMETER OR DIMENSIONS, m(in.)
BAROMETRIC PRESSURE, mm Hg (in. Hg)
CROSS SECTIONAL AREA. m2(ft2)
OPERATORS
PIT.OTTUBEI.D.NO.
AVG. COEFFICIENT, Cp = .
LAST DATE CALIBRATED.
SCHEMATIC OF STACK
CROSS SECTION
Traverse
Pt.No.
Vel.Hd.,Ap
mm (in.)
Stack Temperature
T$,°K(°R)
mm Hg (in.Hg)
Avenge
Figure 2-5. Velocity traverse data.
III-Appendix A-8
-------
3.6 Determine the stack gas dry molecular weight.
Vor combustion processes or processes that emit essen-
tially CO), Oi, CO, nnd.Ni, use Method 3. For processes
.•milting essentially air, an analysis need not be con-
ducted; use a dry molecular weight of 29.0. For other
processes, other methods, subject to the approval of the
Administrator, must be used.
.1.7 Obtain the moisture content from Reference
Method 4 (or equivalent) or from Method 5.
3.8 Determine the cross-sectional area of the stack
or duct at the sampling location. Whenever possible,
physically measure the stack dimensions rather than
using blueprints.
4. Calibration
4.1 Type S Pilot Tube. Before its initial use, care-
tiilly examine the Type S pilot tube in top, side, and
end views to verify that the face openings of the tube
are aligned within the specifications illustrated in Figure
•2-2 or 2-3. The pilot tube shall not be used if it fails to
meet these alignment specifications.
After verifying the face opening alignment, measure
and record the following dimensions of the pitoj tube:
(a) the external tubing diameter (dimension Di, Figure
2-2b); and (b) the base-to-opening plane distances
(dimensions Pt and Pa, Figure 2-2b). If D\ Is between
0.48 and 0.05 cm (M« and H in.) and If PA and Pa are
equal and between 1.05 and 1.50D,, there are two possible
options: (1) the pilot tube may be calibrated according
to the procedure outlined in Sections 4.1.2 through
4.1.5 below, or (2) a baseline (isolated tube) coefficient
value of 0.84 may bo assigned to the pilot tube. Note,
however, that if the pilot tube is part of an assembly,
calibration may slill be required, despile knowledge
of the baseline coefficient value (see Section 4.1.1).a/
If Dt, PA, and PB are outside the specified limits, the
pitot lube must be calibrated as outlined in 4.1.2 through
4.1.5 below.
4.1.1 Type S Pilot Tube Assemblies. During sample
and vclocily traverses, Ibe isolated Type S pitol tube is
not always used; in many instances, the pitot tube is
used in combination with other source-sampling compon-
ents (thermocouple, sampling probe, nozzle) as part of
an "assembly." The presence of other sampling compo-
nents can sometimes affect the baseline value of Ihe Type
8 pitot tube coefficient (Citalion 9 in Section 6); Iherefore
an assigned (or otherwise known) baseline coefficient
value may or may not lie valid for a given assombly. The
baseline and assembly coellicicnt values will be identical
only when the relative placement of the components in
the assembly is such that aerodynamic interference
effects are eliminated. Figures 2-« through 2-8 illustrate
interference-tree component arrangements for Type 8
pitol tubes having external tubing diameters between
0.48 and 0.05 cm (Ma and H in.). Type S pitot tube assem-
blies that fail to meet any or all of the specifications of
Figures 2-6 through 2-8 shall be calibrated according lo
the procedure outlined in Sections 4.1.2 through 4.1.5
below, and prior to calibration, the values of the inter-
component spacings (pitol-nozzle, pilol-lhermocouple,
pilot-proho sheath) shall be measured and recorded.
NOTE.—Do not use any Type S pilot tube assembly
which is constructed such that Ihe impact pressure open-
ing plane of the pitot tube is below the entry plane of Ibe
nozile (see Figure 2-6b).
4.1.2 Calibration Selup. If Ihe Type S pitot tube is to
be calibrated, one leg of the tube shall be permanently
marked A, and the other, B. Calibration shall be done in
a flow system having the following essential design
fealures: 87
TYPES PITOT TUBE
x > 1.90 em (3/4 ia) FOR On -1.3 cm (1/2 in.)
SAMPLING NOZZLE
A. BOTTOM VIEW; SHOWING MINIMUM PITOT NOZZLE SEPARATION.
SAMPLING
PROBE
\
SAMPLING
NOZZLE
STATIC PRESSURE
OPENING PLANE
IMPACT PRESSURE
OPENING PLANE
SIDE VIEW: TO PREVENT PITOT TUBE
FROM INTERFERING WITH GAS FLOW
STREAMLINES APPROACHING THE
NOZZLE. THE IMPACT PRESSURE
OPENING PLANE OF THE PITOT TUBE
SHALL BE EVEN WITH OR ABOVE THE
NOZZLE ENTRY PLANE.
* Figure 2-6. Proper pitot tube • sampling nozzle configuration to present
aerodynamic interference; buttonhook • type nozzle; centers of nozzle
and pitot opening aligned; Df between 0.48 and 0.95 cm (3/16 and
3/8 in.).
Ill-Appendix A-9
-------
-rrr
c
THERMOCOUPLE
Ot
TYPE S PITOT TUBE
SAMPLE PROBE
I
THERMOCOUPLE
z>s.o«em ;
TYPE S PITOT TUBE
, SAMPLE PROBE
Figure 2-7. Proper thermocouple placement to prevent interference;
Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
TYPES PITOT TUBE
SAMPLE PROBE
Y>7.62cm(3inJ
Figure 2-8. Minimum pitot-sample probe separation needed to prevent interference;
Dt between XX48 and 0.95 cm (3/16 and 3/8 in.).
4.1.2.1 The Bowing gas stream must be confined to a
duct of definite cross-sectional area, either circular or
rectangular. For circular cross-sections, the minimum
duct diameter shall be 30.5 cm (12 in.); -for rectangular
cross-sections, the width (shorter side) shall be at least
25.4cm (10 in.).
4.1.2.2 The cross-sectiona1 area of the calibration -duct
must be constant over a distance of 10 or more duct
diameters. For a rectangular cross-section, use an equiva-
lent diameter, calculated from the following equation,
to determine tbe number of duct diameters:
2LW
Equation 2-1
where:
D. = Equivalent diameter
L—Length
W=Width
To ensure the presence of stable, fully developed flow
patterns at the calibration site, or "lest section," the
site must be located at least eight diameters downstream
and two diameters upstream from the nearest disturb-
ances.
NOTE.—The eight- and two-diameter criteria are not
absolute; other test section locations may be used (sub-
ject to approval of the Administrator), provided that the
flow at the test site is stable and demonslrably parallel
to the duct axis.
4.1.2.3 The flow system shall have the capacity to
generate a test-section velocity around 915 m/min (3,000
ft/min). This velocity must be constant with time to
guarantee steady flow during calibration. Note that
Type 8 pitot tube coefficients obtained by single-velocity
calibration at 915 m/min (3,000 ft/min) will generally be
valid to within ±3 percent for the measurement of
velocities above 305 m/min (1,000 ft/min) and to within
±5 to 6 percent for the measurement of velocities be-
tween 180 and 305 m/min (600 and 1,000 ft/min). If a
more precise correlation between C, and velocity is
desired, tbe flow system shall have the capacity to
generate at least four distinct, time-invariant test-section
velocities covering the velocity range from 180 to 1,525
m/min (600 to 5,000 ft/min), and calibration data shall
he taken at regular velocity intervals over this range
(see Citations 9 and 14 in Section 6 for details).
4.1.2.4 Two entry ports, one each for the standard
and Type 8 pitot tubes, shall be cut in the test section;
the standard pitot entry port shall be located slightly
downstream of the Type 8 port, so that the standard
and Type S impact openings will lie in the same cross-
sectional plane during calibration. To facilitate align-
ment of the pitot tubes during calibration, it is advisable
that the test section be constructed of pleiiglas or some
other transparent material.
4.1.3 Calibration Procedure. Note that this procedure
is a general one and must not be used without first
referring to the special considerations presented in Sec-
tion 4.1.5. NoU also that this procedure applies Only to
single-velocity calibration. To obtain calibration data
for the A and B sides of the Type S pitot lube, proceed
as follows:
4.1.3.1 Make sure that the manometer is properly
filled and that the oil is free from contamination and is of
the proper density. Inspect and leak-check all pitot lines;
repair or replace if necessary.
4.1.3.2 Level and tero the manometer. Turn on the
fan and allow the flow to stabilize. Seal the Type S entry
port;
4.1.3.3 Ensure that the manometer Is level and zeroed.
Position the standard pitot tube at the calibration point
(determined as out lined in Sction 4.1.5.1), and align the
tube so that its tip Is pointed directly into the flow. Par-
ticular care should be teken in aligning the tube to avoid
yaw and pitch angles. Make sure that the entry port
surrounding the tube is properly sealed.
4.1.3.4 Read Ap.,d and record its value in a data table
similar to the one shown in Figure 2-9. Remove the
standard pitot tube from the duct and disconnect it from
the manometer. Seal the standard entry port.
4.1.3.5 Connect the Type S pitot tube to the manom-
eter. Open the Type S entry port. Check the manom-
eter level and zero. Insert and align the Type S pitot tube
so that its A side impact opening is at the same point as
was the standard pitot tube and is pointed directly into
tlie llpw. Make sure that the entry port surrounding the
tube is properly sealed.
4.1.3.6 Read Ap. and enter its value in the data table.
Remove the Type S pitot tube from the duct and dis-
connect it from the manometer.
4.1.3.7 Repeal steps 4.1.3.3 through 4.1.3.6 above until
three pairs of Ap readings have been obtained.
4.1.3.8 Repeat steps 4.1.3.3 through 4.1.3.7 above for
the B side of the Type S pitot tube.
4.1.3.9 Perform calculations, as described in Section
4.1.4 below.
4.1.4 Calculations.
4.1.4.1 For each of the six pairs of Ap readings (i.e.,
three from side A and three from side B) obtained in
Section 4.1.3 above, calculate the value of the Type 8
pitot tube coefUcieui as follows:
Ill-Appendix A-10
-------
PITOTTUBE IDENTIFICATION NUMBER:
CALIBRATED BY.'.
.DATE:.
RUN NO.
1
2
3
"A" SIDE CALIBRATION
' Ap,td
cm HaO '
(in. H20)
APM
cm H20
(in. H20)
Cp (SIDE A)
Cp($)
DEVIATION
Cp(s)-Cp(A)
RUN NO,
1
1
3
"B" SIDE CALIBRATION
Ap$td
cm HzO
(in. HzO)
•
APM
cm HzO
(in. H20)
Cp (SIDE B)
CpW
DEVIATION
Cp(,).Cp(B)
AVERAGE DEVIATION - o(AORB)
S|Cp(s)-Cp(AORB)|
-MUSTBE<0.01
| Cp (SIDE A)-Cp (SIDE B) j-«-MUST BE <0.01
Figure 2-9. Pitot tube calibration data.
4.1.4.3 Calculate the deviation of each o( the three A-
side values of C, a > from C, (sideA), and the deviation ol
each B-side value of C,t.} from C, (side B). Use the fol-
lowing equation:
Deviation = Cpf.i-C7,(A or B)
Kquatiun 2-3
4.1.4.4 Calculate a, the average deviation from the
mean, for both the A and B sides of the pilot tube. Use
the following equation:
Equation 2-2
^'-ssscwrsaS-wi.». zs^^^^ttrzz
according to the criteria of Sections 2.7.1 to
2.7.8 of this method.
Ap.,d=Velocity bead measured by the standard pltot
tube, cm H>O (In. H,O)
Ap.=Velocity bead measured by the Type 8 pltot
tube, cm HiO (to. HjO)
4.1.4J Calculate C, Gride A), the mean A-dde coef-
a (side A ur B)=-
coefflclent is unknown and the tube la designed value*.
Equation 2-4
4.1.4.5 Use the Type S pilot tube only if the values of
o (side A) and a (side B) are less than or equal to 0.01
and if the absolute value of the difference between Cp
(A) andCV (B) is 0.01 or less.
4.1.5 Special considerations.'
4.1.5.1 Selection of calibration point.
4.1.5.1.1 When an isolated Type S pitot tube is cali-
brated, select a calibration point at or near the center of
the duct, and follow the procedures outlined in Sections
4.1.3 and 4.1.4 above. The Type S pitot coefficients so
obtained, i.e., C, (side A) and C, (side B), will be valid,
so long as either: (1) the isolated pitot tube is used; or
(2) the pitot tube is used with other components (nozzle,
thermocouple, sample probe) in an arrangement that is
free from aerodynamic interference effects (see Figures
2-6 through 2-8).
4.1.5.1.2 For Type S pitot tube-thermocouple com-
binations (without sample probe), select a calibration
point at or near the center of the duct, and follow the
procedures outlined in Sections 4.1.3 and 4.1.4 above;
The coefficients so obtained will be valid so long as the
pitot tube-thermocouple combination is used by itself
or with other components in an interference-free arrange-
ment (Figures 2-6 and 2-8).
4.1.5.1.3 For assemblies with sample probes, the
calibration point should be located at or near the center
of the duct; however, insertion of a probe sheath into a
small duct may cause significant cross-sectional area
blockage and yield incorrect coefficient values (Citation 9
in Section 6). Therefore, to minimize the blockage effect,
the calibration point may be a few inches off-center if
necessary. The actual blockage effect will be negligible
when the theoretical blockage, as determined by a
projected-area model of the probe sheath, is 2 percent or
less of the duct cross-sectional area for assemblies withont
external sheaths (Figure 2-10a), and 3 percent or less for
assemblies with external sheaths (Figure 2-10b).
4.1.5.2 For those probe assemblies in which pitot
tnbe-nozzle interference is a factor (i.e., those in which
the pitot-nozzle separation distance fails to meet the
specification illustrated in Figure 2-6a), the value of
CM*) depends upon the amount of free-space between
the tube and nozzle, and therefore is a function of nozzle
size. In these instances, separate calibrations shall be
performed with each of the commonly used nozzle sizes
in place. Note that the single-velocity calibration tech-
nique is acceptable for this purpose, even though the
larger nozzKsizes (>0.635 cm or !i in.) are not ordinarily
used for isoUnetic sampling at velocities around 915
m/roin (3,000 ft/min), which is the calibration velocity;
note also that it is not necessary to draw an isokineud
sample during calibration (see Citation 19 in Section 6).o/
4.1.5.3 For a probe assembly constructed such that
HJ pitot tube is always used in the same orientation, only
one side of the pitot tube need be calibrated (the side
which will face the flow). The pitot tube must still meet
t be alignment specifications of Figure 2-2 or 2-3, however,
and must have an average deviation (») value of 0.01 or
less (see Section 4.1.4.4).
III-Appendix A-11
-------
ESTIMATED
SHEATH
BLOCKAGE
*m
Figure 2-10. Projected-area m.odels for typical pilot tube assemblies.
4.1.6 Field Use and Recalibration.
4.1.6.1 Field Use.
4.1.6.1.1 When a Type 8 pilot tube (Isolated tube or
assembly) is used in the field, the appropriate coefficient
value (whether assigned or obtained by calibration) shall
be used to perform velocity calculations. For calibrated
Type B pilot tubes, the A side coefficient shall be used
when the A side of the tube faces the Sow, and the B side
coefficient shall be used when the B side faces the flow;
alternatively, the arithmetic average of the A and B side
coefficient values may be used, irrespective of which side
faces the flow.
4.1.6.1.2 When a probe assembly is used to sample a
email duct (12 to 36 in. in diameter), the probe sheath
sometimes blocks a significant part of the duct cross-
section, causing a reduction in the effective value of
7,CD. Consult Citation 9 in Section 6 for details. Con-
ventional pilot-sampling probe assemblies are not
recommended for use in ducts having inside diameters
smaller than 12 Inches (Citation 16 in Section 6).
4.1.6.2 Recalibration.
4.1.6.2.1 Isolated Pilot Tubes. After each field use, the
pitol tube shall be carefullyTeexamined in top, side, and
end views. If the pilot face openings are still aligned
within the specifications illustrated in Figure 2-2 or 2-3,
It can be assumed that the baseline coefficient of the pilot
tube has not changed. If, however, the tube has been
damaged U> the extent that it no longer meets the specifi-
cations of Figure 2-2 or 2-3, the damage shall either be
repaired to restore proper alignment of the face openings
or the tube shall be discarded.
4.1.6.2.2 Pitol Tube Assemblies. After each field use,
check the face opening alignment of the pilot tube, as
In Section 4.1.6.2.1; also, remeasure the intercomponent
•pacings of the assembly. If the intercomponent spaclngs
nave not changed and the face opening alignment u
acceptable, it can be assumed that the coemclenl of the
assembly has not changed. If the face opening alignment
Is no longer within the specifications of Figures 2-2 or
2-3, either repair the damage or replace the pilot tube
(calibrating the new assembly. If necessary). If the Inter-
component Bpaclngs have changed, restore the original
(pacings or recalibrate the assembly.
4.2 Standard pilot tube (if applicable). If a standard
pilot tube Is used for the velocity traverse the tube shall
be constructed according to the criteria of Section 2.7 and
shall be assigned a baseline coefficient value of 0.99. If
th« standard pilot tube is used as part of an assembly.
the tube shall be In an InUrfennoe-tree arrangement
(subject to the approval of the Administrator).
4£ Temperature Gauges. After each field use, cali-
brate dial thermometers, liquid-filled bulb thermom-
eters, thermocouple-potenliometer systems, and other
gauges at a temperature within 10 percent of the average
absolute stack temperature. For temperatures up to
406" C (761° F), use an ASTM mercury-m-glass reference
thermometer, or equivalent, as a reference; alternatively,
either a reference thermocouple and polenliometar
(calibrated by NBS) or thermometric flied points, e.g.,
loe bath and boiling water (corrected for barometric
pressure) may be used. For temperatures above 405° C
(761° F), use an NBS-calibraled reference thermocouple-
potentiometer system or an alternate reference, subject
to the approval of the Administrator.
If, during calibration, the absolute temperatures meas-
ured with the gauge being calibrated and the reference
gauge agree within 1.6 percent, the temperature data
taken In the field shall be considered valid. Otherwise.
the pollutant emission test shall either be considered
invalid or adjuslmenls (if appropriate) of the lest results
shall be made, subject to the approval of the Administra-
tor.
4.4 Barometer! Calibrate the barometer used against
a mercury barometer.
III-Appendix A-12
-------
6. Calculation*
Carry out calculations, retaining at least one extra
decimal figure beyond that of the acquired data. Round
.03 figures after final calculation.
C.I Nomenclature.
X= Cross-sectional area of stack, m> (ft>).
Bo-Water vapor in the gas stream (from Method 5 or
Reference Method 4), proportion by volume.
CV-Pitot tube coefficient, dimensionless.
A',=Pitot tube constant,
oj Q7 J5_ r(g/g-mole)(mm
* "'secL (°K)(mmH,
0)
tat the metric system and
„ . _
"eec
(°R)(in.H,O)
for the English system.
Aftf-Molecular weight of stack gas, dry basis (see
flection 3.6) g/g-mole (Ib/lb-mole).
J£i—Molecular weight of stack gas, wet basis, g/g-
mole (Ib/lb-mole).
—A/d (1 —Bn)+18.0 Bw, Equation 2-5
Pb.r=Barometric pressure at measurement site, """
Hg (in. Hg).
P, —Stack static pressure, mm Hg (in. Hg).
P.=Absolute stack gas pressure, mm Hg (in. Hg).
. —Pbor+Pi Equation 2-«
Pud-Standard absolute pressure, 760 mm Hg (29.92
In. Hg).
Qid—Dry volumetric stack gas flow rate corrected to
standard conditions, dscm/hr (dscf/hr).
(.—Stack temperature, "C (°F).
T.-Absolute stack temperature, °Z (°R).
—273+*. for metric
*>460+'i for English
Equation 2-7
Equation 2-8
r«d=8tandard absolute temperature, 293°K (528° R)
o.-Average stack gas velocity, m/sec (ft/sec).
Ap- Velocity head of stack gas. mm HiO (in. HjO).
3,600— Conversion factor, sec/hr.
18.0— Molecular weight of water, g/g-mole flb-lb-
mole).
5.2 Average stack gas velocity.
P.M,
Equation 2-9
5.3 Average stack gas dry volumetric flow rate,
Equation 2-10
6. Bibliography
1. Mark, L. 8. Mechanical Engineers' Handbook. New
York. McGraw-Hill Book Co.TlM. 1951.
2. Perry, J. H. Chemical Engineers' Handbook. New
York. McGraw-Hill Book Co.. Inc. 1960.
3. Shiid-linra, R. T., W. F. Todil. ami W. 8. Smith.
Significance of Krrors in Slack .Sampling Measurements.
LT.S. Knvironmental Protection Agency, Research
Triangle Park, N.C. (Presented at the Annual Mooting of
llio Air 1'ollutiun Control Association, St. Louis, Mo.,
June 14-1!), 1970.)
4. Standard Method for Sampling Slacks (or Paniculate
Mall.T. In: 11171 Book of ASTM Standards, 1'art 23.
Philadelphia, Pa. 1971. ASTM Designation I)-isr.»-71.
.). \'«'iniafcl, J. K. Elementary FluiT2. p. 208.
8. Annual Hook of ASTM Standards, I'uri Jtj. 1U74. p.
frIM.
'.I. Yullaro, R. F. (iuidclincs for Type S I'ilot Tulw
Calibration. U.S. Environmental I'roiiviion Agency.
He.<«'arch Triangle Park, N.(.\ (Hrcsi'iiied at 1st Annual
Meeting, Sourec Evaluation Society, Dayton, Ohio,
September 18, 1975.)87
10. Vollaro, R. F. A Type S 1'itot Tube Calibration
Study. U.S. Environmental Protection Agency, Emis-
sion Measurement Branch, Research Triangle Park,
N.C. July 1974.
11. Vollaro, R. F. The Effects of Impact Opening
Misalignment on the Value of the Typo S Pit.ot Tube
Coefficient. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle
Park, N.C. October 1076.
12. Vollaro, R. F. Establishment of a Baseline. Coeffi-
cient Value for Properly Constructed Typo S Pilot
Tubes. U.S. Environmental Protection Auency, Emis-
sion Measurement Branch, Research Triangle Park,
N.O. November 1976.
13. Vollaro, R. F. An Evaluation of Single-Velocity
Calibration Technique as a Means of Determining Type
S Pilot Tube Coefficients. U.S. Enviroruncnlal Protec-
tion Agency, Emission Measuremeiu Dranch, Research
Triangle Park, N.C. August l'J75.8/
14. Vollaro, R. F. The Use of Type S Pilot Tubes for
the Measurement of Low Velocilies. U.S. Environmental
Protection Agency, Emission Measurement Branch,
Research Triangle Park, N.C. November 1976.
15. Smith, Marvin L. Velocity Calibration of EPA
Type Source Sampling Probe. United Technologies
Corporation, Pratt and Whitney Aircraft Division,
Kast Hartford, Conn. 1975.
16. Vollaro, R. F. Recommended Procedure for Sample
Traverses in Ducts Smaller than 12 Inches in Diameter.
U.S. Environmental Proteclion Agency, Emission
Measurement Branch, Research Triangle Park, N.C.
November l'J76.
17. Ower, E. and R. C. Pankhurst. The Measurement
of Air Flow, 4th Ed., London, Pergainon Press. 1966.
18. V'ollaro, R. F. ASurvey of Commercially Available
Instrumentation for the Measurement of Low-Range
(ias Velocities. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle
Park, N.C. November 1976. (Unpublished Paper)87
19. Gnyp, A. W., C. C. St. Pierre, D. 8. Smith, D.
Mozzon, and J. Steiner. An Experimental Investigation
of the Effect of Pitot Tube-Sampling Probe Configura-
tions on the Magnitude of the S Type Pilot Tube Co-
elHciont for Commercially Available Source Sampling
Probes. Prepared by the University of Windsor for the
Ministry of the Environment, Toronto, Canada. Feb-
ruary 1975.
III-Appendix A-13
-------
METHOD 3—(!.\s ANALYSIS FOR CARBON DIOXIDB,
OXYGEN, EXCESS Am, ANDUR*MOI.KI;UI.ARWKIOBT
1. Principle and Applicability
1.1 1'rineiple. A gas sample is extracted from a .stack,
by one of the following methods: (1) single-point, grab
sampling^ (2) single-point, integrated sampling', or (3)
multi-point, integrated sampling. The gas sample Is
analyzed for percent carbon dioxide (COi), percent oxy-
tieu (O<), and, it necessary, |>ereent carbon monoxide
(CO). It a dry molecular wviuht determination is to bo
made, either an Orsat or a Kyi-ite.' analyzer may be used
for the analysis; for excess air or emission rate correction
factor determination, an Orsat analyzer must be used.
1.2 Applicability. This method Is applicable tor de-
termining COi and Oj concentrations, excess air, and
dry molecular weight of a sample from a gas stream of a
fossil-fuel combustion process. The method may also be
applicable to other processes where it has been determined
that compounds other than (.'():, O>, CO, and nitrogen
(Mi) are not present in concentrations sufficient to
affect the results.
Other methods, as well as modifications to the, proce-
dure described herein, are also applicable for some or all
of the above determinations. Examples of spedlic meth-
ods and modifications include: (1) a multi-point samp-
ling method using an Orsat analyzer to analyze indi-
vidual grab samples obtained at each point; (2) a method
using COz or Oj and stoichiometrtc calculations to deter-
mine dry molecular weight and excess air; (3) assigning a
value of 30.0 for dry molecular weight, in lieu of actual
measurements, for processes burning natural gas, eoal, or
oil. These methods and modifications may be used, but,
•.in' «t!i\wt. t/> in,. .mnrnvMl .if ihe. Administrator. I'.s.
Knvininin'-inal 1'rutee'n1 At.-ney87
'-. Apparatus
As an altcrnaiive Ip the sampling ai>;>,irains and sys-
tems described herein, other sampling syslems (e.g.,
liquid displacement) may be used provided such systems
are capable of obtaining a representative sample and
maintaining a constant sampling rate, and are otherwise
capable of yielding acceptable results. Use of such
systems is subject to the approval of the Administrator.
2.1 Grab Sampling (Figure 3-1).
•2.1.1 Probe. The probe should be made of stainless
steel or borosilicdte glass tubing and should bo equipped
with an iu-stack or out-stock filter to remove paniculate
matter (a plug of glass wool is satisfactory for this pur-
pose). Any other material inert to Oi, COi, CO, and Nj
and resistant to temperature at sampling conditions may
be used for the probe; examples of such material are
aluminum, copper, quartz glass and Te.llon.
2.1.2 Purnp. A one-way squeeze bulb, or equivalent,
is used to transport the gas sample to the analyter,
2.2 Integrated Sampling (Figure 3-2).
2.2.1 Probe. A probe such as that described in Section
'.'.1.1 is suitable.
2.2.2 Condenser. An air-cooled or water-cooled con-
denser, or other condenser that will not remove Oi,
COi, CO, and NI, may be used to remove excess moisture
which wonld Interfere with tbe operation of the pump
and flow meter.
2.2.3 Valve. A needle valve is used to adjust sample
gas flow rate.
2.2.4 Pump. A leak-free, diaphregm-tvpe pump, or
equivalent, Is used to transport sample* gas to tbe flexible
bag. Install a small surge tank between the pump and
rate Jneter to eliminate the pulsation effect of the dia-
phragm pump on the rotameter.
2.2.6 Rate Meter. The rotameter, or equivalent rate
nieter, nsed should be capable of measuring flow rate
to within ±2 percent of the selected flow rate. A flow
rale range of MO to 1000 cm'/min is supcested.
2.2.6 Flexible Bat;. Any leak-dee plastic (e.g., Tedlar,
Xlylar, Teflon) or plastic-coated aluminum (e.g., alumi-
nized Mylar) bag, or equivalent, having a capacity
consistent with the selected flow rale and time length
of the test run, may be used. A capacity in the range of
M to 90 liters is suggested.
To leak-check the bag, connect it to a water manometer
•nd pressurize the bag to 5 to 10cm H:O (2 to 4 in. HiO).
Allow to stand for 10 minutes. Any displacement in the
water manometer indicates a leak. An alternative leak-
check method Is to pressurize the bag to 6 to 10 cm HiO
(2 to 4 in. BiO) and allow to stand overnight. A deflated
bag indicates a leak.
2.2.7 Pressure Gauge. A water-filled U-tube manom-
eter, or equivalent, of about 28 cm (12 in.) is used for
the flexible bag leak-check.
2.2.8 Vacuum Gauge. A mercury manometer, or
equivalent, of at least 760 mm Hg (30 in. Hg) is used for
tbe sampling train leak-check.
2.3 Analysis. For Orsat and Fyrite analyzer main-
tenance and operation procedures, follow the instructions
recommended by the manufacturer, unless otherwise
specified herein.
2.3.1 Dry Molecular Weight Determination. An Orsat
•nalyter or Fyrite type combustion gas analyzer may be
used.
2.3.2 Emission Rate Correction Factor or Excess Air
Determination. An Orsat analyzer must be used. For
low COt (less than 4.0 percent) or high Oi (greater than
15.0 percent) concentrations, the measuring burette of
the Great must have at least 0.1 percent subdivisions.
I. Dry Molecular WfifM Determination
A/ny of the three sampling and analytical procedures
described below may be used for determining the dry
molecular weight.
8.1 Single-Point, Grab Sampling and Analytical
Procedure.
8.1.1 The sampling point in the duct shall either be
at tbe eentroid of the cross section or at a point no closer
to the walls than 1.00 m (3.3 ft), unless otherwise specified
by the Administrator.
8.1.2 Bet up the equipment as shown In Figure 8-1,
•making sure all connections ahead of the analyzer are
tight and leak-free. If an Orsat analyzer is used, It is
recommended that the analyzer be leaked-checked by
following tbe procedure in Section 5; however, tbe leak-
check is optional.
8.1.3 Place the probe in the stack, with the tip of the
probe positioned at the sampling point; purge the sampl-
ing line. Draw a sample into the analyzer and imme-
diately analyze it for percent COi and percent Oi. Deter-
mine the percentage of the gas that Is Ni and CO by
subtracting the sum of the percent COi and percent Oi
from 100 percent. Calculate the dry molecular weight as
Indicated in Section 6.3.
3.1.4 Repeat the sampling, analysis, and calculation
procedures, until the dry molecular weights ol any three
grab samples differ from their mean by no more than
0.8 g/g-mole (0.3 Ib/lb-mole). Average these three molec-
ular weights, and report tbe results to the nearest
0.1 g/g-mole (IbAb-mole). .,.,.,,
3.2 Single-Point, Integrated Sampling and Analytical
3.2.1 The tampling point in the duct shall be located
•s specified in Section 3.1.1.
82.2 Leak-check (Optional) the flexible bag as In
Section 2.2.6. Set yp the equipment as shown in Figure
3-2. Just prior to sampling, leak-check (optional) the
train by placing a vacuum gauge at the condenser inlet,
pulling a vacuum of at least 250 mm Hg (10 in. Hg),
plugging the outlet at the quick disconnect, and then
turning off the pump. The vacuum should remain stable
Jor at least 0 S minute. Evacuate the flexible bag. Connect
the probe and place it in the stack, with the tip of the
probe posi I ioned at the sampling point; purge the sampl-
ing line. Next, connect the bag and make sure that all
connections are tight and leak free.
323 Sample at a constant rate. The sampling nin
should be simultaneous with, and for the same total
length of time as, the pollutant emission rale determina-
tion. Collection of at least 30 liters (1.00 ft>) of sample gas
is recommended; however, smaller volumes may be
collected, if desired.
3 2.4 Obtain one integrated flue gas sample during
web pollutant emission rale determination. Within 8
hours after tbe sample is taken, analyze it for percent
COi and percent Oi using either an Orsat analyzer or a
Fyrite-type combustion gas analyzer. If an Orsat ana-
lyzer is used, it is recommended that tbe Orsat leak-
rheck described in Section 5 be performed before this
determination; however, the chwk is optional. Deter-
mine the percentage of the gas that is IM and CO by sub-
tracting the sum of the oercent CO, and percent Oi
from 100 percent. Calculate the dry molecular weight as
indicated in Section 6.3. °'
i Mention of trade names or specific products does not
constitute endorsement by the Environmental Protec-
tion Agency.
FLEXIBLE TUBING
FILTER (GLASS WOOL)
TO ANALYZER
SQUEEZE BULB
Figure 3-1. Grab-sampling train.
III-Appendix A-14
-------
RATE METER
AIR-COOLED
CONDENSER
.PROBE
FILTER
(GLASS WOOL)
RIGID CONTAINER
Figure 3-2. Integrated gas-sampling train.
TIME
TRAVERSE
FT.
AVERAGE
Q
1pm
% DEV.a
'%DEV= (^1^)100 (MUSTBE<10%)
Figure 3-3- Sampling rate data.
Ill-Appendix A-15
-------
8.2.5 Repeat the analysis and calculation procedures
until the individual dry molecular weights (or any three
analyses differ from their mean by no more than 0.3
g/g-mole (0.3 Ib/lb-mole). Average these three molecular
weights, and report tbe results to the nearest 0.1 g/g-mole
(0.1 Ib/lb-mole).
3.3 Multi-Point, Integrated Sampling and Analytical
Procedure.
8.3.1 Unless otherwise specified by the Adminis-
trator, a minimum of eight traverse points shall be used
for circular stacks having diameters less then 0.61 m
(24 In.), a minimum of nine shall be used for rectangular
stacks having equivalent diameters less than 0.61 m
(24 in.), and a minimum of twelve traverse points shall
be used for all other cases. The traverse points shall be
located according to Method 1. The use of fewer points
is subject to approval of the Administrator.
3.3.2 Follow the procedures outlined in Sections 3.2.2
through 3.2.5, except for the following: traverse all sam-
pling points and sample at each point for an equal length
of time. Record sampling data as shown in Figure 3-3.
d. Emiation Rate Corrfdien Factor or E/«M Air Dtltr-
inlnatiott
NOTE.—A Fyrite-type combustion gas analyser is not
acceptable for eicess air or emission rate correction factor
determination, unless approved by the Administrator.
If both percent COi and percent Oj are measured, tbe
analytical results of any of the three procedures given
below may also be used for calculating the dry molecular
weight.
Each of the three procedures below shall be used only
when specified in an applicable subpart of the standards.
The use of these procedures for other purpose? must have
specific prior approval of the Administrator.
4.1 Single-Point, Qrab Sampling and Analytic.-J
Procedure.
4.1.1 The sampling point in the duct shall efthcr be
at the centroid of the cross-section or at a point no closer
to the walls than 1.00 m (3.3 ft), unless olberw ist specified
by the Admiiustrator.
4.1.2 Bet up the equipment as shown in Figure 3-1,
making sure all connections ahead of the analyzer are
tight and leak-free. Leak-check the Orsat analyzer ac-
cording to the procedure described in Section 5. Tins
leak-check is mandatory.
4.1.3 Place the probe in tbe stack, with tbe tip of the
probe positioned at the sampling point; purge the cam-
pling line. Draw a sample Into the analyzer. For «missio i
rate correction factor determination, Immediately ana-
lyze the sample, as outlined in Sections 4.1.4 and 4.1..'>,
for percent COi or percent Ot. If eicess air is desired,
proceed as follows: (1) Immediately analyze the sample,
as In Sections 4.1.4 and 4.1.5, for percent COi. Oi, and
CO; (2) determine the percentage of the gas that Is Ni
by subtracting the sum of the percent COj, percent Oi,
and percent CO from 100 percent; and (3) calculate
percent excess air as outlined In Section 6.2.
4.1.4 To ensure complete absorption of the COt, Oi,
or if applicable, CO, make repeated passes through each
absorbing solution until two consecutive readings are
the same. Several passes (three or four) should be made
between readings. (If constant readings cannot be
obtained after three consecutive readings, replace the
absorbing solution.)
4.1.6 After the analysis Is completed, leak-check
(mandatory) the Orsat analyzer once again, as described
in Section 5. For the results of the analysis to be valid,
the Orsat analyzer must pass this leak test before and
after the analysis. NOTE.—Since this single-point, grab
sampling and analytical procedure Is normally conducted
In conjunction with a single-point, grab sampling and
analytical procedure for a pollutant, only ono analysis
is ordinarily conducted. Therefore, great care must bo
taken to obtain a valid sample and analysis. Although
In most cases only COi or Oi is required, it is recom-
mended that both COi and Oi be measured, and that
Citation f> in the Bibliography be used to validate the
analytical data.
4.2 Single-l'oint, Integrated Sampling nnd Analytic.,I
Procedure.
4.2.1 The sampling point in the duct shall DI: IO-MH-I
as specified in Section 4.1.1.
4.2.2 Leak-check (mandatory) the flexible bag n« in
Section 2.2.6. Set up the equipment as shown in Figure
3-2. Just prior to sampling, leak-check (mandatory) the
train by placing a vacuum gauge at the condenser inlet,
pulling a vacuum of at least 250 mm llg (10 in. HR),
plugging the outlet at the quick disconnect, and then
turning of? the pump. The vacuum shall remain stable
for at least 0.5 minute. Evacuate tho flexible bag. Con-
nect the probe and place It in tbe stack, with tbe tip of the
probe positioned at tbe sampling point; purge tbe sam-
pling line. Next, connect the bag and make cure that
all connections are tight and leak free.
4.2.3 Sample at a constant rate, or as specified by tbe
Administrator. The sampling run must be simultaneous
with, and for the same total length of time as, the pollut-
ant emission rate determination. Collect at least 30
liters (1.00 ft1) of sample gas. Smaller volumes may be
collected, subject to approval of the Administrator.
4.2.4 Obtain one integrated flue gas sample during
each pollutant emission rate determination. For emission
rate correction factor determination, analyze the sample
within 4 hours after it is taken for percent COi or percent
Oi (as outlined in Sections 4.2.5 through 4.2.7). The
Orsat analyzer must be leak-checked (see Section 5)
before the analysis. If excess air is desired, proceed as
follows: (1) within 4 hours after the sample is taken,
analyze it (as in Sections 4.2.5 through 4.2.7; lor percent
CO;. O«, and CO: (2) determine the percentage of the
gas llmt'is Ni by subtracting the sum of the pen-em CUi.
percent Oi, and percent CO from 100 percent: t3) cal-
culate percent excess air, as outlined in Section 6.-'.
4.2.5 To ensure complete absorption of the COi. Oi,
or if applicable, CO, make repeated passes through each
absorbing solution until two consecutive readings are I lie
same. Several passes (three or four) should be made be-
tween readings. (If constant readings cannot be obtained
after three consecutive reading?, replace the absorbing
solution.)
4.2.6 Repeat the analysis until the follow ing criteria
4.2.6.1 For percent COj, repeat the analytical pro-
cedure until tbe results of any three analyses differ by no
more than (a) 0.3 percent by volume when COi Is greater
than 4.0 percent or (b) 0.2 percent by volume when CO>
is less than or equal to 4.0 per.-etit. Average the three oc-
ceptablc values of percent COi and report the results to
the nearest 0.1 percent.
4262 For percent O:. repeat the analytical procedure
until the results of any three analyses diOer by uo more
than (a) 0.3 percent by volume when Oi Is less than 15.0
per. < -it oi il» " :; jvrcent by volume when Oj is greater
than ..-I •_•::'..ij " ;>-n-eiit. Average the three accept-
alile vai'ic* !•• -.-lit n- and report the results to
the nearest 0.' nerce-it. °'
4.2.6.3 For pi.itoi.i c ~. irt'ut the analytical proce-
dure until tin1 results of any three analyses differ by no
more than 0.3 percent. Average the three acceptable
values of percent C 0 and report the results to the nearest
0.1 percent.
4.2.7 After the analysis is completed, leak-check
(mandatory) the Orsat analyzer once again, as described
in Sections. Fortheresultsoftheanalysistobe valid, the
Orsat analyzer must pass this leak test before and after
the analysis. Note: Although in most instances only COi
or Oi is required, it is recommended that both COi and
Oi be measured, and that Citation 5 in the Bibliography
be used to validate the analytical data.
4.3 Multi-Point, Integrated Sampling and Analytical
Procedure.
4.3.1 Both the minimum number of sampling points
and the sampling point location shall be as specified in
Section 3.3.1 of this method. The use of fewer points than
specified to Subject to the approval of the Administrator.
4.3.2 Follow the procedures outlined in Sections 4.2.2
through 4.2.7, except for the following: Traverse all
sampling points ana sample at each point for an equal
length of time. Record sampling data as shown in Figure
8-3.
6. Ltot-dieek Procedure Jar Ortat Analyzeri
Moving an Orsat analyzer frequently causes it to leak.
Therefore, an Orsat analyzer should be thoroughly leak-
checked on site before the flue gas sample is introduced
into it. The procedure for leak-checking an Orsat analyzer
is:
6.1.1 Bring the liquid level in each pipette up to the
reference mark on the capillary tubing and then close tbe
pipette stopcock.
5.1.2 Raise the leveling bulb sufficiently to bring the
confining liquid meniscus onto the graduated portion of
tbe burette and then close the manifold stopcock.
9.1.3 Record the meniscus position.
5.1.4 Observe the meniscus in the burette and tbe
liquid level in the pipette for movement over the next 4
minutes.
6.1.5 For the Orsat analyzer to pass the leak-check,
two conditions must be met.
6.1.5.1 The liquid level in each pipette must not fall
below the bottom of the capillary tubing during this
4-mlnute interval.
6.1.5.2 The meniscus In the burette must not change
by more than 0.2 ml during this 4-mlnuteinterval.
5.1.6 If the analyzer falls the leak-check procedure, oil
rubber connections and stopcocks should be checked
until the cause of the leak Is identified. Leaking stopcocks
must be disassembled, cleaned, and regreased. Leaking
rubber connections must be replaced. Alter the analyzer
la reassembled, the leak-check procedure must ba
repeated.
0. CaleulaUmu
0.1 Nomenclature.
Mj= Dry molecular weight, g/g-mole (Ib.flb-mole).
%EA=Percent excess air.
%COs=Percent COi by volume (dry basis).
%O»=Percent Oiby volume (dry basis).
%CO=Peroent CO by volume (dry basis).
%Ns=Percent Ni by volume (dry basis).
0.264= Ratio of Oi to Ni in air, v/v.
0.280=Molecular weight of Nj or CO, divided by 100.
0.320=Molecular weight of Oi divided by 100.
0.440=Molecular weight of CO: divided by 100.
6.2 Percent Eicess Air. Calculate the percent excess
air (if applicable), by substituting the appropriate
values of percent Oi, C O, and Nj (obtained from Section
4.1.3 or 4.2.4) into Equation 3-1.
%EA=
%02-0.5%CO
10.264 %N2- ( %02-0.5 %CO)
Equation 3-1
100
87
NOTE.—The equation above assumes that ambient
air is used as the source of Oi and that the fuel does not
contain appreciable amounts of N; (as do coke oven or
blast furnace gases). For those cases when appreciable
amounts of N> are present (coal, oil, and natural gas
do not contain appreciable amounts of NO or when
oxygen enrichment is used, alternate methods, subject
to approval of the Administrator, are required.
6.8 Dry Molecular Weight. Use Equation 3-2 to
calculate the dry molecular weight of the stack gas
ftfj=0.440(%COj)+0.320(%0.)+0.280(%N,+%CO)
Equation 3-2
NOTE.—The above equation does not consider argon
In air (about 0.9 percent, molecular weight of 37.7).
A negative error of about 0.4 percent Is introduced.
The tester may opt to include argon in the analysis using
procedures subject to approval of the Administrator.
7. Bibliography
1. Altshuller, A. P. Storage of Oases and Vapors in
Plastic Bags. International Journal of Air and Water
Pollution. 6:75-81.1963.
2. Conner, William D. and I. S. Nader. Air Sampling
with Plastic BWS. Journal of th» Arryrican Industrial
Hypiene Association. M:2M-297.1U64. 87
3. Burrell Manual for UBS Analysts, Seventh edition.
Burrell Corporation, 2223 Fifth Avenue, Pittsburgh,
Pa. 15219.1051.
• 4. Mitchell, W. J. and M. R. Midgett. Field Reliability
of the Orsat Analyzer. Journal of Air Pollution Control
Association £0:491-195. May 1976.
5. Shigehara, R. T., R. M. Neulicht, and W. S. Smith.
Validating Orsat Analysis Data from Fossil Fuel-Fired
Units. Stack Sampling News. 4(2):21-26. August, 1976.
III-Appendix A-16
-------
METHOD 4—DETESMINATIOH or MOISTURE CONTEXT
IN STACK OASES
1. Principle and Applicability
1.1 Principle. A gas sample is extracted at a constant
rate from the source; moisture is removed from the sam-
ple stream and determined either volumetrically 01
gravimetrically.
1.2 Applicability. This method is applicable (or
determining the moisture content off stack gas.
Two procedures are given. The first is a reference
method, for accurate determinations oJ moisture content
(such as are needed to calculate emission data). The
second is an approximation method, which provides
estimates of percent moisture to aid in setting isokinetic
sampling rates prior to a pollutant emission raeasure-
xment run. The approximation method described herein
Is only a suggested approach; alternative means for
approximating the moisture content, e.g., drying tubes,
wet bulb-dry bulb techniques, condensation techniques,
stoichiometric calculations, previous experience, etc.,
are also acceptable.
The reference method is often conducted simultane-
ously with a pollutant emission measurement run; when
It is, calculation of percent isokinetic, pollutant emission
rate, etc., for the run shall be based upon the results of
the reference method or its equivalent; these calculations
shall not be based upon the results of the approximation
method, unless the approximation method is shown, to
the satisfaction of the Administrator, U.S. Environmen-
tal Protection Agency, to be capable of yielding results
within 1 percent HjO of the reference method.
NOTE.—The reference method may yield questionable
results when applied to saturated gas streams or to
streams that contain water droplets. Therefore, when
these conditions exist or are suspected, a second deter-
mination of the moisture content shall be made simul-
taneously with the reference method, as follows: Assume
that the gas stream is saturated. Attach a temperature
sensor (capable of measuring to *1° C (2° F)| to the
reference method probe. Measure the stack gas tempera-
ture at each traverse point (see Section 2.2.1) during the
reference method traverse: calculate the average stack
gas temperature. Next, determine the moisture percent-
age, either by: (1) using a psychrometric chart and
making appropriate corrections if stack pressure is
different from that of the chart, or (2) using saturation
vapor pressure tables. In cases where the psychrometric
chart or the saturation vapor pressure tables are not
applicable (based on evaluation of the process), alternate
methods, subject to the approval of the Administrator,
shall be used.
2. Reference Method
The procedure described in Method 5 for determining
moisture content is acceptable as a reference method.
2.1 Apparatus. A schematic of the sampling train
used in this reference method is shown in Figure 4-1.
All components shall be maintained and calibrated
according to the procedure outlined in Method 5.
2.1.1 Probe. The probe is constructed of stainless
iteel or glass tubing, sulfieiently heated to prevent
water condensation, and is equipped with a filter, either
in-slack (e.g., a plug of gloss wool inserted into the end
of the probe) or heated out-stack (e.g., as described in
Method 5), to remove paniculate matter.
When stack conditions permit, other metals or plastic
tubing may be used for the probe, subject to the approval
of the Administrator.
2.1.2 Condenser. The condenser consists of four
Imoingers connected in series with ground glass, leak-
free fittings or any similarly leak-free non-contaminating
fittings. The first, third, and fourth impingers shall be
of the Oreenburg-Smith design, modified by replacing
the tip with a 1.3 centimeter (H inch) ID glass tube
extending to about 1.3 cm (H in-) from the bottom of
the flask. The second impjnger shall be of the Greenburg-
flmith design with the standard tip. Modifications (e.g.,
using flexible connections between the impingers, using
materials other than glass, or using flexible varuum lines
to connect the lillcr holder to the condenser) may be
used, s.uhjei't to the approval of the Administrator.
The first two impingers shall contain known volumes
of water, tlie third shall be empty, and the fourth shall
contain a known weight of 6- to Irt-mesh indicating type
silica gel, or equivalent di'Sicomt. If the silica gel has
been previously used, dry at 175° C (350° F) for 2 hours.
New silica gel may be used as received. A thermometer,
capable of measuring temperature to within 1° C (2° F),
shall be placed at the outlet of the fourth impinger, for
monitoring purposes.
Alternatively, any system may be used (subject to
the approval of the Administrator) that cools the sample
fas stream and allows measurement of both the water
that has been condensed and the moisture leaving the
condenser, each to within 1 ml or 1 g. Acceptable means
are to measure the condensed water, either gravi-
inetrieally or volumetrically, and to measure the mois-
ture leaving the condenser by: (1) monitoring the
temperature and pressure at the exit of the condenser
and using Dalton's law of partial pressures, or fj) passing
the sample gas stream through a tared silica gel (or
equivalent desiccant) trap, with exit gases kepl-below
20° C (68° F). and determining the weight gain. °'
FILTER
(EITHER IN STACK
OR OUT OF STACK)
STACK
WALL
CONDENSER-ICE BATH SYSTEM INCLUDING
SILICA GEL TUBE
AIR-TIGHT
PUMP
Figure 4-1. Moisture sampling train-reference method.
Ill-Appendix A-17
-------
If means other than silica gel are used to determine the
amount ol moisture leaving the condenser, it is recom-
mended that silica gel (or equivalent) still be used be-
tween the condenser system and pump, to prevent
moisture condensation in the pump and metering
devices and to avoid the need to make corrections for
moisture in the metered volume.
2.1.3 Cooling System. An ice bath container and
crushed ice (or equivalent) are used to aid in condensing
moisture.
2.1.4 Metering System. This system includes a vac-
uum gauge, leak-free pump, thermometers capable of
measuring temperature to within 3° C (6.4° F), dry gas
meter capable of measuring volume to within 2 percent,
and related equipment as shown in Figure 4-1. Other
metering systems, capable of maintaining a constant
sampling rate and determining sample gas volume, may
be used, subject to the approval of the Administrator.
2.1.5 Barometer. Mercury, aneroid, or other barom-
eter capable of measuring atmospheric pressure to within
2.6 mm Hg (0.1 in. Hg) may be used. In many cases, the
barometric reading may be obtained from a nearby
national weather service station, in which case the sta-
tion value (which is the absolute barometric pressure)
shall be requested and an adjustment for elevation
differences between the woather station and the sam-
pling point shall he applied at a rate of minus 2.B mm Hg
(0.1 in. Ug) per 30 m (100 ft) elevation increase or vice
versa for elevation decrease.
2.1.6 (Jraduated Cylinder and.'or Balance. These
items are used to measure condensed water and moisture
caught in the silica gel to within 1 ml or 0.5 g. Graduated
cylinders shall have subdivisions no greater than 2 ml.
Most laboratory balances are capable of weighing to the
nearest 0.0 g or less. These balances are suitable for
use here.
2.2 Procedure. The following procedure is written for
a condenser system t.such as the impinger system de-
scribed in Section 2.1.2) incorporating volumetric analy-
sis to measure the condensed moisture, and silica gel and
gravimetric analysis to measure the moisture leaving the
condenser.
2.2.1 Unless otherwise specified by the Administrator,
a minimum of eight traverse points shall be used for
circular stacks having diameters less than 0.61 m (24 in.),
a minimum of nine points shall be used for rectangular
stacks having equivalent diameters less than 0.61 m
(24 in.), and a minimum of twelve traverse points shall
be used iu all other cases. The traverse points shall be
located according to Method 1. The use of fewer points
is subject to the approval of the Administrator. Select a
suitable probe and probe length such that all traverse
points can be sampled. Consider sampling from opposite
sides of the stack (four total sampling ports) for large
stacks, to permit use of shorter probe lengths. Mark the
probe with heat resistant tape or by some other method
to denote the proper distanfe into the stack or duct for
each sampling point. Vlace known volumes of water in
the first two impingers. Weigh and record the weight of
the silica gel to the nearest 0.5 g, and transfer the silica
gel to the fourth impinger; alternatively, the silica gel
may Urst be transferred to the impinger .and the weight
of the silica gel plus impinger recorded.87
2.2.2 Select a total sampling time such that a mini-
mum total gas volume of O.tiO sem (21 scf) will be col-
lected, at a rate no greater than 0.021 m'/min (O.T5 elm).
When both moisture content and pollutant emission rate
are to be determined, the moisture determination shall
be simultaneous with, and for the same total length of
time as. the pollutant emission rate run, unless otherwise
specllied in an applicable subpart of the standards.
2.2.3 Set up the sampling train as shown in Figure
4-1. Turn on the probe heater and (if applicable) tbe
niter heating system to temperatures ol about 120° C
(248° F), to prevent water condensation ahead of the
condenser: allow time for the temperatures to stabilise.
Place crushed ice in the Ice bath container. It ii recom-
mended, but not required, that a leak check be dom, m
follows: Disconnect the probe from tbe first impinger or
(if applicable) from the filter bolder. Plug the Inlet to the
first impinger (or filter bolder) and pull a 380 mm (15 in.)
Hg vacuum; a lower vacuum may be used, provided that
it is not exceeded during the test. A leakage rate In
excess of 4 percent of the average sampling rat* or 0.00057
m'/min (0.02 cfm), whichever Is less, is unacceptable.
Following the leak check, reconnect the probe to the
sampling" train. 87
2.2.4 During tbe sampling run, maintain a sampling
rate within 10 percent of constant rate, or as specified by
the Administrator. For each run, record the data re-
quired on the example data sheet shown In Figure 4-2.
Be sure to record the dry gas meter reading at the begin-
ning and end of each sampling time increment and when-
ever sampling Is halted. Take other appropriate readings
at each sample point, at least once during each time
Increment.
2.2.S To begin sampling, position the probe tip at the
nrst traverse point. Immediately start the pump and
adjust the flow to the desired rate. Traverse the cross
section, sampling at each traverse point for an equal
length of time. Add more ice and, if necessary, salt to
maintain a temperature of less than 20° C (68° F) at the
silica gel outlet.
2.2.6 After collecting the sample, disconnect the probe
from the filter holder (or from the first impinger) and con-
duct a leak check (mandatory) as described in Section
1.2.8. Record the leak rate. If the leakage rate exceeds the
allowable rate, the tester shall either reject the test re-
iults or shall correct the sample volume as in Section 6 3
of Method 5. Next, measure the volume of the moisture
condensed to the nearest ml. Determine the increase in
weight of the silica gel (or silica gel plus impinger) to the
nearest 0.5 g. Record this information (see example data
•beet. Figure 4-3) and calculate the moisture percentage,
as described in 2.3 below.
PLANT
LOCATION.
OPERATOR.
DATE
BUN NO
AMBIENT TEMPERATURE.
BAROMETRIC PRESSURE.
PROBE LENGTH m(ft)
SCHEMATIC OF STACK CROSS SECTION
TRAVERSE POINT
NUMBER
TOTAL
SAMPLING
TIME
(fl).nu..
AVERAGE
STACK
TEMPERATURE
«C (BF)
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE METER
(AH).
mmtinj H{0
METER
READING
GAS SAMPLE
VOLUME
mJ(ftl)
AV.
•'(hi
GAS SAMPLE TEMPERATURE
AT DRY GAS METER
MLET
(Tmin).»c(«F)
A«|.
A*.
OUTLET
(TmoBtl.^CI'Fl
A*.
TEMPERATURE
OF GAS
LEAVING
CONDENSER OR
LAST IMPINGER.
•Ct'F)
Figure 4-2. Field moisture determination-reference method.87
III-Appendix A-18
-------
HEATED PROBE
SILICA GEL TUBE
FILTER
(GLASS WOOL)
ICE BATH
RATE METER,
VALVE
DRY GAS ]
.METER y
MIDGET IMPINGERS
PUMP
Figure 4-4. Moisture-sampling train - approximation method.
LOCATION.
TEST
COMMENTS
DATE.
OPERATOR
BAROMETRIC PRESSURE
CLOCK TIME
GAS VOLUME THROUGH
METER, (Vm),
m3 (ft3)
RATE METER SETTING
m3/min. (ftVmin.)
METER TEMPERATURE,
°C (°F)
'
Figure 4-5. Field moisture determination - approximation method.
Ill-Appendix A-19
-------
2.3 Calculations. Carry out the following calculations
retaining at least one extra decimal figure beyond thai of
the acquired data. Round off figures after final calcula-
tion.
FINAL
INITIAL
DIFFERENCE
(WINGER '
VOLUME.
ml '
SILICA GEL
WEIGHT.
9
Fiijurc 4 3. Analytical data - reference method.
2..1.1 Nomenclature.
./?,„= Proportion of water vapor, by volume, in
the eas stream.
A/w = Moleeuiar weight of water, 18.0 g-'g-mole
(18.01b/lb-mole).
Pm — Absolute pressure (for this method, same
as barometric pressure) at the dry pus meter,
nun Hg (in. fig).
f.u- Standard absolute pressure, 701) mm Hg
(29.92 in. Hg).
R = Ideal gas constant, 0.06236 (mm Kg) tin1)/
(It-mole) (°K) for metric units and 21.85 (in.
HB) (ft3)/(lb-mole) (°B) for English units.
7\, = Absolute temperature at meter. °K (°R).
'J',n=3tandard absolute temperature, 203° K
(S28" R).
Vn — Dry gas volume measured by dry gas meter,
dcm (dcf).
Al/m = Incremental dry gas volume measured by
dry gas meter at each traverse point, dcm
(dcf).
V»(.id> = Dry gas volume measured by the dry gas
meter, corrected to standard conditions,
dscm (dscf).
V*,luii=Volume of water vapor condensed corrected
to standard conditions, scm (set).
Vini(tiif) =Volume of water vapor collected in silica
gel corrected to standard conditions, scm
(scQ.
Vf—Final volume of condenser water, ml.
Vi=Initial volume, if any, of condenser water,
ml.
W;=Final weight of silica gel or silica gel plus
irupinger, g.
W,=Initial weight of siliea gel or silica gel plus
impinger, g.
V=Dry gas meter calibration factor.
p»=Densityn,of water, 0.9«82 g/ml (0.003201
v Ib/ml). 87
2.3.2 Volume of water vapor condensed.
V"u.,(st.» =
Mqlmlion 4 1
where:
#1=0.001333 m'/uil for metric units
=0.04707 fts/mt for English units
2.3.3 Volume of water vapor collected in silica gel.
where:
jri=0.001335 m'/'g for metric units
=0.04716 fti/g for English unils
2.3.4 Sample gas volume.
Kquation 4-2
where:
A'j=»0.38fiS°K/inm Up fur metric unils
= 17.64 °R/in. UK for KiiKlish units
il 43
NOTE.— If the post-test leak rate t
eeeds the allowable rate, eon-ret the
Kiiurtiitm 4-3, as described in Section
1! .'ty Moisture Content.
r I
ccti..n •_• -j H) cx-
value of \'m in
0.3 of Method 5.
Kqnatinn 4-4
XOTK.—In saturated or moisture droplet-laden gas
streams, two calculations of the. moisture content of the
stack gas shall be made, one using a value based upon
the saturated conditions (see Section 1.2), and another
based upon the results of the impinger analysis. The
lower of these two values of Blt, shall be considered cor-
rect.
2.3.H Verification of constant sampling rate. For each
time increment, determine the AK». Calculate the
average, if the value for any time increment dillers from
the average by more than 10 percent, reject the results
and repeat the run.
3. Approximation Method
The approximation method described below is pre-
sented only as a suggested method (see Section 1.2).
3.1 Apparatus.
3.1.1 Probe. Stainless steel or glass tubing, sufficiently
heated to prevent water condensation and equipped
with a filter (either in-slack or heated out-stack) to re-
move participate matter. A ping of glass wool, inserted
into the end of the probe, is a satisfactory filter.
3.1.2 Impingers. Two midget impingers, each with
30 ml capacity, or equivalent.
3.1.3 Ice Bath. Container and ice, to aid in condens-
ing moisture in impingers.
3.1.4 Drying Tube. Tube packed with new or re-
generated 6- to 16-mesh indicating-type silica gel (or
equivalent desiceant), to dry the sample gas and to pro-
let:! the meter and pump.
3.1.5 Valve. Needle valve, to regulate the sample gas
flow iat.>.
3.1.8 Pump. Leak-free, diaphragm type, or equiva-
lent, to pull the gas sample through the train.
3.1.7 Volume meter. Dry gas meter, sufficiently ac-
curate to measure the sample volume within 2%, and
calibrated over the range of flow rates and conditions
actually encountered during sampling.
3.1.8 Rate Meter. Rotameter, to .measure the flow
range from 0 to 31 pm (0 to 0.11 cfm). °/
3.1.9 Graduated Cylinder. 25 ml.
3.1.10 Barometer. Mercury, aneroid, or other barom-
. eter, as described in Section 2.1.5 above.
3.1.11 Vacuum Gauge. At least 760 mm Ilg (HO in.
Hg) gauge, to be used for the sampling leak cheek.
3.2 Procedure.
3.2.1 Place exactly 5 ml distilled water in each im-
pinger. Leak check the sampling trainas follows:
Temporarily insert a vacuum gauge at or
near the probe inlet; then, plug the probe
inlet and pull a vacuum of at least 250 mm
Hg (10 in. Hg). Note, the time rate of
change of the dry gas meter dial: alternati-
vely, a rotameter (0-40 cc/min) may be tem-
porarily attached to the dry gas meter
outlet to determine the leakage rate. A leak
rate not In excess of 2 percent of the aver-
age sampling rate Is acceptable.
NOTE.—Carefully release the probe inlet
pluft before turning off the pump.'7
3.3.2 Connect the probe, insert it into the stack, and
sample at a constant rate of 21pm (0.071 cfm). Continue
sampling until the dry gas meter registers about 30
liters (1.1 ft1) or until visible liquid droplets are carried
over from the first impinger to the second. Record
temperature, pressure, and dry gas meter readings as
required by Figure 4-5.
3.2.3 After collecting the sample, combine the con-
leuis of the two impingers and measure the volume to the
nearest 0.5 ml,
.1.3 Calculations. The calculation method presented is
designed to estimate the. moisture In the stack gas;
therefore, other data, which are only necessary for ac-
curate moisture determinations, are not collected. The
following equations adequately estimate ihn moisture
content, for the purpose of determining isokinctic sam-
pling rate settings.
3.3.1 Nomenclature.
/?,,» = Approsimate proportion, by volume, nf
water vapor in the gas stream leaving the
second impinger. 0.025.
B«.= Water vapor in the gas stream, proportion by
volume.
A/.=Molecular weight of water, 18.0 g/g-mole
(18.01b/lb-mol6)
/".^Absolute pressure (for this method, same as
barometric pressure) at the dry gas meter.
P,n= Standard absolute pressure. 760 mm Hi
(29.92 in. Hg).
fl= ideal gas constant, 0.06236 (mm Hg) (mi)/
(g-mole) (°K) for metric units and 21.85
(in. Hg) (ft")/lb-mole) (°K) for English
T.=Absolute temperature at meter, "K (°R)
",^Si^f^ »bsolute temperature, 293° K
£
V/- Final volume of impinger contents, ml.
•^Initial volume of Impinger contents, ml.
K»-l)ry gas volume measured by dry gas meter
dcm (dcf).
v»(.i<)=Dry gas volume measured by dry gas meter
corrected to standard conditions, dscm
(dscf).
»'.,(.n>=Volume of water vapor condensed, corrected
to standard conditions, scm (set).
p*: Density of water, 0.9982 g/ml (0.002201 Ib/ml).
Y = Dry gas meter calibration factor. 87
3.3.2 Volume of water vapor collected.
Equation 4-5
where:
K,=0.001333 mVml for metric units
=0.04707 ft'/ml for English units.
3.3.3 Gas volume.
Equation 4-fl
87
wtere:
£1=0.3868 °K/mm Hg tor metric units
=17.84 "B/in. Hg for English units
3..1.4 Approiimate moisture content.
+(0.025)
4. Calibration
Equation 4-7
87
4.1 For the reference nicihod, calibrate equipment aa
specified in the following sections of Method 5: Section 5.3
(metering system); Section 6.5 (temperature gauges);
and Section 5.7 (barometer). The recommended leak
check of the metering system (Section 5.6 of Method 5)
also applies to the reference method. For the approxima-
tion method, use the procedures outlined in Section 5.1.1
of Method 6 to calibrate the metering system, and the
procedure of Method 5, Section 5.7 to calibrate the
barometer.
5. Bibliography
1. Air Pollution Engineering Manual (Second Edition).
Danielson, J. A. (ed.). U.S. Environmental Protection
Agency, Office of Air Quality Planning and Standards.
Research Triangle Park, N.C. Publication No. AP-40.
1973.
2. Devorkin, Howard, et al. Air Pollution Source Test-
ing Manual. Air Pollution Control District, Los Angeles,
Calif. November, 1963.
3. Methods for Determination of Velocity, Volume,
Dust and Mist Content of Gases. Western Precipitation
Division of Joy Manufacturing Co., Los Angeles. Calif.
Bulletin WP-50.1968.
III-Appendix A-20
-------
METHODS— DETERMINATION OFPARTICCLATE EMISSIONS
FROM STATIONARY SOURCES
1. Principle and ApfHeabUily
1.1 Principle. Particular matter is withdrawn iso-
kinetically from the source and collected on a glass
fiber filter maintained at a temperature In the range ol
120±14« C (248±2S° F) or such other temperature aa
specified by an applicable subpart of the standards or
approved by the Administrator, U.S. Environmental
Protection Agency, for a particular application. The
paniculate mass, which includes any material that
condenses at or above the filtration temperature, is
determined gravimetrically after removal of uncombined
water.
1.2 Applicability. This method is applicable for the
determination of paniculate emissions from stationary
sources.
2. Apparatus
2.1 Sampling Train. A schematic of the sampling
train used in this method is shown in Figure 5-1. Com-
plete construction details are given in APTD-0581
(Citation 2 in Section 7); commercial models of this
train are also available. For changes from APTD-0581
and for allowable modifications of the train shown in
Figure 5-1, see the following subsections.
The operating and maintenance procedures for the
sampling train are described in APTD-0576 (Citation 3
In Section 7). Since correct usage is important in obtain-
ing valid results, all users should read: APTD-0576 and
adopt the operating and maintenance procedures out-
lined in it, unless otherwise specified herein. The sam-
pling train consists of the following components:
1.1-1 Probe Nozzle. Stainless steel (316) or glass with
•harp, tapered leading edge. The angle of taper shall
be <30° and the taper shall be on the outside to preserve
• constant internal diameter. The probe nozzle shall be
of the button-hook or elbow design, unless otherwise
•peclfied by the Administrator. If made of stainless
steel, the nozzle shall be constructed from seamless tub-
Ing; other materials of construction mavbe used, subject
to the approval of the Administrator. B/
A range ol notzle sizes suitable for isokinetic sampling
Ibould be available, e.g., 0.32 to 1.27 cm (>4 to H in.)—
or larger if higher volume sampling trains are used—
inside diameter (ID) notzles in increments of 0.16 cm
(M« in.). Each nozzle shall be calibrated according to
the procedures outlined in Section 5.
2.1.2 Probe Liner. Borosilicate or quartz glass tubing
with a heating system capable of maintaining a gas tem-
perature at the eiit end during sampling of 120±14° C
(248±25° F), or such other temperature as specified by
•n applicable subpart of the standards or approved by
the Administrator for a particular application. (The
tester may opt to operate the equipment at a temperature
lower than that specified.) Since the actual temperature
at the outlet of the probe is not usually monitored during
templing, probes constructed according to APTD-0581
and utilizing the calibration curves of APTD-0576 (or
calibrated according to the procedure outlined in
APTD-0576) will be considered acceptable.
Either borosilicc.te or quart* glass probe liners may be
•nd for stack temperatures up to about 480° C ,900° F):
quartz liners shall be used for temperatures between 480
end 900° C (900 and 1,650° F;. Both types of liners may
be used at higher temperatures than specified for short
periods of time, subject to the approval of the Adminis-
trator. The softening temperature for borosilicate is
820° C (1,508° F), and for quartz it is 1,501 ° C (2,732° F).
Whenever practical, every effort should be made to use
borosilicate or quaru glass probe liners. Alternatively.
metal liners (e.g., 316 stainless steel, Incotoy 825,: Or other
corrosion resistant metals) made of aeamleas tubing may
be used, subjec. to the approval of the Administrator.
2.1.3 Pilot Tube. Type 8, as described in Section 2.1
of Method 2, or other device approved by the Adminis-
trator The pilot tube shall be attached to the probe (as
rtiown in Figure 5-1) to allow constant monitoring of the
•tack gat velocity The impact (high pressure) opening
plane of the pilot tube shall be even with or above the
nozzle entry plane (see Method 2, Figure 2-6b) during
sampling. The Type S pilot tube assembly shall have a
known coefficient, determined as outlined in Section 4 of
Method 2.
> Mention ol trade names or specific products does not
constitute endorsement by the Environmental Protec-
tion Agency.
2.1.4 Differential Pressure Gauge. Inclined manom-
eter or equivalent devo Uwo), as uscribed in Section
2.2 of Method 2. One manometer shall be'used .or velocity
head (Ap) readings, and the other, for orifice differential
pressure readings.
2.1.5 Filter Holder. Borosilicate frtass, with a glass
frit filter support and a silicone rubber gasket. Other
materials of conslruction (e.g.. stainless steel. Teflon,
Viton) may be used, subject to approval of the Ad-
ministrator. The holder design shall provide a positive
seal against leakage Irom the outside or around the filter.
The bolder shall be attached immediately at the outlet
of the probe (or cyclone, if used).
2.1.6 Filter Heating System. Any heating system
capable of maintaining a temperature around the filter
holder during sampling o. 120±14° C (248±2.',° F), or
such other temperature as specified by an applicable
subpart ol the slandards or approved by Ihc Adminis-
tralor for a particular application. Alternatively, the
tester may opl to operate the equipment at a temperature
lower than that specified. A temperature gauge capable
of measuring temperature to within 3° C (5.4° F) shall
be installed so that the temperature around the filler
holder can be regulated and monitored during sampling.
Healing systems other than the one shown in APTD-
0581 may be used.
2.1.7 Condenser. The following system shall be used
to determine Ihe stack gas moisture content: Four
impingers connected in series with leak-free ground
glass fillings or any similar leak-free non-contaminating
fillings. The first, third, and fourth impingers shall be
ol Ihe Greenburg-fimith design, modified by replacing
the Up with 1.3 cm (H in.) ID glass lube extending to
about 1.3 cm M in.) from the bottom of Ihe flask. The
second impinger shall be of the Oreenburg-Smlth design
with Ihe standard tip. ModiQcalions (e.g., using flexible
eonnections between the Impingers, using materials
other than glass, or using flexible vacuum lines to connect
the filter holder to the condenser) may be used, subject
to the approval of the Administrator. The first and
second Impingers shall contain known quantities of
water (Section 4.1.3), the third shall be empty, and Ihe
fourth shall contain a known weight of silica gel, or
equivalent deaiccant. A thermometer, capable of measur-
car
TEMPERATURE SENSOR
- PROBE
TEMPERATURE
SENSOR
IMPINGER TRAIN OPTIONAL, MAY BE REPLACED
BY AN EQUIVALENT CONDENSER
HEATED AREA THERMOMETER
THERMOMETER
PITOTTUBE
PROBE
REVERSE-TYPE
PITOT TUBE
IMPINGERS ICE BATH
BY-PASS VALVE
PITOT MANOMETER
ORIFICE
CHECK
VALVE
VACUUM
LINE
VACUUM
GAUGE
THERMOMETERS
MAIN VALVE
DRY GAS METER
AIR-TIG.HT
PUMP
figure 5 1. Paniculate-sampling train.
Ill-Appendix A-21
-------
Ing temperature to within 1° C (2° F) shall be placed
at the outlet of the fourth tmplnger for monitoring
purposes.
Alternatively, any system that cools the sample gas
stream and allows measurement of the water condensed
and moisture leaving the condenser, each to within
1 ml or 1 g may be used, subject to the approval of the
Administrator. Acceptable means are to measure the
condensed water either gravimetrically or volumetrically
and to measure the moisture leaving the condenser by:
(1) monitoring the temperature and pressure at the
exit of the condenser and using Dalton s law of partial
pressures; or (2) passing the sample gas stream through
a tared silica gel (or equivalent desiccant) trap with
exit gases kept below 20° C (68° F) and determining
the weight gain.
If means other than silica gel are used to determine
the amount of moisture leaving the condenser, it is
recommended that silica gel (or equivalent) still be
used between the condenser system and pump to prevent
moisture condensation in the pump and metering devices
and to avoid the need to make corrections for moisture in
the metercd volume.
NOTE.—If a determination of the paniculate matter
collected In the impingers is desired in addition to mois-
ture content, the impinger system described above shall
be used, without modification. Individual States or
control agencies requiring this information shall be
contacted as to the sample recovery and analysis of the
Impinger contents.
2.1.8 Metering System. Vacuum gauge, teak-free
pump, thermometers capable of measuring temperature
to within 3° C (5.4° F), dry gas meter capable of measuring
volume to within 2 percent, and related equipment, as
shown in Figure 5-1. Other metering systems capable of
maintaining sampling rales within 10 percent of iso-
kinetic and of determining sample volumes to within 2
percent may. be used, subject to the approval o! the
Administrator. When the metering system is used in
conjunction with a pilot tube, the system shall enable
checks oi isokinctic rates.
Sampling trainsutilizingmeteringsystems designed for
higher flow rates than that described in APTD-0581 or
APTD-057C may be used provided that the specifica-
tions 01 this method are met.
2.1.0 Barometer. Mercury, aneroid, or other barometer
capable of measuring atmospheric pressure to within
2.5 mm Hg (0.1 in. Ilg). In many eases, the barometric
reading may be obtained from a nearby national weather
Mrvice station, in which case the station value (which is
the absolute barometric pressure) shall be requested and
an adjustment for elevation differences between the
weather station and sampling point shall be applied at a
rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m (100 ft)
elevation increase or vice versa for elevation decrease.
21.10 Gas Density Determination Equipment.
Temperature sensor and pressure gauge, as described
in Sections 2.3 and 2.4 of Method 2, and gas analyzer,
if necessary, as described in Method 3. The temperature
wnsor shall, preferably, be permanently attached to
the pitot tube or sampling probe in a filed configuration,
such that the tip of the sensor extends beyond the leading
edge of the probe sheath and does not touch any metal.
Alternatively, the sensor may be attached Just prior
to use in the field. Note, however, that if the temperature
sensor is attached in the field, the sensor must be placed
in an interference-free arrangement with respect to the
Type S pitot tube openings (see Method 2, Figure 2-7).
Asa second alternative, if a difference of not more than
1 percent in the average velocity measurement is to be
introduced, the temperature gauge need not be attached
to the probe or pitot tube. (This alternative is subject
to the approval of the Administrator.)
2.2 Sample Recovery. The following items are
221 Probe-Liner and Probe-Nozzle Brushes. Nylon
bristle brushes with stainless steel wire handles. The
probe brush shall have extensions (at least as long as
the probe) of stainless steel, Nylon, Teflon, or similarly
inert material. The brushes shall be properly sized and
shaped to brush out the probe liner and nozzle.
2.2.2 Wash Bottles—Two. Glass wash bottles are
recommended; polyethylene wash bottles may be used
at the option of the tester. It is recommended that acetone
not be stored in polyethylene bottles for longer than a
month.
2.2.3 Glass Sample Storage Containers. Chemically
resistant, borosilicate glass bottles, for acetone washes,
600 ml or 1000 ml. Screw cap liners shall either be rubber-
backed Teflon or shall be constructed so as to be leak-free
and resistant to chemical attack by acetone. (Narrow
mouth glass bottles have been found to be less prone to
leakage.) Alternatively, polyethylene bottles may be
used.
2.2.4 Fetri Dishes. For filter samples, glass or poly-
ethylene,.imless otherwise specified by the Admin-
istrator. °/
2.2.5 Graduated Cylinder and/or Balance. To meas-
ure condensed water to within 1 ml or 1 g. Graduated
cylinders shall have subdivisions no greater than 2 ml.
Most laboratory balances are capable of weighing to the
nearest 0.5 g or less. Any of these balances is suitable for
use here and in Section 2.3.4.
2.2.6 Plastic Storage Containers. Air-tight containers
to store silica gel.
2.2.7 Funnel and Rubber Policeman. To aid In
transfer of silica gel to container: not necessary if silica
gel is weighed in the field.
2.2.8 Funnel. Glass or polyethlene, to aid in sample
2.3 Analysis. For analysis, the following equipment Is
needed.
2.8.1 Glass Weighing Dishes.
2.8.2 Desiccator.
2.3.3 Analytical Balance..To measure to within 0.1
mg.
2.3.4 Balance. To measure to within 0.5 g.
2.8.5 Beakers. 250 ml.
2.3.6 Hygrometer. To measure the relative humidity
of the laboratory environment.
2.3.7 Temperature Gauge. To measure the tempera-
tore of the laboratory environment.
8. Reafenti
8.1 Sampling. The reagents used in sampling ale as
follows:
1.1.1 Filters. .Glass fiber filters, without organic
binder, exhibiting at least 99.95 percent efficiency (<0.05
percent penetration) on 0.3-micron dioctyl phthalate
smoke particles. The filter efficiency test Shan be con-
ducted in accordance with A8TM standard method D
2986-71. Test data from the supplier's quality control
program are sufficient for this purpose.
In sources containing SO, or SO., the filter
material must be of a type that is unreactive
to SO, or SO,. Citation 10 in Section 7 may be
used to select the appropriate filter."8
8.1.2. Silica Gel. Indicating type, 6 to 18 mesh. If
previously used, dry at 175° C (350° F) for 2 hours. New
silica gel may be used as received. Alternatively, other
types of desiccants (equivalent or better) may be used,
subject to the approval of the Administrator.
3.1.3 Water. When analysis of the material caught in
the impingers is required, distilled water shall be used.
Run blanks prior to field use to eliminate a high blank
on test samples.
3.1.4 Crushed Ice.
8.1.5 Stopcock Grease. Acetone-insoluble, heat-stable
silicone grease. This is not necessary If screw-on con-
nectors with Teflon sleeves, or similar, are used. Alterna-
tively, other types of stopcock grease may be used, sub-
ject to the approval of the Administrator.
3.2 Sample Recovery. Acetone—reagent grade, <0.001
percent residue, In glass bottles—is required. Acetone
from metal containers generally has a high residue blank
and should not be nsed. Sometimes, suppliers transfer
aceUme to glass bottles from metal containers; thus,
acetone blanks shall be run prior to field use and only
acetone with low blank values (<0.001 percent) shall be
used. In no ease shall a blank Tame of greater than O.'Ol
percent of the weight of acetone used be subtracted fr im
the nmplt weight.
S.3 Analysis. Two reagents are required for the anajy-
iis:
8.8.1 Acetone. Same as 3.2.
8.8.3 Desiccant. Anhydrous calcium sulfate, Indicat-
ing type. Alternatively, other types of desiccants may be
nsed, subject to the approval of the Administrator.
4. Procedure
4.1 Sampling. The complexity of this method is such
that, in order to obtain reliable results", testers should he
trainivi mid experienced with the test procedures.
4.1.1 Pretest Preparation. All the components snail
be maintained and calibrated according to the procedure
described in APTD-0576, unless otherwise specified
herein.
Weigh several 200 to 300 g portions of silica gel in air-tight
containers to the nearest 0.5 g. Record the total weight of
the silica gel plus container, on each container. As an
alternative, the silica gel need not be preweighed, but
may be weighed directly in its impinger or sampling
holder lust prior to train assembly.
Check filters visually against light for irregularities and
flaws or pinholc leaks. Label filters of the proper diameter
on the back side near the edge using numbering machine
ink. As an alternative, label the shipping containers
(glass or plastic petri dishes) and keep the filters in these
containers at all times except during sampling and
weighing.
Desiccate the filters at 20±5.6° C (68±10° F) and
ambient pressure for at least 24 hours and weigh at in-
tervals of at least 6 hours to a constant weight, i.e.,
<0.5 mg change from previous weighing; record results
to the nearest 0.1 mg. During each weighing the filter
must not be exposed to the laboratory atmosphere for a
period greater than 2 minutes and a relative humidity
above 50 percent. Alternatively (unless otherwise speci-
fied by the Administrator), the filters may be oven
dried at 105° C (220° F) for 2 to 3 hours, desiccated for 2
hours, and weighed. Procedures other than those de-
scribed, which account for relative humidity effects, may
be used, subject to the approval of the Administrator.
4.1.2 Preliminary- Determinations. Select the sam-
pling site and the minimum number of sampling points
according to Method 1 or as specified by the Administra-
tor. Determine the stack pressure, temperature, and the
range of velocity heads using Method 2; It is recommended
that a leak-check of the pitot lines (see Method 2, Sec-
tion 3.1) be performed. Determine the moisture content
using Approximation Method 4 or its alternatives for
the purpose of making isotinetic sampling rate settings.
Determine the stack gas dry molecular weight, as des-
cribed in Method 2, Section 3.6; if integrated Method 3
sampling is used for molecular weight determination, the
integrated bag sample shall be taken simultaneously
with, and for the same total length of time as, the par-
ticulatc sample run.
Select a nozzle size based on the range of velocity heads,
such that it is not necessary to change the nozzle size in
order to maintain isokinetic sampling rates. During the
run, do not change the nozzle size. Ensure that the
proper differential pressure gauge is chosen for the range
of velocity heads encountered (see Section 2.2 of Method
2).
Select a suitable probe liner and probe length such that
all traverse points can be sampled. For large stacks,
consider sampling from opposite sides, of the stack to
reduce the length of probes.
Select a total sampling tune greater than or equal to
the minimum total sampling time specified in the test
procedures for the specific industry such that (1) the
sampling time per point is not less than 2 min (or some
greater time interval as specified by the Administrator),
and (2) the sample volume taken (corrected to standard
conditions) will exceed the required minimum total gas
sample volume. The latter is based on an approximate
average sampling rate.
It is recommended that the number of minutes sam-
pled at each point be an integer or an integer plus one-
half minute, in order to avoid timricmplnp errors.jhie
iwiDlinirtimpe.t
-------
Doing a tweeser or dean disposable surgical stoves,
piece o labeled (identified) and weighed niter in the
filter holder. Pe oure that the filter is properly centered
end the gasket properly placed eo os to prevent the
cample gas stream from circumventing the filter. Chacfc
the filter for tears after assembly is completed.
When glass liners ore used, install the selected noaals
uainv a viton A O-rins ubsn stack temperatures ere
kas than 280° C (Ktf F) and on csbastos string gostiet
oban tsmpcraturea ere higher. Baa APTD-C376 Cor
details. Other connecting systems using either 31C stain
tess steel or Teflon ferrules may be used. When metal
liners are used, Install the nozzle as above or by a leak-
free direct mechanical connection. Mark the probe with
fae&t resistant tape or by some other method to denote
the proper distance into the stack or duct for each sam-
pling point.
Bet up the train as in Figure 5-1, using (if necessary)
a very light" coat of silicone grease on all ground glass
Joints, greasing only the outer portion (see APTD-C570)
to avoid possibility of contamination by the silicone
grease. Subject to the approval of the Administrator, a
glass cyclone may be used between the probe and filter
holder when the total paiticulate catch is expected 10
exceed 100 mg or when water droplets are present in the
stack gas.
Place crushed ice around the impingers.
4.1.4 Leak-Check Procedures.
4.1.4.1 Pretest Leak-Check. A pretest leak-oluvk is
recommended, but not required. If the tester opts to
conduct the pretest leak-check, the following procedure
shall be used. ,,
After the sampling train has been assembled, turn on
and set the filter and probe heating systems at the desired
operating temperatures. Allow time for the temperatures
to stabilize. If a Viton A O-ring or other leak-free connec-
tion is used in assembling the probe nozzle to the probe
liner, leak-check the train at the sampling site by plug-
ging the nozzle and pulling a 380 mm Hg (15 in. Hg)
vacuum.
NOTE.—A lower vacuum may be used, provided that
it is not exceeded during the test.
If an asbestos string is used, do not connect the probe
to the train during the leak-check. Instead, leak-check
the train by first plugging the inlet to the filter holder
(cyclone, if applicable) and pulling a 380 mm Ug (15 in.
Hg) vacuum (see Note immediately above). Then con-
nect the probe to the train and leak-check at about 2i
mm Hg (1 in. Hg) vacuum; alternatively, the probe may
be leak-checked with the rest of the sampling train, in
one step, at 380 mm Hg (15 in. Hg) vacuum. Leakage
rates in excess of 4 percent of the average sampling rate
or 0.00057 m>/min (0.02 cfm), whichever is less, are
unacceptable.
The following leak-check instructions for the sampling
train described in APTD-0576 and APTD-OS81 may be
helpful. Start the pump with bypass valve fully open
and coarse adjust valve completely closed. Partially
open the coarse adjust valve and slowly close the bypass
valve until the desired vacuum is reached. Do not reverse
direction of bypass valve; this will cause water to back
up into the filter holder. If the desired vacuum is ex-
ceeded, either leak-check at this higher vacuum or end
the leak check as shown below and start over.
When the leak-check is completed, first slowly remove
the plug from the inlet to the probe, filler holder, or
cyclone (if applicable) and immediately turn off the
vaccum pump. This prevents the water in the impingers
from being forced backward into the filter holder and
silica gel from being entrained backward into the third
impingcr.
4.1.4.2 Leak-Checks During Sample Run. If, during
the sampling run, a component (e.g., filter assembly
or impiuger) change becomes necessary, a leak-check
shall be conducted immediately before the change is
made. The leak-check shall be done according to the
. procedure outlined in Section 4.1.4.1 above, except that
it shall be done at a vacuum equal to or greater than the
maximum value recorded up to that point in the test.
. If the leakage rate is found to be no greater than 0.00057
m'/min (0.02 cfm) or 4 percent of the average sampling
rate (whichever is less), the results are acceptable, and
no correction will need to be applied to the total volume
of dry gas metered; if, however, a higher leakage rate
is obtained, the tester shall either record the leakage
rate and plan to correct the sample volume as shown in
Section 6.3 of this method, or shall void the sampling
run.87
Immediately after component changes, leak-checks
are optional; if such leak-checks are done, the procedure
outlined in Section 4.1.4.1 above shall be used.
4.1.4.3 Post-test Leak-Check. A leak-check is manda-
tory at the conclusion of each sampling run. The leak-
check shall be done in accordance with the procedures
outlined in Section 4.1.4.1, except that it shall be con-
ducted at a vacuum equal to or greater than the maxi-
mum value reached during the sampling run. If the
leakage rate is found to be no greater than 0.00057 m'/rnin
(0.02 cfm) or 4 percent of the average sampling rate
(whichever is less), the results are acceptable, and no
correction need be applied to the total volume of dry gas
metered. If, however, a higher leakage rate is obtained,
the tester shall either record the leakage rate and correct
the sample volume as shown in Section 6.3 of iliis method,
or shall void the sampling run.
4.1.5 Particular Train Operation. During the
sampling run, maintain on isokinetic sampling rate
(v/itliin 10 percent of true isokinetic unless otherwise
specified by the Administrator) and a temperature
around Mie filter of 120±14° C (24S±25° F), or such other
temperature as specified by an applicable subpart of the
standards or approved by the Administrator.
For each run, record the data required on a data sheet
ouch as the one shown in Figure 6-2. Be sure to record the
initial dry gas meter reading. Record the dry gas meter
readings at the beginning and end of each sampling tints
Increment, when changes in flow rates are made, refers
cad after each leak check, and wheu sampling is baited.
PLANT
LOCATION.
OPERATOR,.
BATE
RUN NO
SAMPLE. BOX MO..
METER BOX f!0._
METER &H@.
6 FACTOR
AMBIENT TEMPERATURE.
BAROMETRIC PRESSURE _
ASSUMED MOISTURE, %_
PROBE LENGTH, tn (ft)
PITOT TUBE COEFFICIENT, Cp.
SCHEMATIC OF STACK CROSS SECTION
NOZZLE IDENTIFICATION WO
AVERAGE CALIBRATED NOZZLE DIAMETER. era(in.)_
PROBE HEATER SETTING
IEAK RATE,ra3/min.(cfm)
PROBE LINER MATERIAL
STATIC PRESSURE, mm Hg (in. HtL
FILTER WO
TRAVERSE POINT
.NUMBER
TOTAL
SAMPLING
TIME
($1. min.
AVERAGE
VACUUM
mm Hg
{In. Hg)
STACK
TEMPERATURE
1TS)
«C («F)
VELOCITY
HEAD
I&PS).
nimfln.JHzO
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METER
mrnHjO
(in. H20)
GAS SAMPLE
VOLUME
ffl3 (ft3!
GAS SAMPLE TEMPERATURE
AT DRY GAS METER
INLET.
°C (°F)
Avg.
OUTLET
°C (8FI
Avg.
Avg. .
FILTER HOLDER
TEMPERATURE.
°C (°FI
TEMPERATURE
' OF GAS '
LEAVING
CONDENSER Oil
LAST IMPINGER.
8C(»F)
Figure 5-2. Participate field data.
III-Appendix A-23
-------
'ake other readings required by Figure 5-2 at least once
t eacb sample point during eacb time increment and
iditipna) readings when significant changes (20 percent
ariation in velocity bead readings) necessitate addi-
onal adjustments in flow rate. Level and tero tbe
lanometer. Because the manometer level and zero may
rift due to vibrations and temperature changes, make
eriodic checks during tbe traverse.
Clean tbe portholes prior to the test ran to minimize
be chance of sampling deposited material. To begin
smpling, remove the nozzle cap, verify that the filter
nd probe beating systems are up to temperature, and
bat the pilot tube and probe are properly positioned.
'osltlon the nozzle at the first traverse point with the tip
olntlng directly into the gas stream. Immediately start
be pump and adjust the flow to isokinetic conditions.
tomographs are available, which aid in the rapid adjust-
aent of the isokinetle sampling rote without excessive
ompntatlons. These nomographs are designed for use
rhen tbe Type 8 pilot tube coefficient is O.&5±0.02. and
be stack gas equivalent density (dry molecular weight)
i equal to 29±4. APTD-0576 details tbe procedure for
sing tbe nomographs. If C, and Mi are outside the
Dove stated ranges do not use the nomographs unless
ppropriate steps (see Citation 7 In Section 7) are taken
a compensate for tbe deviations.
When the stack is under significant negative pressure
beigbt of impinger stem), take care to close tbe coarse
djust valve before inserting the probe Into the stack to
revent water from backing into the filter holder. If
ecessary, tbe pump may be turned on with tbe coarse
djust valve closed. •
When the probe is in position, block off tbe openings
round the probe and porthole to prevent unrepre-
sntative dilution of the gas stream.
Traverse the stack cross-section, as required by Method
or as specified by the Administrator, being careful not
5 bump the probe nozzle into the stack walls when
impling near the walls or when removing or inserting
be probe through the portholes; this minimizes tbe
hance of extracting deposited material.
During the test run, make periodic adjustments to
eep the temperature around the filter holder at the
roper level; add more ice and, if necessary, salt to
laintain a temperature of less than 20° C e; hold a sample
container underneath the lowr end of the probe, and
catch any acetone and paniculate matter which is
brushed from the probe. Run the brush through the
probe three times or more until no visible paniculate
matter is carried out with the acetone or until none
remains in the prolie liner on visual insjwction. With
Painless steel or other metal prolx'S, run the brush
through in the above prescribed manner at least six
times since metal probes have small crevices iu which
paniculate matte'- can be entrapped. Rinse the brush
with aoetone. and quantitatively collect these washings
w\ the sample container. After the brushing, make a
final aceloue rinse of the*probe as described above.
It is recommended that two people be used to clean
the probe to minimize saraplelosses. Between sampling
runs, keep brushes clean aud protected from contamina-
tion.
After ensuring that all Joints have been wiped clean
of sih'cone grease, cl«au the inside of the (rout half of the
filter bolder by rubbing the surfaces with a Nylon bristle
brush and rinsing with acetone. Rinse eacb surface
uiree times or more if needed to remove visible panicu-
late. Make • final rinse of the brush and filler bolder.
Carefully rinse out the glass cyclone, also (if applicable).
After all acetone washings and paniculate matter have
been collected in the sample container, tighten the lid
on the sample container to that aoetone will not leak
out when it is shipped to the laboratory. Mark the
height of the fluid level to determine whether or not
leakage occurred during transport. Label the container
to clearly identify its contents.o/
Container No. i. Note the color of the indicating silica
(el to determine if it has been rompMely spent and make
a notation of its condition. Transfer the silica gel from
the fourth impinger to its original container and seal.
A funnel may make it easier to pour the silicagel without
spilling. A rubber policeman B>ay be used as an aid in
removing the silica gel from the impinger. It ts not
necessary to remove the small amount of dust particles
that may adhere to the impinger wall and are difficult
t* mrtere. Since the gain in weight is to be used for
xaoisture calculations, do not use any water or other
liqnids to transfer the silica grt.'If a balance in available
ii tbe field, follow the procedure for container'No. 3
in flection 4.8.
Impinaer Hater. Treat the impingers as follows: Make
•notation of any color or film in the liquid catch. Measure
tbe liquid which is in tbe first three impingers to within
-1 ml by using a graduated cylinder or by weighing it
to within *0.5 g by using a balance (if one is available).
Record the volume or weight of liquid present. This
information is required to calculate the moisture content
of UK effluent gas.
Discard the liquid after measiiring and recording the
volume or weight, unless analysis of the impiuger catch
it required (see Not*, Section 2.1.7).
H a different type of condenser is used, measure the
•mount of moisture condensed either volumetric-ally or
(ravimetrically.
Whenever possible, containers should be shipped in
web a way that they remain upright at all times.
4.3 Analysis. Record the data required on a sheet
such as the one shown in Figure 6-3. Uaudle eacb sample
container as follows:
Container No. 1. Leave the contents in the shipping
container or transfer the tiller and any loose paniculate
from the sample container to a tared glass weighing dish.
Desiccate for 24 hours in a desiccator containing anhy-
drous calcium sulfate. Weigh to a constant weight and
report the results to the nearest 0.1 mg. For purposes of
ihit Section, 4.3, the term "constant weight" means a
difference of no more than 0.5 nig or 1 percent of total
weight less tare weight, whichever Is greater, between
two ronaecutivt weighings, with no less than i hours of
desiccation time between weighings.
Alternatively, the sample may be oven dried at 105" C
(220° F) for 2 to 3 hours, cooled in the desiccator, and
weighed to a constant weight, unless otherwise specified
by the Administrator. The tester may also opt to oven
dry the sample at 105 ° C (220 ° F) for 2 to 3 hours, weigh
tbe sample, and use this weight as a final weight.
Container No. t. Note the level of liquid in the container
and confirm on the analysis sheet whether or not leakage
occurred during transport. If a noticeable amount of
leakage has occurred, either void the sample or use
methods, subject to the approval of the Administrator,
to correct the final results. Measure the liquid in this
container either volumetrically to ±1 ml or gravi-
melrically to ±0.5 g. Transfer the contents to a tared
250-ml beaker and evaporate to dryness at ambient
temperature and pressure. Desiccate for 24 hours and
weigh to a constant weight. Report the results to the
nearest 0.1 mg.
Container No. S. Weigh the spent silica gel (or silica gel
plus impinger) to the nearest 0.5 g using a balance. This
step may be conducted in the field.
Acetone Blank" Container. Measure acetone In this
container either volumetrically or gravimetrically.
Transfer the acetone to a tared 250-ml beaker and evap-
orate to dryness at ambient temperature and pressure.
Desiccate for 24 hours and weigh to a contsant weight.
Report the results to the nearest 0.1 mg.
NOTE.—At the option of the tester, the contents of
Container No. 2 as well as the acetone blank container
may be evaporated at temperatures higher than ambi-
ent. If evaporation is done at an elevated temperature,
the temperature must be below the boiling point of the
solvent; also, to prevent "bumping," the evaporation
process must be closely supervised, and the contents of
the beaker must be swirled occasionally to maintain an
even temperature. Use extreme care, as acetone is highly
flammable and has a low flash point.
Ill-Appendix A-24
-------
6. Calibration
Maintain a laboratory log of all calibrations.
5.1 Probe Nozzle. Probe nozzles shall be calibrated
before their initial use in the field. Using a micrometer,
measure the inside diameter of the nozzle to the nearest
0.025 mm (0.001 in.). Make three separate measurements
using different diameters each time, and obtain the aver-
age of the measurements. The diflerence between the high
and low numbers shall not exceed 0.1 mm (0.004 in.).
When nozzles become nicked, dented, or corroded, they
shall be reshaped, sharpened, and recalibrated before
use. Each nozzle shall be permanently and uniquely
identified.
6.2 Pitot Tube. The Type S pltot tube assembly shall
be calibrated according to the procedure outlined in
Section 4 of Method 2.
5.3 Metering System. Before its initial use in the field,
the metering system shall be calibrated according to the
procedure outlined in APTD-OJ70. Instead of physically
adjusting the dry gas meter dial readings to correspond
to the wet test meter readings, calibration factors may be
used to mathematically correct the gas meter dial readings
to the proper values. Before calibrating the metering sys-
tem, it is suggested that a leak-check be conducted.
For metering systems having diaphragm pumps, the
normal leak-check procedure will not detect leakages
within the pump. For these cases the following leak-
check procedure is suggested: make a 10-minute calibra-
tion run at 0.00057 m Vrnin (0.02 c£m); at the end of the
run, take the difference of the measured wet test meter
and dry gas meter volumes; divide the difference by 10,
to get the leak rate. The leak rate should not exceed
0.00057 m '/min (0.02 cfm).
After each field use, the calibration of the metering
system shall be checked by performing three calibration
runs at a single, intermediate orifice setting (based on
the previous field test), with the vacuum set at the
maximum value reached during the test series. To
adjust the vacuum, insert a valve between the wet test
meter and the inlet of the metering system. Calculate
the average value of the calibration factor. If the calibra-
tion has changed by more than 5 percent, recalibrate
the meter over the full range of orifice settings, as out-
lined in APTD-0576.
Alternative procedures, e.g., using the orifice meter
coefficients, may be used, subject to the approval of the
Administrator.
NOTE.—If the dry gas meter coefficient values obtained
before and after a test series differ by more than 5 percent,
the test series shall either be voided, or calculations for
the test series shall be performed using whichever meter
coefficient value (i.e., before or after) gives the lower
value of total sample volume.
6.4 Probe Heater Calibration. The probe beating
system shall be calibrated before its initial use In the
field according to the procedure outlined in APTD-0576.
Probes constructed according to APTD-0581 need not
be calibrated if the calibration curves in APTD-0576
are used.
6,5 Temperature Gauges. Use the procedure in
Section 4.3 of Method 2 to calibrate in-stack temperature
gauges. Dial thermometers, such as are used for the dry
gas meter and condenser outlet, shall be calibrated
against merciiry-in-glass thermometers.
5.6 Leak Check of Metering System Shown In Figure
5-1. That portion of the sampling train from the pump-
to tbe orifice meter should be leak checked prior to Initial
use and after each shipment. Leakage after the pump will
result in less volume being recorded than Is actually
sampled. The following procedure is suggested (see
Figure 5-4): Close the main valve on the meter box.
Insert a one-hole rubber stopper with robber tubing
attached Into the orifice exhaust pipe. Disconnect and
vent the low side of the orifice manometer. Close off the
low side orifice tap. Pressurize the system to 13 to 18 cm
(6 to 7 in.) water column by blowing Into the rubber
tubing. Pinch off the tubing and observe the manometer
for one minute. A loss of pressure on the manometer
Indicates a leak in the meter box; leaks, if present, must
be corrected.
5.7 Barometer. Calibrate against a mercury barom-
eter.
6. Calculations
Carry out calculations, retaining at least one extra
decimal figure beyond that of the acquired data. Round
oft figures after the final calculation. Other forms of the
equations may be used as long as they give equivalent
results.
Plant.
Date.
Run No..
Filter No..
Amount liquid lost during transport
Acetone blank volume, ml
Acetone wash volume, ml
Acetone blank concentration, mg/mg (equation 5-4).
Acetone wash blank, mg (equation 5-5}
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED,
mg
FINAL WEIGHT
^xC!^
TARE WEIGHT
]]^X^
Less acetone blank
Weight of paniculate matter
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME,
ml.
SILICA GEL
WEIGHT,
g
8*1 ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER (10/m!).
INCREASE, g . V£)LUME WAT£R m|
1 g/ml
Figure 5-3. Analytical data.
Ill-Appendix A-25
-------
RUBBER
TUBING
RUBBER
STOPPER
ORIFICE
BY-PASS VALVE
VACUUM
GAUGE
BLOW INTO TUBING
UNTIL MANOMETER
READS 5 TO 7 INCHES
WATER COLUMN
ORIFICE
MANOMETER
Figure 5-4. Leak check of meter box.
6. 1 Nomenclature
A,
£„
C,
c,
L,
M,
P,
P,n
T.
T.,t
V,
V, „
= Cross-sectional area of nozzle, m> (It').
—Water vapor in the gas stream, proportion
by volume. R7
—Acetone blank residue concentration, mg/g.
= Concentration of paniculate matter in stack
ga>, dry basis, corrected to standard condi-
tions, g/dscm (g/dscf).
« Percent of isokinetic sampling.
—Maximum acceptable leakage rate for either a
Stest leak check or for a leak check follow-
a component change; equal to 0.00057
min (0.02 cfm) or 4 [percent of the average
sampling rate, whichever is less.
= Individual leakage rate observed during the
leak check conducted prior u> the ''{*>>"
component change (1=1, 2, 3 .... it),
m>/min (cfm).
—Leakage rate observed during the post-test
leak check, m'/min (cfm).
— Total amount of paniculate matter collected,
Tag.
—Molecular weight of water, 18.0 g/g-mole
(18.01b/lb-mole).
—Mass of residue of acetone after evaporation,
mg.
—Barometric pressure at the sampling sit*,
mm Hg (in. fig).
- Absolutestack gas pressure, mm Hg (in. Hg).
-Standard absolute pressure, 760 mm Hg
(2».92 in. Hg).
—Ideal gas constant, 0.06236 mm Hg-m'/°K-g-
mole (21.85 in. Hg-ft»/°R-lb-mole).
» Absolute average dry gas meter temperature
(see Figure 5-2), °K (°R).
<= Absolute average stack gas temperature (see
Figure 5-2), °K (°R).
= Standard absolute temperature, 293° K
(528° R).
= Volume of acetone blank, ml.
—Volume of acetone used in wash, ml.
Vi.=Total volume of liquid collected in impingers
and silica gel (see Figure 5-3), ml.
V.=Volume of gas sample »s iicasuroc. by dry gas
meter, dcm (dcf).
. n)=Volume of gas sample measureo t/y the my
gas meter, corrected to standard condition-:.
dscm (dscf)°.
V.(.n>=Volume of water vapor In the gas sample.
corrected to standard condition:, scm (set).
V. - Stack gas velocity, calculated by Method 2,
Equatio
,
tion 2-0, using data obtained from
Method 5, m/sec (ftfcec). 87
W.= Weight of residue in acetone wash, mg.
V=Dry gas meter calibration factor.
AH= Average pressure differential across the orifice
meter (see Figure 5-2), mm HiO (In. HiO).
P. = Density of acetone, mg/ml (see label on
bottle),
».- Density of water, 0.9982 I/ml (0.002201
Ib/ml).
•=Total sampling time, min.
0; = Sampling time interval, from the beginning
of a run until the first component- change,
min.
0i=8ampling time interval, between two suc-
cessive component changes, beginning with
the interval between the first and second
changes, min.
«,=8ampling time interval, from the final (n't)
component change until the end of the
sampling run, min.
13.6=Specific gravity of mercury.
60=Sec/min.
100= Conversion to percent.
6.2 Average dry gas meter temperature and average
orifice pressure drop. See data sheet (Figure 5-2).
(.3 Dry Gas Volume. Correct the sample volume
measured by the dry gas meter to standard conditions
(20° C, 760 mm Hg or 68° F, 29.92 in. Bg) by using
Equation 5-1.
v.c
yp..A |Pb"+13.61
mY\^)\ P.« I
Equation 6-1
where: 0-j
K,-O.S8S8*K/mmHg for metric unite B/
1 -17 .M 'a/in. Hg for English units
NOTS.— Equation 6-1 oan b« and as written
the leakage rate observed during any of the mandatory
le»k checks (I.e., the post-test leak check or leak ebeeta
conducted prior to component changes) exceeds L.. If
It. or IH exceeds £•, Equation 6-1 must be modified at
tollows;
(a) Caw I. No component changes made daring
•ampling run. In this case, replace 1'. in Equation 5-1
with the expression;
(b) Case II. One or more component changes made
during the sampling run. In this case, replace Vm in
Equation 5-1 by the expression:
T
n
-§
I* only to
•.4 Volunw of water vapor.
and mbstitnU only lor those leakage rateg (£,• or L,)
wbicii cxoeed L..
Equation 5-2
where:
#•1=0.001333 m'/ml for metric unite
«O.M707 ft'/ml lor English units.
e.5 Moisture Content.
B,.-.
• <•«> + V* (nd)
Equation 1-3
Ill-Appendix A-26
-------
Non.—In •tunted or water droplet-laden |u
(trams, two calculations of tbe moisture content of tbt
•tack gas shall be made, one from tbe impinger analysis
(Equation 5-3), and a second from tbe assumption of
•aturated conditions. Tbe lover of tbe two values of
£„ shall be considered correct. Tbe procedure fer deter-
mining tbe moisture content baaed upon assumption of
saturated conditions is given in the Note of Section 1.2
of Method 4. For tbe purposes of this method, tbe average
•tack gas temperature from Figure 6-2 ma; be used to
make this determination, provided that the accuracy of
the in-etack temperature sensor is ± 1° C (2* F).
6.6 Acetone Blank Concentration.
Equation 5-4
6.7 Acetone Wash Blank.
Equation 6-5
6.8 Total Paniculate Weight. Determine tbe total
paniculate catch from tbe sum of tbe weights obtained
from containers 1 and 2 less tbe acetone blank (see Figure
W). Noil.—Refer to Section 4.1.6 to assist in calculation
of results Involving two or more, filter assemblies or two
or more sampling trains.
6.9 Paniculate Concentration.
«.= (0.001 g/mg) (m,/r..<.„),)
Equation 5-4T
6.10 Conversion Factors:
From To Multiply by
«/
gft'
g/ft'
g/fl'
m»
gr/fi1
lb/ft«
t/m«
0.02832
15.43
2. 206X10-'
35.31
6.11 Isokinetic Variation.
C.ll.l Calculation From.P>'- Data.
,=
600i>. P.An
87
n >>7
vbere:
Xt-O.OOMM mm Hg-mVml-°K for.metric units.
-0.002869 in. Hg-ft'/ml-'R for English units.
6.11.2 Calculation From Intermediate Values.
7
= A- J[.v,.!...!L
Equation 5-8
where:
#4-4.320 for metric units
"0.09450 for English units.
6.12 Acceptable Results. If 90 percent < 7 . Philadelphia P«.
4. Smith, W. 8.. R. T. Shigehara, and W. F. Todd. ,9T4 pyp 6,7^22.
A Method of Interpreting Stack Sampling Data. Paper ,n Coliv I r r I rlinarH r P I xrev
Presented at the 63d Annual Meeting of tbe Air Pollu- 10. Felix, L. U., O. I. Umard. U. b. Ldcey.
tion Control Association, St. Louis, Mo. June 14-19, anci j. Q. McCain. Inertial Cascade Impactor
'Tsrr.ith. W. 8.. et al. Stack Gas Sampling Improved ' Substrate Media for Flue Gas Sampling. U.S.
an
-------
METHOD 6—DETERMINATION or Si'Lrrn DIOXIDE
EMISSIONS FROM BTATIO.NARY Sovmts
1. Principlt and Applicability
1.1 Principle. A gas sample is -extracted from the
sampling point in tbe stack. Tbe sulfuric acid mist
(including sulfur trioxide) and tbe sulfur dioiide are
separated. Tbe sulfur dioxide fraction is measured by
tbe barium-tborin titration metbod.
1.2 Applicability. This metbod is applicable for the
determination of sulfur dioxide emissions from stationary
sources. The minimum detectable limit of t be metbod
has been determined to be 3.4 milligrams dug) of 6Oi'm>
(2.12X10-' Ib/fl'). Although no upper limit has been
established, tests have shown that concentrations as
2.1.10 Volume Meter. Dry gas meter, sufficiently
accurate to measure the sample volume within 2 percent,
calibrated at the selected flow rate and conditions
actually encountered during sampling, and equipped
with a temperature gauge (dial thermometer, or equiv-
alent) capable of measuring temperature to within
VC (S.4T ).
2.1.11 Barometer. Mercury, aneroid, or other barom-
eter capable of measuring atmospheric pressure to within
2.5 mm Hg (0.1 In. Eg). In many cases, the barometric
reading may be obtained from a nearby national weather
•errice station, In which case the station value (which
la the absolute barometric pressure) shall be requested
and an adjustment for elevation differences between
the weather station and sampling point shall be applied
piaousn™ lesu; nave snown tnat concentrations as atarateofminus2.5mm"Hg^6'.nm Hg) per 30"m"(ji66'ft)07
high as 80,000 mg/m> of SOj can be collected efficiently elevation Increase or vice versa for elevation decrease.87
in two midget impingcrs, each containing 15 ruuliliters 2.1.1! Vacuum n«ncp and rntun*t»r At !.««» T«I
of 3 percent hydrogen peroiide, at a rate ol 1.0 Ipm for
20 minutes. Based on theoretical calculations, the upper
concentration limit in a 20-liter sample is about 93,300
mg/rn3.
Possible interferents are free ammonia, water-soluble
cations, and fluorides. Tbe cations and fluorides are
removed by glass wool filters and an isopropanol bubbler,
and hence do not affect the SOj analysis. When samples
are being taken from a gas stream with high concentra-
tions of very line metallic fumes (snch as in inlets to
control devices), a hiph-elnciency glass fiber filler must
be used in place of the glass wool plug (i.e., the one in
the probe) to remove the cation interferenlf.
Free ammonia interferes by reacting with SOj to form
paniculate sulfite and by reacting with the indicator.
If free ammonia is present (this can be determined by
knowledge of the process and noticing white particulate
matter in the probe and isopropanol bubblerX alterna-
tive methods, subject to the approval of the Administra-
tor, U.S. Environmental Protection Agency, AT*
required.
2. Apparatus
2.1 Sampling. The sampling train ia ehown in Figure
6-1, and component parts are discussed below. The
tester has the option of substituting sampling equip-
ment described in Method 8 in place of the midget im-
pinger equipment of Metbod 6. However, tbe Method 8
train must be modified to include a heated filter between
tbe probe and isopropanol Impinger, and tbe operation
of the sampling train and sample analysis must be at
tbe flow rates and solution volumes defined in Metbod 8.
The tester also has the option of determining SO,
simultaneously with particulate matter and moisture
determinations by (1) replacing the water in a Metbod 5
Impinger system with 3 percent peroxide solution, or
(2) by replacing the Method 5 water impinger system
with a Metbod 8 isopropanol-fllter-peroxlde system. Tbe
analysis for SOi must be consistent with the procedure
In Method 8 87
2.1.1 Prooe. Borosllicate glass, or stainless steel (other
materials of construction may be used, subject to the
approval of the Administrator), approximately 6-mm
Inside diameter, with a heating system to prevent water
condensation and a filter (either in-slack or heated out-
stack) to remove particulate matter, including sulfuric
•eld mist. A plug of glass wool is a satisfactory filter.
2.1.2 Bubbler and Implngen. One midget bubbler,
with medium-coarse glass frit and borosiUcate or quartz
glass wool packed in top (see Figure 6-1) to prevent
sulfuric acid mist carryover, and three 30-ml midget
Impingers. The bubbler and midget implngers must be
connected in series with leak-free glass connectors. Sill-
cone frrease may be used, if necessary, to prevent leakage.
At the option of tbe tester, a midget impinger may be
tued in place of the midget bubbler.
Other collection absorbers and flow rates may be used,
but are subject to tbe approval of the Administrator.
Also, collection efficiency must be shown to be at least
99 percent for eacb test run and must be documented In
tbe report. If the efficiency is found to be acceptable after
a series of three tests, further documentation is not
required. To conduct the efficiency test, an extra ab-
sorber must be added and analyied separately. Tbls
extra absorber must not contain more than 1 percent of
the total SOi.
S.1.8 Glass Wool. Borosllicate or quartz.
2.1.4 Stopcock Orease. Acetone-insoluble, beat-
stable slucone grease may be used. If necessary.
3.1.5 Temperature Gauge. Dial thermometer, or
equivalent, to measure temperature of gas leaving Im-
pinger train to within 1° C (2s F.)
2.1.6 Drying Tube. Tube packed with 6- to Ifl-mesh
Indicating type silica gel, or equivalent, to dry tbe gas
sample and to protect the meter and pump. If the (Ulca
gel has been used previously, dry at 175° C (350° F) for
2 hours. New silica gel may be used as received. Alterna-
tively, other types of desiccants (equivalent or better)
may be used, subject to approval of the Administrator. 87
2.1.7 Valve. Needle value, to regulate sample gas flow
rate.87
2.1.8 Pump. Leak-free diaphragm pump, or equiv-
alent, to pull gas through the tram, install a small surge
tnk Between th« pump and rate meter to eliminate
the "'-'sation effect of thetiinphragm pump on the rota -
meter. 8/
2.1.9 Rate Meter. Rotameter, or equivalent, capable
of measuring flow rate to within 2 percent of the selected
flow rate of about 1000 cc/min
2.1.12 Vacuum Gauge and rotametar. At least 760
mm Hg (30 ui.Hg) gauge, and 0-40 cc/mln rotameter
to be used lot leak che. k of tbe sampling train. 87
2.2.1 Wash bottles. Polyethylene or Kiass, 500 ml,
two.
2.2.2 Storage Bottles. Polyethylene, 100 ml, to store
Impinger samples (one per sample).
2.3 Analysis.
2.8.1 Pipettes. Volumetric type, 5-ml, 20-ml (one per
sample), and 25-ml sixes.
2.3.2 Volumetric Flasks. 100-ml site (one per sample)
2.3.3 Burettes. 5- and 50-ml sites.
2.8.4 Erlenmeyer Flasks. 250 mi-size (one for each
•ample, blank, and standard).
2.8.6 Dropping Bottle. 125-ml site, to add Indicator.
J.3.6 Graduated Cylinder. 100-ml size.
2.3.7 Spectrophotometer. To measure absorbance at
162 nanometers.
8. Reaamtt
Unless otherwise Indicated, all reagents must conform
to the specifications established by tbe Committee on
Analytical Reagents of the American Chemical Society.
Where such specifications are not available, use the best
available grade.
8.1 Sampling.
8.1.1 WaterTDelonized, distilled to conform to ASTM
specification D1193-74, Type 3. At tbe option of the
analyst, the KMnO< test for oxidizable organic matter
may be omitted when high concentrations of organic
matter are not expected to be present.
8.1.2 Isopropanol, 80 percent. Mix 80 ml of isopropanol
with 20 ml of deionized. distilled water. Check each lot of
Isopropanol for peroxide Impurities as follows: shake 10
ml of Isopropanol with 10 ml of freshly prepared 10
percent potassium Iodide solution. Prepare a blank by
similarly treating 10 ml of distilled water. After 1 minute,
read the absorbance at 362 nanometers on a spectro-
photometer. If absorbance exceeds 0.1, reject alcohol for
use.
Peroxides may be removed from isopropanol by redis-
tilling or by passage through a column of activated
alumina; however, reagent grade Isopropanol with
suitably low peroxide levels may be obtained from com-
mercial sources. Rejection of contaminated lots nay,
therefore, be a more efficient procedure.
8.1.8 Hydrogen Peroxide, 3 Percent. Dilute 30 percent
hydrogen peroxide 1:9 (v/v) with deionized, distilled
water (80 ml Is needed per sample). Prepare fresh daily.
8.1.4 Potassium Iodide Solution, 10 Percent. Dissolve
10.0 grams KI in delonited, distilled water and dilute to
100ml. Prepare when needed.
8.2 Sample Recovery.
8.2.1 Water. Deionized, distilled, as in 3.1.1.
8.2.2 Isopropanol, 80 Percent. Mix 80ml ofisopropano!
with 20 ml of deionized, distilled water.
3.3 Analysis.
8.3.1 Water. Deioniied, distilled, as in 3.1.1.
3.3.2 Isopropanol, 100 percent.
3.3.3 Thorin Indicator. l-(o-arsonophenylaK>)-2-
naphthol-3,6-disulfonic acid, disoditim salt, or equiva-
lent. Dissolve 0.20 g in 100 ml of deionized, distilled
water.
3.3.4 Barium Perchlorate Solution, 0.0100 N. Dis-
solve 1.05 g of barium percblorate trihydrate (Ba(CIOi)i •
3H.O1 in 200 ml distilled water and dilute to 1 liter with
isopropanol Alternatively, 1.22 g ol [BaCli-2HiO| may
be usta instead of tbe perchlorate. Standardize as in
Section 5.5.87
3.3.5 SuUuric Acid Standard, 0.0100 N. Purchase or
standardize to =".0.0002 N against 0.0100 N NaOH which
has previously been standardized against potassium
acid phthalate (primary standard grade).
4. Proeedun.
4.1 Sampling.
4.1.1 Preparation of collection train. Measure 15 ml of
80 percent isopropanol into the midget bubbler and 15
ml of 3 percent hydrogen peroxide into each of the first
two midget impingers. Leave the final midget Impinger
dry. Assemble the train as shown In Figure 6-1. Adjust
probe heater to a temperature sufficient to prevent water
conde isation. Place crushed ice and water around the
impingers.
4.1.2 Leak-check procedure. A leak check prior to the
sampling run is optional: however, a leak check after the
sampling run Is mandatory. The leak-check procedure Is
as follows:
Temporarily attach a suitable (e.g., 0-40
tc/mln) rotameter to the outlet of the dry
gas meter and place a vacuum gauge at or
near tbe probe Inlet Plug the probe inlet,
pull a vacuum of at least 250 mm Hg (10 to.
Hg). and note the flow rate as indicated by
the rotameter. A leakage rate not in excess
of 2 percent of tbe average sampling rate Ja
acceptable.
NOTK Carefully release the probe Inlet
plug before turning off tbe pump.
It is suggested (not mandatory) that tbe
pump be leak-checked separately, either
prior to or after the sampling run. If done
prior to the sampling run. the pump leak-
check shall precede tbe leak check of the
sampling train described Immediately above:
If done after the sampling run, the pump
leak-check shall follow the train leak-check.
To leak check the pump, proceed as follows:
Disconnect the drying tube from the probe-
implnger assembly. Place a vacuum gauge at
tbe inlet to either the drying tube or the
pump, pull a vacuum of 250 rnirt (10 in.) Hg.
plug or pinch off the outlet of the flow
meter and then turn off the pump. The
vacuum should remain stable for at least 30
seconds. 87
Other leak check procedures may be used, subject to
the approval of tbe Administrator, U.S. Environmental
Protection Agency. The procedure used In Method 5 Is
not suitable for diaphragm pumps.
4.1.3 Sample collection. Record the Initial dry gas
meter reading and barometric pressure. To begin sam-
pling, position the tip of the probe at the sampling point,
connect the probe to the bubbler, and start the pump.
Adjust the sample flow to a constant rate of ap-
proximately 1.0 liter.'mln as indicated by the rotameter.
Maintain this constant rate (*10 percent) during the
entire sampling run. Take readings (dry gas meter,
temperatures at dry gas meter and at Impinger outlet
and rate meter) at least every 5 minutes. Add more ice
during the run to keep the temperature of tbe gases
leaving the last Impinger at 20° C (88° F) or less. At the
conclusion of each run, turn oft the pump, remove probe
from the stack, and record the final readings. Conduct a
leak check as in Section 4.1.2. (This leak check is manda-
tory ) If a leak Is found, void the test run. or i><« proced •
nres acceptable to thr Aumlnls'rator to adjust the wunpk
volume for the leakage Drain the '•-• h»th, and purge
t.hfl remaining part of the train by dreeing clean ambient
air through the system for 15 minutev at the sampling
rate. 87
Clean ambient air can be provided by passing air
through a charcoal filter or through an extra midget
impinger with 15 ml of 3 percent HiOi. The tester may
opt to simply use ambient air, without purification.
4.2 Sample Recovery. Disconnect the Impingers after
purging. Discard the contents of the midget bubbler. Pour
the contents of the midget Impingers into a leak-free
polyethylene bottle for shipment. Rinse the three midget
impingers and tbe connecting tubes with deionized,
distilled water, and add the washings to tbe same storage
container. Mark the fluid level. Seal and Identify the
sample container.
4.8 Sample Analysis. Note level of liquid In container,
and confirm whether any sample was lost during ship-
ment; note this on analytical data sheet. If a noticeable
amount of leakage has occurred, either void the sample
or use methods, subject to tbe approval of the Adminis-
trator, to correct the final results.
Transfer the contents of the storage container to a
100-ml volumetric flask and dilute to exactly 100 ml
with deionized, distilled water. Pipette a 20-ml aliquot of
this solution into a 250-ml Erlenmeyer flask, add 80 ml
of 100 percent Isopropanol and two to four drops of thortn
indicator, and titrate to a pink endpolnt using 0.0100 N
barium perchlorate. Repeat and average the titration
volumes. Run a blank with each series of samples. Repli-
cate titrations must agree within 1 percent or 0.2 ml,
whichever Is larger.
(NOTE.—Protect the 0.0100 N barium perchlorate
solution from evaporation at all times.)
5. Calibration
5.1 Metering System.
5.1.1 Initial Calibration. Before its initial use in the
field, first leak check the metering system (drying tube.
needle valve, pump, rotameter, and dry gas meter) ft"
III-Appendix A-2 8
-------
follows: plice * vacuum grace at the inlet to the drying
tube and pull a vacuum of 250 mm (10 in.) Hg; plug or
pinch off the outlet of the flow meter, and then turn off
the pump. The vacuum ahall remain stable for at lent
30 seconds. Carefully release the vacuum gauge before
releasing the flow meter end. 87
Next, calibrate the metering system (at the mmpUng
flow rate specified by the method) as follows: connect
an appropriately sited wet test meter (e.g., 1 liter per
revolution) to the inlet of the drying tube. Make three
Independent calibration runs, using at least five revolu-
tions of the dry gas meter per run. Calculate the calibra-
tion factor, Y (wet test meter calibration volume divided
by the dry gas meter volume, both volumes adjusted to
the same reference temperature and pressure), for e*eh
run, and average the results. If any Y value deviate* by
more than 2 percent from the average, the metering
system is unacceptable for use. Otherwise, use the aver-
age as the calibration factor for subsequent test run*.
5.1.2 Post-Test Calibration Check. After each field
test series, conduct a calibration check as in Section 5.1.1
above, except for the following variations: (a) the leak
check Is not to be conducted, (b) three, or more revolu-
tions of the dry gas meter may be used, and (c) only two
independent runs need be made. If the calibration factor
does not deviate by more than 5 percent from the Initial
calibration factor (determined In Section 5.1.1), then the
dry gas meter volumes obtained during the test series
are acceptable. If the calibration factor deviates by more
than 6 percent, recalibrate the metering system as in
Section 5.1.1, and for the calculations, use the calibration
factor (initial or recallbratlon) that yields the lower gas
volume for each test run.
5.2 Thermometers. Calibrate against mereniy-in-
glass thermometers.
5.3 Rotameter. The rotameter need not be calibrated
but should be cleaned and maintained according to the
manufacturer's Instruction.
£.4 Barometer. Calibrate against a mercury barom-
eter.
5-5 Barium Perchlorate Solution. Standardise the
barium perchlorate solution against 25 ml of standard
suUuric acid to which 100 ml of 100 percent isopropenol
has been added.
6. Caleulatlmt
Carry out calculations, retaining at least one eitra
decimal figure beyond that of the acquired data. Round
off figures after final calculation.
6.1 Nomenclature.
Co .-Concentration of sulfur dioxide, dry basis
1 corrected to standard conditions, mg/dscm
. (Ib/dscf).
.Y= Normality of barium perchlorate tltrant,
mUllequivalents/ml.
ft, r=* Barometric pressure at the exit orifice of the
dry gas meter, mm Hg (in. Hg).
Pud -Standard absolute pressure, 760 mm Hg
(29.92 in. Hg).
r.- Average dry gas meter absolute temperature,
TIKI- Standard absolute temperature, 293° K
(528° R).
V.aVolume of sample aliquot titrated, ml.
l'.=-Dry gas volume as measured by the dry gas
meter, dcm (dcf) .
V.(.,j)-Dry gas volume measured by the dry gas
meter, corrected to standard conditions,
dscm (dscf).
Vioio—Total volume of solution in which the sulfur
dioxide sample is contained, 100 ml.
V,- Volume of barium perchlorate tltrant used
for the sample, ml (average of replicate
tltrations).
Vu= Volume of barium perchlorate titrant used
for the blank, ml.
V=- Dry gas meter calibration factor.
32.03= Equivalent weight of sulfur dioxide.
6.2 Dry sample gas volume, corrected to standard
conditions.
y yVm Pl»r
-
tfi-0.3858 "K/mrn Hg for metric unit*.
-17.64 °R/ln. Hg for English units.
6.3 Sulfur dioxide concentration.
where:
Equation 0-1
Equation 6-2
where:
K,-32.03 mx/meq. for metric units.
-7.081X10-«lb/meq. for English unlu.
7. BMIdfrapkf
1. Atmospheric Emissions from Sulfuric Acid Manu-
facturing Processes. U.S. DHEW, PHS, Division of Air
Pollution. Public Health Service Publication No.
999-AP-13. Cincinnati, Ohio. 1965.
2. Corbett, P. F. The Determination of 8O« and 8O»
In Flue Oases. Journal of the Institute of Fuel. t£ 237-
243,1961.
3. Matty, R. E. and E. K. Dlehl. Measuring Flue-Oas
SOt and SOi. Power. 101: 94-97. November 1957.
4. Patton, W. F. and J. A. Brink, Jr. New Equipment
and Techniques for Sampling Chemical Process Gases.
J. Air Pollution Control Association. IS: 162. 1963.
5. Rom, ].]. Maintenance, Calibration, and Operation
of Isokinetic Source-Sampling Equipment. Office of
Air Programs, Environmental Protection Agency.
Research Triangle Park, N.C. APTD-0576. March 1972.
6. Hamil, H. F. and D. E. Camann. Collaborative
Study of Method for the Determination of Sulfur Dioxide
Emissions from Stationary Sources (Fossil-Fuel Fired
Steam Generators). Environmental Protection Agency,
Research Triangle Park, N.C. EPA-650/4-74-024.
December 1973.
7. Annual Book of ASTM Standard!. Part 31; Water.
Atmospheric Analysis. American Society for Testing
and Materials. Philadelphia, Pa. 1974. pp. 40-42.
8. Knoll, J. E. and M. R. Midgett. The Application of
EPA Method 6 to High Sulfur Dioxide Concentrations.
Environmental Protection Agency. Research Triangle
Park, N.C. EPA-600/4-76-038. July 1976.
PROBE (END PACKED'
WITH QUARTZ OR
PYREX WOOL)
STACK WALL
GLASS WOOL
THERMOMETER
MIDGET IMPINGERS
MIDGET BUBBLER
ICE BATH
THERMOMETER
•=51
SILICA GEL
DRYING TUBE
DRY
GAS METER
Figure 6-1. S02 sampling train.
PUMP
SURGE TANK
Ill-Appendix A-2 9
-------
METHOD 7—DETERMINATION or NITROGEN Ozmi
EMISSIONS FROM STATIONAIT SOOKCM
1. Principle and AppllcabaUt
1.1 Principle. A grab sample Is collected In an evacu-
ated flask containing a dilute sulfuric acid-hydrogen
peroxide absorbing solution, and the nitrogen oxides,
except nitrous oxide, are measured colorimeterically
tuing the phenoldisulfonlc acid (POS) procedure.
1.2 Applicability. This method is applicable to the
measurement of nitrogen oxides emitted from stationary
sources. The range of the method has been determined
tc be 2 to 400 milligrams NO. (as NOi) per dry standard
cubic meter, without having to dilute the sample.
LApporotut
2.1 Sampling (see Figure 7-1). Other grab sampling
systems or equipment, capable of measuring sample
volume to within ±2.0 percent and collecting a sufficient
sample volume to allow analytical reprxxfucibility to
within ±5 percent, will be considered acceptable alter-
natives, subject to approval of the Administrator, U.S.
Environmental Protection Agency. The following
equipment is used in sampling:
2.1.1 Probe. Boroslllcate glass tubing, sufficiently
heated to prevent water condensation and equipped
with an in-otack or out-stack filter to remove paniculate
matter (a plug of glass wool is satisfactory for this.
purpose). Stainless steel or Teflon' tubing may also be
used for the probe. Heating is not necessary if the probe
remains dry during the purging period.
> Mention of trade namee or specific products does not
constitute endorsement by the Environmental Pro-
tection Agency.
2.1.2 Collection Flask. Two-liter borosillcate, round
bottom flask, with short neck and 24/40 standard taper
opening, protected against implosion or breakage.
2.1.3 Flask Valve. T-bore stopcock connected to a
24/40 standard taper Joint.
2.1.4 Temperature Gauge. Dial-type thermometer, or
other temperature gauge, capable of measuring 1° C
(2° F) Intervals from -5 to 50°C (25 to 125° F).
2.1.5 Vacuum Line. Tubing capable of withstanding
a vacuum of 75 mm Hg (3 in. Eg) absolute pressure, with
"T" connection and T-bore stopcock.
2.1.6 Vacuum Gauge. tJ-tube manometer, 1 meter
(36 In.), with 1-mm (0.1-in.) divisions, or other gauge
capable o'f measuring pressure to within ±2.5 nun Hg
(0.10 in. Hg).
2.1.7 Pump. Capable of evacuating the collection
flask to a pressure equal to or less than 75 mm Hg (3 in.
Hg) absolute.
2.1.8 Squeeze Bulb. One-way.
2.1.9 Volumetric Pipette. 25 ml.
2.1.10 Stopcock and Ground Joint Grease. A high-
vacuum, high-temperature chlorofluorocarbon grease is
required. Halocarbon 2S-5S has been found to be eflective.
2.1.11 Barometer. Mercury, aneroid, or other barom-
eter capable of measuring atmospheric pressure to within
2.5 mm Hg (0.1 in. Hg). In many cases, the barometric
reading may be obtained from a nearby national weather
service station, in which case the station value (which Is
the absolute barometric pressure) shall be requested and
an adjustment for elevation differences between the
weather station and sampling point shall be applied at a
rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m (100 ft)
elevation increase, or vice versa for elevation decrease.
2.2 Sample Recovery. The following equipment is
required for sample recovery:
2.2.1 Graduated Cylinder. 50 ml with 1-ml divisions.
2.2J Storage Containers. Leak-free polyethylene
bottles.
2.2.3 Wash Bottle. Polyethylene or (lass.
2.2.4 Glass Stirring Rod.
2.2.5 Test Paper for Indicating pH. To cover the pH
imngeof7to!4.
2.3 Analysis. For the analysis, the following equip-
ment Is needed: . -if
2.3.1 Volumetric Pipettes. Two 1 ml, two 2 ml, one
» ml, one 4 ml, two 10 ml, and one 26 ml for each sample
and standard.
2.3.2 Porcelain Evaporating Dishes. 175- to 250-ml
capacity with lip for pouring, one for each sample and
each standard. The Coors No. 45006 (shallow-form, 185
ml) has been found to be satisfactory. Alternatively,
polymeviiyl pentene beakers (Nalge No. 1203, 150ml), or
glass beakers (150 ml) may be used. When glass beakers
are used, etching of the beakers may cause solid matter
to be present in the analytical step; the solids should be
removed by filtration (see Section 4.3). 87
2.3.3 Steam Bath. Low-temperature ovens or thermo-
statically controlled hot plates kept below 70° C (160° F)
are acceptable alternatives.
2A4 Dropping Pipette or Dropper. Three required.
2.3.5 Polyethylene Policeman. One for each sample
and each standard.
2.3.6 .Graduated Cylinder. 100ml with 1-ml divisions.
2.3.7 Volumetric FViks. 50 ml (one for each sample
and each standard), 100 ml (one for each sample and each
80t100rkln*SUn
-------
». Reayentt
Unless otherwise indicated, II Is Intended that all
reagents conform to the specifications established by the
Committee on Analytical Reagents of the American
Chemical Society, where such specifications are avail-
able; otherwise, use the best available grade.
S.I Sampling. To prepare the absorbing solution,
cautiously add 2.8 ml concentrated HiSOi to 1 liter of
deionized, distilled water. Mix well and add 6 ml of 3
percent hydrogen peroxide, freshly prepared from SO
percent hydrogen peroxide solution. The absorbing
solution should be used within 1 week of Its preparation.
Do not expose to extreme heat or direct sunlight.
12 Sample Recovery. Two reagents are required for
•ample recovery:
8.2.1 Sodium Hydroxide (IN). Dissolve 40 g NaOH
in delimited, distilled water and dilute to 1 liter.
8.2.2 Water. Deionited, distilled to conform to ASTM
ipeclflcatlon DU93-74, Type 3. At the option of the
analyst, the KMNOi test for oxidliable organic matter
may be omitted when high concentrations of organic
matter are not expected to be present.
3.3 Analysis. For the analysis, the following reagents
an required:
3.3.1 Fuming Sulfuric Acid. 15 to 18 percent by weight
free sulfur trioxlde. HANDLE WITH CAUTION.
3.3.2 Phenol. White solid.
3.3.8 Sulfuric Acid. Concentrated. 95 percent mini-
mum assay. HANDLE WITH CAUTION.
3.3.4 Potassium Nitrate. Dried at 105 to 110° C (220
to 230° F) for a minimum of 2 hours Just prior to prepara-
tion of standard solution.
3.3.5 Standard KNOi Solution. Dissolve exactly
2.198 g of dried potassium nitrate (KNOi) in deioniied,
distilled water and dilute to 1 liter with deioniced,
distilled water in a 1,000-ml volumetric flask.
3.3.6 Working Standard KNOi Solution. Dilute 10
ml of the standard solution to 100 ml with deionited
distilled water. One mUliliter of the working standard
solution is equivalent to 100 ** nitrogen dioiide (NOi).
8.3.7 Water. Deioniied, distilled as in Section 3.2.2.
8.3.8 Phenoldisulfonic Acid Solution. Dissolve 25 g
of pure white phenol in 150 ml concentrated sulfuric
add on a steam bath. Cool, add 75 ml fuming sulfuric
acid, and heat at 100° C (212° F) for 2 hours. Store In
a dark, stoppered bottle.
4. Procedure*
4.1 Sampling.
4.1.1 Pipette 25 ml of absorbing solution into a sample
flask, retaining a sufficient quantity for use in preparing
the calibration standards. Insert the flask valve stopper
Into the flask with the valve In the "purge" position.
Assemble the sampling train as shown in Figure 7-1
and place the probe at the sampling point. Make sure
that all fittings are tight and leak-free, and that all
ground glass Joints have been properly greased with a
nigh-vacuum, high-temperature chlorofluorocarbon-
based stopcock grease. Turn the flask valve and the
pump valve to their "evacuate" positions. Evacuate
ihe flask to 75 mm Hg (3 in. Hg) absolute pressure, or
less. Evacuation to a pressure approaching the vapor
pressure of water at the existing temperature is desirable.
Turn the pump valve to its "vent" position and turn
off the pump. Check for leakage by observing the ma-
nometer for any pressure fluctuation. (Any variation
greater than 10 mm Hg (0.4 in. Hg) over a period of
I minute Is not acceptable, and the flask is not to be
.. used until the leakage problem Is corrected. Pressure
In the flask Is not to exceed 75 mm Hg (3 in. Hg) absolute
at the time sampling is commenced.) Record the volume
of the flask and: valve (V/), the flask temperature (T.),
and the barometric pressure. Turn the flask valve
counterclockwise to its "purge" position and do the
same with the pump valve. Purge the probe and the
vacuum tube using the squeeze bulb. If condensation
occurs in the probe and the flask valve area, heat the
probe and purge until the condensation disappears.
Next, turn the pump valve to its "vent" position. Turn
the flask valve clockwise to its "evacuate1' position and
record the difference In the mercury levels in the manom-
eter. The absolute internal pressure in the flask (Pi)
Is equal to the barometric pressure less the manometer
reading. Immediately turn the flask valve to the "sam-
ple" position and permit the gas to enter the flask until
pressures in the flask and sample line (i.e., duct, stack)
are equal. This will usually require about 15 seconds;
a longer period indicates a "plug" in the probe, which
must be corrected before sampling is continued. After
collecting the sample, turn the flask valve to its "purge"
position and disconnect the flask from the sampling
train. Shake the flask for at least 5 minutes.
4.1.2 If the gas being sampled contains Insufficient
oxygen for the conversion of NO to NOj (e.g., an ap-
plicable subpart of the standard may require taking a
sample of a calibration gas mixture of NO in Ni). then
oxygen shall be Introduced into the flask to permit this
conversion. Oxygen may be introduced into the flask
by one of three methods; (1) Before evacuating the
sampling flask, flush with pure cylinder oxygen, then
evacuate flask to 75 mm Hg (3 in. Hg) absolute pressure
or less; or (2) inject oxygen into the flask after sampling;
or (3) terminate sampling with a minimum of 50 mm
Hg (2 In. Hg) vacuum remaining in the flask, record
this final pressure, and then vent the flask to the at-
mosphere until the flask pressure Is almost equal to
atmospheric pressure.
4.2 Sample Recovery. Let the flask set for a minimum
of IB hours and then snake the contents for 2 mirutes
Connect the flask to a mercury filled U-tube manometer
Open the valve from the flask to the manomet"< ai>-
record the flask temperature (TV), the barometric
pressure, and the difference between the mercury levels
in the manometer. The absolute internal pressure In
the flask (Pi) is the barometric pressure less the man-
ometer reading. Transfer the contents of the flask to a
leak-free polyethylene bottle. Rinse the flask twice
with 5-ml portions of deioniied, distilled water and add
the rinse water to the bottle. Adjust the pH to between
9 and 12 by adding sodium hydroxide (1 N), dropwise
(about 25 to 35 drops). Check the pH by dipping a
stirring rod into the solution and then touching the rod
to the pH test paper. Remove as little material as possible
during this step. Mark the height of the liquid level so
that the container can be checked for leakage after
transport. Label the container to clearly Identify its
contents. Seal the container for shipping. 87
4.3 Analysis. Note the level of the liquid in container
and confirm whether or not any sample was lost during
shipment; note this on the analytical data sheet. If a
noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of
the Administrator, to correct the final results. Immedi-
ately prior to analysis, transfer the contents of the
shipping container to a 50-ml volumetric flask, and
rinse the container twice with 5-ml portions of deionited,
distilled water. Add the rinse water to the flask and
dilute to the mark with deionited, distilled water; mix
thoroughly. Pipette a 25-ml aliquot into the procelaln
evaporating dish. Return any unused portion of the
sample to the polyethylene storage bottle. Evaporate
the 25-ml aliquot to dryness on a steam bath and allow
to cool. Add 2 ml phenoldisulfonic acid solution to the
dried residue and triturate thoroughly with a polyethyl
ene policeman. Make sure the solution contacts all the
residue. Add 1 ml deioniied, distilled water and four
drops of concentrated sulfuric acid. Heat the solution
on a steam bath for 3 minutes with occasional stirring.
Allow the solution to cool, add 20 ml deionited, distilled
water, mix well by stirring, and add concentrated am-
monium hydroxide, dropwise, with constant stirring,
until the pH Is 10 (as determined by pH paper). If the
sample contains solids, these must be removed by
nitration (centrifugation is an acceptable alternative,
subject to the approval of the Administrator), as follows:
flltei through Whatman No. 41 filter paper into a 100-ml
volumetric flask; rinse the evaporating dish with three
5-ml portions of deioniied, distilled water; filter these
three rinses. Wash the filter with at least three 15-ml
portions of deionited, distilled water. Add the filter
washings to the contents of the volumetric flask and
dilute to the mark with deionited, distilled water. If
solids are absent, the solution can be transferred directly
to the 100-ml volumetric flask and diluted to the mark
with deionited. distilled water. Mix the contents of the
flask thoroughly, and measure the absorbance at the
optimum wavelength used for the standards (Section
5.2.1), using the blank solution as a tero reference. Dilute
the sample and the blank with equal volumes of deion-
iied, distilled water if the absorbance exceeds A,, the
absorbance of the 400 pg NO) standard (see Section 5.2.2)9'
C. CaltonHm
6.1 Flask Volume. The volume of the collection flask -
flask valve combination must be known prior to sam-
pling. Assemble the flask and flask valve and fill with
water, to the stopcock. Measure the volume of water to
±10 ml. Record this volume on the flask.
0.2 Spectrophotometer Ce'.ibration.
5.2.1 Optimum Wavelength Determination.
Calibrate the wavelength scale of the spec-
trophotometer every 6 months. The calibra-
tion may be accomplished by using an
energy source with an Intense line emission
•uch as a mercury lamp, or by using a series
of glass filters spanning the measuring
range of the spectrophotometer. Calibration
materials are available commercially and
from the National Bureau of Standards.
Specific details on the use of such materials
should be supplied by the vendor; geueral
information about calibration techniques
can be obtained from general reference
books on analytical chemistry. The wave-
length scale of the spectrophotometer must
read correctly within ± 5 nm at all calibra-
tion points; otherwise, the spectrophoto-
meter shall be repaired and recalibrated.
Once the wavelength scale of the spectro-
photometer is in proper calibration, use 410
nm as the optimum wavelength for the mea-
surement of the absorbance of the stan-
dards and samples. 87
Alternatively, a scanning procedure may
be employed to determine the proper mea-
suring wavelength. If the Instrument is a
double-beam spectrophotometer, scan the
spectrum between 400 and 415 nm using a
200 jig NO, standard solution in the sample
cell and a blank solution in the reference
cell. If a peak does not occur, the spectro-
photometer is probably malfunctioning and
should be repaired. When a peak is obtained
within the 400 to 415 nm range, the wave-
length at which this peak occurs shall be
the optimum wavelength for the measure-
ment of absorbance of both the standards
and the samples. For a single-beam spectro-
photometer, follow the scanning procedure
described above, except that the blank and
standard solutions shall be scanned sepa-
rately. The optimum wavelength shall be
the wavelength at which the maximum dif-
ference in absorbance between the standard
and the blank occurs.87
8.2.2 Determination of Spectrophotometer
Calibration Factor K*. Add 0.0 ml. 2 ml. 4
ml, 6 ml, and 8 ml of the KNOi working
standard solution (1 ml = 100 jig NO,) to a
series of five 50-ml volumetric flasks. To
each flask, add 25 ml of absorbing solution,
10 ml deionized. distilled water, and sodium
hydroxide (1 N) dropwise until the pH is be-
tween 9 and 12 (about 25 to 35 drops each).
Dilute to the mark with deionized. distilled
water. Mix thoroughly and pipette a 25-ml
aliquot of each solution into a separate por-
celain evaporating dish. 87
Beginning with the evaporation step, follow the analy-
sis procedure of Section 4.3, until the solution has been
transfejred to the 100 ml volumetric flask and diluted to
the mark. Measure the absorbance of each solution, at the
optimum wavelength, as determined in Section 5.2.1.
This calibration procedure must be repeated on each day
that samples arc analyted. Calculate the spectrophotom-
eter calibration factor as follows:
Equation 7-1
where:
AT, = Calibration factor
A\= Absorbance of the 100-/ig NO; standard
Xi=Absorbance of the 200-jig NOj standard
Ai=> Absorbance of the 300-jig NO2 standard
/4(= Absorbance of the 400-** NO! standard
5.3 Barometer. Calibrate against a mercury barom-
eter.
5.4 Temperature Gauge. Calibrate Jia. tlieiTK.net. rs
86*:. st mercury-in-glass thermometers.
5.5 Vacuum Oauge. Calibrate mechanical gauges, if
used, against a mercury manometer such as that speci-
fied in 2.1. 6.
5.6 Analytical Balance. Calibrate against standard
weights.
6. Calculation*
Carry out the calculations, retaining at least one extra
decimal figure beyond that of the acquired data. Round
off figures after final calculations.
6.1 Nomenclature.
A = Absorbance of sample.
C=Concentration of NO, as NOi, dry basis, cor-
rected to standard conditions, mg/dscm
Ob/dscf).
F=Dilution factor (i e., 25/6, 26/10, etc., required
only if sample dilution was needed to reduce
the absorbance into the range of calibration).
Jf <=8pectrophotometer calibration factor. „,
m=MassofNO,as NOi in gas sample, itf.. °'
P/— Final absolute pressure of flask, mm Hg (in. Hp).
P.-=Initial absolute pressure of flask, mm Hg (in.
Hg).
P,ui= Standard absolute pressure, 760mm Hg (29.92 in.
He).
T/=Final absolute temperature of flask ,°K (°R).
Ti = Initial absolute temperature of flask. °K (°R).
r,tj = Standard absolute temperature, 293° K (528° R)
V'i«=Sample volume at standard conditions (dry
basis), ml.
V/=Volume of flask and valve, ml.
V.=Volume of absorbing solution, 26 ml.
2=60/26, the aliquot factor. (If other than a 25-ml
aliquot was used for analysis, the correspond-
ing factor must he substituted).
6.2 Sample volume, dry basis, corrected to standard
conditions.
where:
,= 0.3858
°K
mm Hg
Equation 7-2
for metric units
= 17.64 —^r- for English units
in. Hg
Ill-Appendix A-31
-------
6.3 Total itg NOi per sample.
m=2KcAF
Equation 7-3
NOTE.—If other than a 25-ml aliquot IB used (or analy-
iis, the (actor 2 must be replaced by a corresponding
actor.
6.4 Sample concentration, dry basis, corrected to
tandard conditions.
Equation 7-4
rhere:
K,= 101 for metric units
pg/ml
3. Jacob, M. B. The Chemical Analysis of Air Pollut-
ants. New York. Intersclence Publishers, Inc. 1960.
Vol. 10, p. 351-356.
4. Beatty, R. L., L. B. Berger, and H. H. Schrenk.
Determination of Oxides of Nitrogen by the Phenoldisul-
fonic Acid Method. Bureau of Mines, U.S. Dept. of
Interior. R. I. 3687. February 1943.
5. Bamil, H. F. and D. E. Camann. Collaborative
Study of Method for the Determination of Nitrogen
Oxide Emissions from Stationary Sources (Fossil Fuel-
Fired Steam Generators). Southwest Research Institute
report (or Environmental Protection Agency. Research
Triangle Park, N.C. October 5,1973.
6. Hamil, H. F. and R. E. Thomas. Collaborative
Study of Method (or the Determination of Nitrogen
Oxide Emissions from Stationary Sources (Nitric Acid
Plants). Southwest Research Institute report for En-
vironmental Protection Agency. Research Triangle
Park, N.C. May8,1974.87
=6.243X10-' - for English units
pg/ml
. Blbliofraphy
1. Standard Methods of Chemical Analysis. 6th ed.
•lew York_D. Van Nostrand Co., Inc. 1962. Vol. 1,
I. 329-330. of
2. Standard Method of Test for Oxides of Nitrogen In
Jaseous Combustion Products (Phenoldisulfonic Acid
•rocedure). In: 1968 Book of ASTM Standards, Part 2C.
>hiladelphla, Pa. 1968. ASTM Designation D-1608-60,
i. 726-729.
Ill-Appendix A-32
-------
METHOD g—DETERMINATION or SoLroaic Acra Mai
AND SuiruB DIOXIDE EMISSIONS FROM STATIONARY
SOURCES
1. Principle and Applicability
1.1 Principle. A gas sample is extracted Isokinetlcally
from the stack. The sulfuric acid mist (Including sulfur
trloxlde) and the sulfur dloiide are separated, and both
fractions are measured separately by the barium-thorin
Utration method.
1.2 Applicability. This method is applicable for the
determination of sulfuric acid mist (Including sulfur
trloiide, and in the absence of other paniculate matter)
and sulfur dloiide emissions from stationary sources.
Collaborative tests have shown that the minimum
detectable limits of the method are 0.05 milligrams/cubic
meter (0.03XKH pounds/cubic foot) for sulfur trloiide
and 1.2 rng/m> (0.74 10-' lb/(t>) for sulfur dioilde. No
upper limits have been established. Based on theoretical
calculations for 200 miUililers of 3 percent hydrogen
peroiide solution, the upper concentration limit for
sulfur dioxide in a 1.0 m» (35.3 ft>) gas sample is about
12.400 mg/mJ (7.7X10-* lb/ft>). The upper limit can be
extended by increasing the Quantity of peroxide solution
In the impmgers.
Possible interfering agents of this method are fluorides,
free ammonia, and dimethyl aniline. If any of these
Interfering agents are present (this can be determined by
knowledge of the process), alternative methods, subject
to the approval of the Admlnlstrator.U.S.EPAare
required. 87
Filterable participate matter may be do- .
termined along with SO, and Sd (subject to
the approval of the Administrator) by In-
serting a heated glass fiber filter between
the probe and isopropanol impinger (see
Section 2.1 of Method 6). If this option is
chosen, participate analysis is gravimetric
only:' H.SO. acid mist is not determined sep-
arately. 87
2. Afparatut
2.1 Sampling. A schematic of the sampling train
used In this method Is shown In Figure 8-1; It is similar
to the Method 5 train except that the filler position is
different and the filler holder dot's not have lo be heated.
Commercial models of this train are available. For those
who desire to build their own, however, complete con-
struction details arc described in Al'TD-ftVJl. Changes
from the Al'TU-UVil document and allowable modi-
fications to Figure 8-1 are discussed In the following
subsections.
The operating and maintenance procedures for the
sampling train are described In A l*Ti)-Oo76. Since correct
usage Is Important In obtaining valid results, all users
should read Ihu A1'T1>-0076 dorurnent and adopt the
operating and maintenance procedures outlined In It,
unless otherwise specified herein. Further details and
guidelines on operation and maintenance are (riven In
Method 5 and should bu read and followed whenever
they are applicable.
2.1.1 ProlH! Nozzle. Same as Method 5, Section 2.1.1.
2.1.2 I'rolw Uncr. UorodlUcatn or uuarU glass, with a
healing system to prevent visible condensation during
sampling. Do not use metal probe liners.
•J.I.a 1'itot Tube. Same 03 Method 5. Section 2.1.3.
5.1.4 Differential Pressure Gauge. Same as Method 5,
Section 2.1.4.
2.1.6 Filter Bolder. Borosllicate glass, with a glass
Ml filter support and a slllcone rubber gasket. Other
gasket materials, e.g., Teflon or Vlton, may be used sub-
ject to the approval of the Administrator. The holder
design shall provide a positive seal against leakage from
the outside or around tbe filter. The filter bolder shall
be placed between the first and second Implngers. Note:
Do not heat the filter holder.
3.1.6 Implngers—Four, as shown In Figure W. The
Ant and third shall be of tbe Ore«nburg-8mlth design
with standard tips. Tbe second and fourth shall be of
the Greenburg-Smlth design, modified by replacing the
Insert with an approximately 13 millimeter (0.5 In.) ID
glass tube, having an unconstricted tip located 13 nun
(0.5 In.) from the bottom of the flask. Similar collection
(TStems, which have been approved by the Adminis-
trator, may be nsed.
2.1.7 Metering System. Same as Method 6, Section
2.1.8 Barometer. Same as Method b. Section 2.1.9.
2.1.9 Oas Density Determination Equipment. Same
at Method 9, Section 2.1.10.
2.1.10 Temperature Gauge. Thermometer, or equiva-
lent, to measure the temperature of the gas leaving tbe
Impinger train to within 1° C (2° F).
2.2 Sample Recovery.
TEMPERATURE SENSOR
PROBE
PITOT TUBE
TEMPERATURE SENSOR
-*m
«_J _-rrv— ---
«
~rTTW— . ^
THERMOMETER
FILTER HOLDER
.CHECK
VALVE
7
REVERSE TYPE
PITOT TUBE
VACUUM
LINE
VACUUM
GAUGE
MAIN VALVE
DRY TEST METER
Figure 8-1. Sulfuric acid mist sampling train.
Ill-Appendix A-33
-------
12.1 Wash Bottles. Polyethylene or glass, 500 ml.
(two).
J.2.2 Graduated Cylinders. 280 ml, 1 liter. (Volu-
metric flasks may also be used.)
JJ.8 Storage Bottles. Leak-tree polyethylene bottles,
1000 ml die (two for each sampling run).
2.2.4 Trip Balance. 500-gram capacity, to measure to
±0.51 (necessary only If a moisture content analysis Is
to be done).
2.3 Analysis.
2.3.1 Pipettes. Volumetric 25 ml, 100 ml.
2.3.2 Burette. «0ml. 87
2.3.3 Erlenmeyer Flask. 250 ml. (one for each sample
blank and standard).
2.3.4 Graduated Cylinder. 100 ml.
2.3.5 Trip Balance. 500 g capacity, to measure to
±0.5 g.
2.3.6 Dropping Bottle. To add Indicator solution,
125-ml site.
3. Rraecnti
Unless otherwise Indicated, all reagents are to conform
to the specifications established by the Committee on
Analytical Reage.nts of the American Chemical Society,
where such specifications are available. Otherwise, use
the best available grade.
3.1 Sampling.
3.1.1 Filters. Same as Method 5, Section 3.1.1.
8.1.2 Silica Qel. Same as Method 5. Section 3.1.2.
3.1.3 Water. Delonlted. distilled to conform to A8TM
specification D1193-74, Type 3. At the option of the
analyst, the KMnOi test (or oxldicable organic matter
may be omitted when high concentrations of organic
matUr are not eipecled to be present.
1.1.4 Isopropanol. 80 Percent. Mil 800 ml of Isopro-
panol with 200 ml of delonlted, distilled water.
Noil.—Experience hasahown that only A.C.S. grade
Isopropanol Is satisfactory. Tests bave shown that
Isopropanol obtained bom commercial sources occa-
easionally has peroxide Impurities that will cause er-
roneously high sulfurlc acid mist measurement. Use
the following test for detecting peroxides in each lot of
Isopropanol: Shake 10 ml of the Isopropanol with 10 ml
photometer at 352 nanometers. II tbo absorbance exceeds
0.1. the Isopropanol shall not be used. Peroxides may be
removed from Isopropanol by redistilling, or by passage
Uuough a column of activated alumina. However, re-
agent-trade Isopropanol with suitably low peroxide levels
Is readily available from commercial sources; therefore,
rejection of contaminated lots may be more efficient
than following the peroxide removal procedure.
3.1.5 Hydrogen Peroxide. 3 Percent. Dilute 100 ml
of 30 percent hydrogen peroxide to 1 liter with delonlted,
distilled water. Prepare fresh dally.
3.1.6 Crushed Ice.
8.2 Sample Recovery.
SJ.l Water. Same as 3.1.3.
3.2.2 Isopropanol, 80 Percent. Same as 3.1.4.
3.3 Analysis.
3.3.1 Water. Same as 3.1.3.
3.3.2 Isopropanol, 100 Percent.
8.3.3 Thorin Indicator. l-(o-arsonophenylaro)-2-naph-
thol-3, e-dlsulfonlc acid, dlsodlum salt, or equivalent.
Dissolve 0.201 In 100 ml of delonlted. distilled water.
8.3.4 Barium Perchlorate (0.0100 Normal). Dissolve
1.95 g of barium perchlorate trlhydrate (B»(C10<)i-3HiO)
In 200 ml delonlted, distilled water, and dilute to 1 liter
with Isopropanol; 1.22 g of barium chloride dlhydmte
(BaCli-2HiO) may be used instead of the barium per-
chlorate. Standardly with sulfurie acid as in Section 5.2.
This solution must be protected against evaporation at
all times.
3.3.5 Sulfurie Acid Standard (0.0100 N). Purchase or
standardize to ±0.0002 N against 0.0100 N NaOH that
has previously been standardized against primary
standard potassium acid phthaiate.
4. Procedure
4.1 Sampling.
4.1.1 Pretest Preparation. Follow the procedure out-
lined in Method 5, Section 4.1.1; niters should be In-
spected, but need not be desiccated, weighed, or identi-
fied. If the effluent gas can be considfred dry, i.e., mois-
ture free, the silica gel need not be weighed.
4.1.2 Preliminary Determinations. Follow the pro-
cedure outlined in Method 5, Section 4.1.2.
4.1.3 Preparation of Collection Train. Follow the pro-
cedure outlined in Method 5, Section 4.1.3 (except for
the second paragraph and other obviously inapplicable
parts) and use Figure 8-1 instead of Figure 5-1. Replace
the second paragraph with: Place 100 ml of 80 percent
isopropanol in the first impinger, 100 ml of 3 percent
hydrogen peroxide in both the second and third im-
plngers; retain a portion of each reagent for use as •
blank solution. Place about 200 g of silica gel in the fourth
impinger.
PLANT.
LOCATION
OPERATOR
DATE
RUN NO
SAMPLE BOX NO..
METER BOX N0._
METER A Kg
CFACTOR
PITOT TUBE COEFFICIENT, Cp.
STATIC PRESSURE, mm HI (in. H|).
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
ASSUMED MOISTURE, X
PROBE LENGTH, m (ft)
SCHEMATIC OF STACK CROSS SECTION
NOZZLE IDENTIFICATION NO
AVERAGE CALIBRATED NOZZLE DIAMETER, cm (in.).
PROBE HEATER SETTING ; .
LEAK RATE,m3/min,(efm)
PROBE LINER MATERIAL
FILTER NO.
TRAVERSE POINT
NUMBEF.
TOTAL
SAMPLING
TIME
(0), min.
AVERAGE
VACUUM
mm H|
(in. H|)
STACK
TEMPERATURE
JT5>'
°C <*F)
VELOCITY
HEAD
-------
NOTE.—If moisture content Is to be determined by
Impinger analysis, welsh ecch of the first three implngero
(plus absorbingsolutlon) to the nearest O.S c and record
then weights. The weight of the silica gel (or silica eel
plus container) must also be determined to the nearest
0.5 a and recorded.
4.1.4 Pretest Leak-Check Procedure. Follow tho
bealc procedure outlined in Method 5, Section 4.1.4.1,
noting that the probe heater shall be adjusted to tho
minimum temperature required to prevent condensa-
tion, and also that verbese such as, " • • • plugging the
Inlet to the filter holder • • • ," shall be replaced by,
"° ' ' plugging the inlet to the first impinger « • °."
The pretest leak-checb Is optional. 8/
4.1.5 Train Operation. Follow the basic procedures
outlined In Method 5, Section 4.1.5, in conjunction with
the following special instructions. Data snail be recorded
on o sheet similar to the one in Figure 8-2. The campling
rote shall not exceed 0.030 m'/min (1.0 cfm) during too
run. Periodically during the test, obsarve the connecting
line between the probe and first impinger for signs cJ
condensation. If it does occur, adjust the probe heater
setting upward to the minimum temperature required
to prevent condensation. If component changes beeomo
necessary during a run, & leak-check shall be done im-
mediately before each change, according to the procedure
outlined in Section 4.1.4.2 of Method 5 (with appropriate
modifications, as mentioned In Section 4.1.4 of thlo
method); record all leak rates. If the leakage rate(o)
exceed the specified rate, the tester shall either void tho
run or shall plan to correct the sample volume ss out-
lined in Section 6.3 of Method 5. Immediately after com-
ponent changes, leak-checks are optional. If thesa
le&tr-chectis are done, the procedure outlined in Section
4.1.4.1 of Method 5 (with appropriate modifications)
shall be usad. •
After turning of! the pump and recording the final
readings at the conclusion of each run, remove the probe
from the stack. Conduct a post-test (mandatory) leak-
check as in Section 4.1.4.3 of Method 5 (with appropriate
modification) and record the leak rate. If the post-test
leakage rate exceeds the specified acceptable rate, the
tester shall either correct the sample volume, as outlined
in Section 6.3 of Method 5, or shall void the run.
Drain the ice bath and, with the probe disconnected,
purge the remaining part of the train, by drawing clean
ambient air through the system for 15 minutes at the
average flow rate used for sampling.
NOTE.—Clean ambient air can be provided by passing
air through a charcoal filter. At the option of the tester,
ambient air (without cleaning) may be used.
4.1.6 Calculation of Percent Isokinetic. Follow the
procedure outlined in Method 5, Section 4.1.6.
4.2 Sample Recovery.
4.2.1 Container No. 1. If a moisture content analysis
is to be done, weigh the first Impinger plus contents to
the nearest 0.5 g and record this weight.
Transfer the contents of the first impinger to a 250-ml
graduated cylinder. Rinse the probe, first Impinger, all
connecting glassware before the filter, and the front half
of the filter holder with 80 percent isopropanol. Add the
rinse solution to the cylinder. Dilute to 250 ml with 80
percent isopropanol. Add the filter to the solution, mix,
end transfer to the storage container. Protect the solution
against evaporation. Mark the level of liquid on the
container and identify the sample container, o/
4.2.2 Container No. 2. If a moisture content analysis
Is to be done, weigh the second and third impingera
(plus contents) to the nearest 0.5 g and record these
weights. Also, weigh the spent silica gel (or silica gel
plus impinger) to the nearest 0.5 g.
Transfer the solutions from the second and third
impingera to a 1000-ml graduated cylinder. Rinse all
connecting glassware (Including back half of filter holder)
between the filter and silica geflmpinger with deionized,
distilled water, and add this rinse water to the cylinder.
Dilute to a volume of 1000 ml with deionized, distilled
water. Transfer the solution to a storage container. Marl:
the level of liquid on the container. Seal and identify the
sample container.
4.3 Analysis.
Note the level of liquid In containers 1 and 2, and con-
firm whether or not any sample was lost during ship-
ment; note this on the analytical data sheet. If a notice-
able amount of leakage has occurred, either void the
sample or use methods, subject to the approval of the
Administrator, to correct the final results. •
4.3.1 Container No. 1. Shake the container holding
the isopropanol solution and the filter. If the filter
breaks up, allow the fragments to settle for a few minutes
before removing a sample. Pipette a 100-ml aliquot of
this solution into a 250-ml Erlenmeyer flask, add 2 to 4
drops of thorin indicator, and titrate to a pink endpoint
using 0.0100 N barium perchlorate. Repeat the titratlon
with a second aliquot of sample and average the titratlon
TOjp«>. Replicate titrations must ogrea within 1 psreant
or 0.2 ml, whichever Is greater.
Volnme of sample aliquot titrated, 100 ml
tor HtSOi and 10 ml for S0>.
Vi,=Total volume of liquid collected in Impingers
and silica gel, ml.
V0=Volume of gas sample as measured by dry
,, gas meter, ocm (dcf).
v mi>iK>=volume of gas sample measured by the dry
gas meter corrected to standard conditions,
oscm (dscf). 87
t>.*°Average stack gas velocity, calculated by
Method 2, Equation 2-9, using data obtained
. r from Method 8, m/sec (ft/sec).
v join=Total volume of solution in which the
sulfurlr acid or sulfur dioxide sample is
contained, 250 ml or 1,000 ml, respectively.87
Vi=Volume of barium perchlorate titrant used
for the sample, ml.
Vu=Volume of barium perchlorate titrant used
for the blank, ml.
K=>Dry gas meter calibration factor.
AH=Average pressure drop across orifice meter,
mm (In.) HrO.
6=Total sampling time, mln.
13.6=8peclfic gravity of mercury.
60=sec/min.
100=Conversion to percent.
3.2 Average dry gas meter temperature and average
orifice pressure drop. See data sheet (Figure 8-2).
6.3 Dry Oas Volume. Correct the sample volume
measured by the dry gas meter to standard conditions
(20° C and 760 mm Hg or 68° F and 29.92 in. Hg) by using
Equation 8-1.
coJate the moisture content of the otccS gas, using Equa-
tion 5-3 of Method 5. The "Note" In Section 6.5 of Method
5 also applies to this method. Note that If the effluent gcs
stream can be considered dry, the volume of water vapor
cod molstare content need not be calculated.
6.5 Sulfuric acid mist (including SOi) concentration.
(old)
Equation 8-2
where:
Si=0.04904 g/milliequivalent for metric units.
=1.031X10-4 Ib/meq for English units.
0.6 Sulfur dioxide concentration.
(old)
Equation 8-3
where:
JST,=0.03203 eVmeq for metric units.
=7.081X10-» Ib/meq for English units.
3.7 lEokinetic Variation.
9.7.1 Calculation from raw data.
100 T0[Kt
Equation 8-4
87
where:
5T(=0.003464 mm Hg-m'/ml-<>K for metric unite.
=0.002876 in. Hg-ft'/ml-°R for English units.
3.7.2 Calculation from Intermediate values.
7=
(oU) ali
Pali 100
Equation 8-1
where:
£f,^0.3858°K/mm Hg for metric units.
= 17.64 °R/in. Hg for English units.
NOTE.—If the leak rate observed during any manda-
tory leak-checks exceeds the specified acceptable rate,
the tester shall either correct the value of VQ In Equation
6-1 (as described In Section 6.8 of Method 5), or shell
Invalidate the test run.
8.4 Volume of Water Vapor and Moisture Content.
Calculate the volume of water vapor using Equation
5-2 of Method 5; the weight of water collected in the
implngers and silica gel can be directly converted to
milllliters (the specific gravity of water Is 1 s/ml). Cal-
TMv,eAaP, 60 (1-B.a)
— K TaVa (QtJ)
-*•' P.»o^o»(l-B«)
Equation 8-5
where:
£Tt=4.320 for metric unite.
=0.09450 for English units.
6.8 Acceptable Results. If SO percent
-------
METHOD 9—VISUAL DETEB1HNATTON OF THE
OPACITY OF EMISSIONS PBOM 6TATIONABT
SOURCES "5
Many stationary sources discharge visible
emissions into the atmosphere; these emis-
sions are usually in the shape of a plume.
This method Involves the determination of
plume opacity by qualified observers. The
method Includes procedures for the training
and certification of observers, and procedures
to be used in the field for determination of
plume opacity. The appearance of a plume as
viewed by an observer depends upon a num-
ber of variables, some of which may be con-
trollable and some of which may not be
controllable in the field. Variables which can
be controlled to an extent to which they no
longer exert a significant influence upon.
plume appearance Include: Angle of the ob-
server with respect to the plume; angle of the
observer with respect to the sun; point of
observation of attached and detached steam
plume; and angle of the observer with re-
spect to a plume emitted from a rectangular
stack with a large length to width ratio. The
method includes specific criteria applicable
to these variables.
Other variables which may not be control-
lable in the field are luminescence and color
contrast between the plume and the back-
ground against which the plume is viewed.
These variables exert an Influence upon the
appearance of a plume as viewed by an ob-
server, and can affect the ability of the ob-
server to accurately assign opacity values
to the observed plume. Studies of the theory
of plume opacity and field studies have dem-
onstrated that a plume is most visible and
presents the greatest apparent opacity when
viewed against a contrasting background; It
follows from this, and is confirmed by field
trials, that the opacity of a plume, viewed
under conditions where a contrasting back-
ground Is present can be assigned with the
greatest degree of accuracy. However, the po-
tential for a positive error Is also the greatest
when a plume Is viewed under such contrast-
Ing conditions. Under conditions presenting
a less contrasting background, the apparent
opacity of a plume is less and approaches
zero as the color and luminescence contrast
decrease toward zero. As a result, significant
negative bias and negative errors can bo
made when a plume is viewed under less
contrasting conditions. A negative bias da-
creases rather than increases the possibility
that a plant operator will be cited for a vio-
lation of opacity standards due to observer
error.
Studies have been undertaken to determine
the magnitude of positive errors which can
be made by qualified observers while read-
Ing plumes under contrasting conditions and
using the procedures set forth in this
method. The results of these .studies (field
trials) which Involve a total of 769 sets of
25 readings each are as follows:
(I) For black plumes (133 sets at a smoke
generator), 100 percent of the sets were
read with a positive error1 of less than 7.5
percent.opacity; 99 percent were read with
a positive error of less than 5 percent opacity.
(2) For white plumes (170 sets at a smoke
generator, 168 sets at a coal-fired power plant,
298 seta at a sulfurlc acid plant). 99 percent
of the sets were read with a positive error of
less than 7.5 percent opacity; 95 percent were
read with a positive error ofless than 5 per-
cent opacity.
The positive observational error associated
with an average of twenty-five readings is
therefore established. The accuracy of- the
method. must be taken into account-when
determining possible violations of appli-
cable opacity standards.
»For a set, positive error=average opacity
determined by observers' 25 observations—
average opacity determined from transmis-
someter'B 25 recordings.
1. Principle and applicability.
l.i Principle. The opacity of emissions
from stationary sources is determined vis-
ually by a qualified observer. -
1.2 Applicability. This method is appli-
cable for the determination of the opacity
of emissions from stationary sources pur-
suant to !60.11(b) and for qualifying ob-
servers for visually determining opacity of
emissions. .
2. Procedures. The observer qualified In
accordance with paragraph 8 of this method
shall use the following procedures for vis-
ually determining the opacity of emissions:
2.1 Posltion-Tha qualified observer shall.
stand at a distance sufficient to provide- a
clear view of the emissions with the sun
oriented in the 140* sector to his back. Con-
sistent with maintaining the above require-
ment, the observer shall, as much as possible,
make his observations from a position such
that his line of vision is approximately
perpendicular to the plume direction, and
when observing opacity of emissions from
rectangular outlets (e.g. roof monitors, open
baghouses, noncircular stacks), approxi-
mately perpendicular to the longer axis of
the outlet. The observer's line of sight should
not include more than one plume at a tune
when multiple stacks are involved, and in
any case the observer should make his ob-
servations with bis line of sight perpendicu-
lar to the longer axis of such a set of multi-
ple stacks (e.g. stub stacks on baghouses).
22 Field records. The observer shall re-
cord the name of the plant, emission loca-
tion, type facility, observer's name and
affiliation, and the date on a field data sheet
(Figure 9-1). The time, estimated distance
to the emission location, approximate wind
direction, estimated wind speed, description
of the sky condition (presence and color of
clouds). and plume background are recorded
on a field data sheet at the time opacity read-
ings are initiated and completed. • .
2.3 Observations. Opacity observations
snail bo made at the point of greatest opacity
in that portion of the plume where con-
densed water vapor Is not present. The ob-
server shall not look continuously at the
plume, but lntts«<3 shall observe tbo plume
momentarily at iS-iecond intervals.
2.3.1 Attached steam plumes. When con-
densed water vapor is present within the
plume as It emerges from the emission out-
let, opacity observations shall bo made be-
yond the point in the plume at which con-
densed water vapor Is no longer visible. The
observer shall record the approximate dis-
tance from the emission outlet to the point
in the plume at which the observations are
made.
2.3.2 Detached steam plume. When water
vapor in the plume condenses and becomes
visible at a distinct distance from the emis-
sion outlet, the opacity of emissions should
be evaluated at the emission outlet prior to
the condensation of water vapor and tbe for-
mation of the steam plume. • •
2.4 Recording observations. Opacity ob-
servations shall be recorded to the nearest 5
percent at 15-second intervals on an ob-
servational record sheet. (See Figure 9-2 for
an example.) A minimum of 24 observations
shall be recorded. Each momentary observa-
tion recorded shall bo deemed to represent
the average opacity of emissions for a IB-
second period.
2.5 Data Reduction. Opacity shall be de-
termined as an average of 24 consecutive
observations recorded at 15-second intervals.
Divide the observations recorded on the rec-
ord sheet Into sets of 24 consecutive obser-
vations. A set Is composed of any 24 con-
secutive observations. Sets need not be con-
secutive in time and.In no case shall two
sets overlap. For each set of 24 observations,
calculate the average by summing the opacity
of the 24 observations and dividing this sum
by 24. If an applicable standard specifies an
averaging time requiring more than 24 ob-
servations, calculate the average for all ob-
servations made during the specified time
period. Record the average opacity on a record
sheet. (See Figure 9-1 for an example.)
3. Qualifications and testing. -
3.1 Certification requirements. To receive
certification as a qualified observer, a can-
didate must be tested and .demonstrate the
ability to assign opacity readings la 6 percent
Increments to 25 different black plume* and
39 different white plumes, with «n error
not to exceed 16 percent opacity on any one
reading and an average error not to exceed
7.5 percent opacity In each category. Candi-
dates shall be tested according to the pro-
cedures described In paragraph 82. Smoke
generators, used pursuant to paragraph 32
shall be equipped with a smoke meter which
meets the requirements of paragraph 3.3. '
The certification shall be valid for a period
of 6 months, at which time tbe qualification
procedure must be repeated by any observer
in order to retain certification. _ ;
• 32 Certification procedure. The certifica-
tion test consists of showing the candidate a
complete run of 60 plumes—25 black plumes
and 25 white plumes—generated by a smoke
generator. Plumes within each set of 26 black
and 25 white runs shall be presented in ran-
dom order. The candidate assigns an opacity
value to each plume and records his obser-
vation on a suitable form. At the completion
of each run of 60 readings, the score of the
candidate is determined. If a candidate falls
to qualify, the complete run of 50 readings
must be repeated in any retest. The smoke
test may be administered as part of a smoke
school or training program, and may be pre-
ceded by training or familiarization runs of
the smoke generator during which candidates
are shown black and white plumes of known
opacity. . . •
• 3.3 Smoke generator 'specifications. Any
smoke generator used for the purposes of
paragraph 82 «hau be equipped with a smoke
meter installed to measure opacity across
(he diameter of the smoke generator stock.
The smoke meter output shall display In-
stack opacity based upon a pathlengtb equal
to tbe stock exit diameter, on a full 0 to 100
percent chart recorder scale. The smoke
meter optical design and performance shall
meet the specifications shown In Table 9-1.
The smoke meter shall be calibrated as pre-
scribed in paragraph 3.3.1 prior to tbe con-
duct of each smoke reading test. At th«
completion of each test, the zero and span
drift shall be checked and If the drift ex-
ceeds ±1 percent opacity, the condition shall
be corrected prior to conducting any subse-
quent test runs. The smoke meter shall bo
demonstrated, at the time of Installation, to
meert the specifications listed in Table 9-1.
This demonstration shall bo repeated fol-
lowing any subsequent repair or replacement
of the photocell or associated electronic cir-
cuitry including the chart recorder or output
meter, or every 6 months, whichever occurs
first.
331 Calibration. Tbe smoke meter Is
calibrated after allowing a mfnimnm of 80
minutes -warmup by alternately producing
simulated opacity of 0 percent and 100 per-
cent. When stable response at 0 percent of
100 percent is noted, the smoke meter is ad-
justed to produce an output of 0 percent or
100 percent, as appropriate. This calibration
shall be repeated until stable 0 percent and
100 percent readings are produced without
adjustment. Simulated 0 percent and 100
percent opacity values may be produced by
alternately switching the power to the light
source on and off while the smoke generator
is not producing smoke.
Ill-Appendix A-36
-------
Parameter:
a. Light source...-.
b. Spectral response
• of photocell.'
TABU •—I—-6KOKS MZTKB DESIGN AMD
! BPBCTF1CATXOKS
. Specification
Incandescent lamp
operated at nominal
rated voltage.
Photoplc (daylight
- spectral response of
the human eye—
. reference 4.3).
15* TMJ^TlTTlTlm tOtal
angle.
15* maximum total
angle.
±3% opacity, maxi-
mum.
±1% opacity, 30
minutes.
£6 seconds.
e. Angle of view
d. Angle . of projec-
tion.
e. Calibration error.
f. Zero and span
•drift.
g. Response time—
3.32 Smoke meter evaluation. The smoke
meter design and performance are to be
evaluated as follows:
3.32.1 Light source. Verify from manu-
facturer's data and from voltage measure-.
merits made at the lamp, as Installed, that
the lamp is .operated within ±5 percent of
the nominal rated voltage.
8322 Spectral response of photocell.
Verify from manufacturer's data that the
photocell has a photoplc response; I.e., the
spectral sensitivity of the cell shall closely
approximate the standard spectral-luminos-
ity curve for photoplc vision which is refer-
enced in (b) of Table 9-1.
3.32.3 Angle of view. Check construction
geometry to ensure that the total angle of
view of the smoke plume, as seen by the
photocell, does not exceed 16*. The total
angle of view may be calculated from: e=2
tan-* d/2L, where 0=total angle of view:
d=the sum of the photocell diameter+the
diameter of the limiting aperture; and
!>=the distance from the photocell to the
limiting aperture. The limiting aperture is
the point in the path between the photocell
and the smoke plume, where the angle of
view la most restricted. In smoke generator
smoke meters tbl> is normally »n orifice
plate.
832.4 Angle of projection. Check con-
struction geometry to ensure that the total
angle of projection of the lamp on the
smoke plume does not exceed 16*. The total
angle of projection may be calculated from:
6=2 tan-1 d/2L, where 8= total angle of pro-
jection; d= the sum of the length of the
lamp filament + the diameter of the li^Mtlrg
aperture; and L= the distance from the lamp
to the limiting aperture.
3.32.5 Calibration error. Using neutral-
density filters of known opacity, check the
error between the actual response and the
theoretical linear response of the smoke
meter. This check la accomplished by first
calibrating the smoke meter according to
3.3.1 and then Inserting a series of three
neutral-density filters of nominal opacity of
20, 50, and 75 percent in the smoke meter
.pathlength. Filters callbarted within ±2 per-
cent shall be used. Care should be taken
when inserting the .filters to prevent stray
light from affecting the meter. Make a total
of five nonconsecutlve readings for each
filter. The maximum error on any one read-
Ing shall be 3 percent opacity.
3.32.6 Zero and span drift. Determine
the zero and span drift by calibrating and
operating the smoke generator In a normal
manner over a 1-hour period. The drift is
measured by checking the zero and span at
the end of this period.
3.32.7 Response time. Determine the re-
sponse time by producng the series of five
simulated 0 percent and 100 percent opacity
values and observing the time required to
reach stable response. Opacity values of 0
percent and 100 percent may be simulated
by alternately switching the power to the
light source off and on while 'the smoke
generator is not operating.
4. References.
4.1 Air Pollution Control District Rules
and Regulations, Los Angeles County Air
Pollution Control District, Regulation IV,
Prohibitions, Rule 50.
42 Waisburd, Melvin 1^ Field Operations
and Enforcement Manual for Air, tTJS. Envi-
ronmental Protection Agency, Research Tri-
angle Park, N.C., AFTD-1100. August 1S72.
pp. 4.1-4.36.
43 Condon, E. XT., and Odishaw, H., Hand-
book of Physios, McGraw-Hill Co., N.T, N.Y,
1968, Table 3.1, p. 6-62.
Ill-Appendix A-37
-------
COMPANY
LOCATION
TEST NUMBER.
DATE :
TYPE FACILITY^
CONTROL DEVICE
FIGURE 9-1
RECORD OF VISUAL DETERMINATION OF OPACITY
PAGE cf
HOURS OF OBSERVATION,
OBSERVER
OBSERVER CERTIFICATION DATE_
OBSERVER AFFILIATION
POINT OF EMISSIONS
HEIGHT OF DISCHARGE POINT
H
I
'O
(D
I
OJ
00
CLOCK TIME
J2 OBSERVER LOCATION
Distance to Discharge
Direction from Discharge
Height of Observation Point
BACKGROUND DESCRIPTION
WEATHER CONDITIONS
Mind Direction
Wind Speed
Ambient Temperature
• • ( ':
SKY CONDITIONS (clear.
overcast, % clouds, etc.) ,
PLUME DESCRIPTION '
Color
Distance Visible
OTHER INFOKttnOIl
initial
Final
SUMMARY OF AVERAGE OPACITY
Set
Number
. • ;
Time'
Start— End
Opacity • .
Sum
..' ,
Average
' v
• • \
• •• •'• • r
Readings ranged from to
,35 opacity
The source was/was not in compliance with
the time evaluation was made:
.-at
-------
FIGURE 9-2 OBSERVATION RECORD
PAGE UF
COMPANY
LOCATION
TEST NUMBER"
HATE
OBSERVER .
TYPE FACILtYY
POINT OF EMISSIONS
H
(D
3
PJ
H-
X
I
OJ
Hr.
Min.
0
1
2
3
4
5
6
7
8
9
10
M
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
0
Seconds
15
JU
4b
STEAM PLUME
(check If applicable)
Attached
Detached
COMMENTS
,-
FIGURE 9-2 G
(Cor
.COMPANY
LOCATION
TEST
DATE
•Hr.
NUMBER
Min.
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
Seconds
0
Ib
30
4b
(ch
Ai
(FR 00C.74
OBSERVATION RECORD
PAGE OF_
OBSERVER
TYPE FAClLIYY ""
POINT OF EHISSI5NT
[VR Doc.74-26160 Filed ll-ll-74;8:45 am]
-------
Method 9—Visual Determination of lh«
Opacity of EmisukM From Stattonwy
Sources
Alternate Method 1—Determination of the
Opacity of Emission* From Stationary
Sources Remotely by Udar I3'
This alternate method provides the
quantitative determination of the opacity of
an emissions plume remotely by a mobile
lidar system (laser radar Light Detection and
Ranging). The method includes procedures
for the calibration of the lidar and procedures
to be used in the field for the lidar
determination of plume opacity. The lidar is
used to measure plume opacity during either
day or nighttime hours because it contains its
own pulsed light source or transmitter. The
operation of the lidar is not dependent upon
ambient lighting conditions (light, dark, sunny
or cloudy).
The lidar mechanism or technique is
applicable to measuring phime opacity at
numerous wavelengths of laser radiation.
However, the performance evaluation and
calibration test results given in support of
this method apply only to a lidar that
employs a ruby (red light) laser [Reference
5.1].
1. Principle and Applicability
1.1 Principle. The opacity of visible
emissions from stationary sources (stacks,
roof vents, etc.) is measured remotely by a
mobile lidar (laser radar).
1.2 Applicability. This method is
applicable for the remote measurement of the
opacity of visible emissions from stationary
sources during both nighttime and daylight
conditions, pursuant to 40 CFR | 60.11(b). It is
also applicable for the calibration and
performance verification of the mobile lidar
for the measurement of the opacity of
emissions. A performance/design
specification for a basic Kdar system is also
incorporated into this method.
1.3 Definitions;
Azimuth angle: The angle in the horizontal
plane that designates where the laser beam is
pointed. It is measured from an arbitrary
fixed reference line in that plane.
Backscatter. The scattering of laser light In
a direction opposite to that of the incident
laser beam due to reflection from particulates
along the beam's atmospheric path which
may include a smoke plume.
Backscatter signal: The general term for tht
lidar return signal which results from laser
light being backscattered by atmospheric and
smoke plume particulates.
Convergence distance: The distance from
the lidar to the point of overlap of the lidar
receiver's field-of-view and the laser beam.
Elevation angle: The angle of inclination of
the laser beam referenced to the horizontal
plane.
Far region: The region of the atmosphere's
path along the lidar line-of-sight beyond or
behind the plume being measured.
Lidar Acronym for Light Detection and
Ranging.
Lidar range: The range of distance from the
Hdar to a point of interest along the lidar line-
of-sight.
Near region: The region of the atmospheric
path along the Hdar line-of-sight between the
lidar's convergence distance and the plume
being measured.
Opacity: One minus the optical
transmittance of a smoke plume, screen
target, etc.
Pick interval: The time or range intervals fan
the lidar backscatter signal whose minimum
average amplitude is used to calculate
opacity. Two pick intervals are required, ont
in the near region and one in the far region.
Plume: The plume being measured by lidar.
Plume signal: The backscatter signal
resulting from the laser light pulse passing
through a plume.
1/R* correction: The correction made for
the systematic decrease in lidar backscatter
signal amplitude with range.
Reference signal: The backscatter signal
resulting from the laser light pulse passing
through ambient air.
Sample interval: The time period between
successive samples for a digital signal or
between successive measurements for an
analog signal.
Signal spike: An abrupt momentary .
increase and decrease in signal amplitude.
Source: The source being tested by lidar.
Time reference: The time~(t0) when the
laser pulse emerges from the laser, used as
the reference in all lidar time or range
measurements.
2. Procedures.
The mobile lidar calibrated In accordance
with Paragraph 3 of this method shall use the
following procedures for remotely measuring
the opacity of stationary source emissions:
2.1 Lidar Position. The lidar shall be
positioned at a distance from the plume
sufficient to provide an unobstructed view of
the source emissions. The plume must be at a
range of at least 50 meters or three
consecutive pick intervals (whichever is
greater) from the lidar's transmitter/receiver
convergence distance along the line-of-sight.
The maximum effective opacity measurement
distance of the lidaHs a function of local
atmospheric conditions, laser beam diameter,
and plume diameter. The test position of the
lidar shall be selected so that the diameter of
the laser beam at the measurement point
within the plume shall be no larger than
three-fourths the plume diameter. The beam
diameter is calculated by Equation (AMl-1):
D(lidar)=A+R
-------
reference signals it calculated (Equation
AM1-2). For »hot-to-»hot consistency, the
opacity values shall be within ± 3% of 0%
opacity and the associated S, values less
than or equal to 8% (full scale) [Section 2.6].
If a set of reference signals fails to meet the
requirements of this section, then all plume
signals [Section 2.4] from the last set of
acceptable reference signals to the failed set
•hall be discarded.
2.3.1 Initial and Final Reference Signals.
Three reference signals shall be obtained
within a 90-second time period prior to any
data run. A final set of three reference signals
•hall be obtained within three (3) minutes
after the completion of the same data run.
2.3.2 Temporal Criterion for Additional
Reference Signals. An additional set of
reference signals shall be obtained during a
data run if there is a change in wind direction
or plume drift at 30* or more from the
direction that was prevalent when the last set
of reference signals were obtained. An
additional set of reference signals shall also
be obtained if there is a change in amplitude
in either the near or the far region of the
plume signal, that is greater than 6% of the
near signal amplitude and this change in
amplitude remains for 30 seconds or more.
2.4 Plume Signal Requirements. Once
properly aimed, the lidar is placed in
operation with the nominal pulse or firing
rate of six pulses/minute (1 pulse/10
seconds). The lidar operator shall observe the
plume backscatter signals to determine the
need for additional reference signals as
required by Section 2.3.2. The plume signals
are recorded from lidar start to stop and are
called a data run. The length of a data run is
determined by operator discretion. Short-
term stops of the lidar to record additional
reference signals do not constitute the end of
a data run if plume signals are resumed
within 90 seconds after the reference signals
have been recorded, and the total stop or
Interrupt time does not exceed 3 minutes.
2.4.1 Non-hydrated Plumes. The laser
•hall be aimed at the region of the plume
which displays the greatest opacity. The lidar
operator must visually verify that the laser is
aimed clearly above the source exit structure.
2.4.2 Hydrated Plumes. The lidar will be
used to measure the opacity of hydraterJ or
so-called steam plumes. As listed in the
reference method, there are two types, i.e.,
attached and detached steam plumes.
2.4.2.1 Attached Steam Plumes. When
condensed water vapor is present within a
plume, lidar opacity measurements shall be
made at a point within the residual plume
where the condensed water vapor is no
longer visible. The laser shall be aimed into
the most dense region (region of highest
opacity) of the residual plume.
During daylight hours the lidar operator
locates the most dense portion of the residual
plume visually. During nighttime hours a
high-intensity spotlight, night vision scope, or
low light level TV, etc., can be used as an aid
to locate the residual plume. If visual
determination is ineffective, the lidar may be
used to locate the most dense region of the
residual plume by repeatedly measuring
opacity, along the longitudinal axis or center
of the plume from the emissions outlet to a
point just beyond the steam plume. The lidar
operator should also observe color
differences and plume reflectivity to ensure
that the lidar is aimed completely within the
residual plume. If the operator does not
obtain a clear indication of the location of the
residual plume, this method shall not be used.
Once the region of highest opacity of the
residual plume has been located, aiming
adjustments shall be made to the laser line-
of-sighl to correct for the following:
movement to the region of highest opacity out
of the lidar line-of-sight (away from the laser
beam) for more than 15 seconds, expansion of
the steam plume (air temperature lowers
and/or relative humidity increases) so that it
just begins to encroach on the field-of-view of
the lidar's optical telescope receiver, or a
decrease in the size of the steam plume (air
temperature higher and/or relative humidity
decreases) so that regions within the residual
plume whose opacity is higher than the one
being monitored, are present.
2.4.2.2 Detached Steam Plumes. When the
water vapor in a hydrated plume condenses
and becomes visible at a finite distance from
the stack or source emissions outlet, the
opacity of the emissions shall be measured in
the region of the plume clearly above the
emissions outlet and below condensation of
the water vapor.
During daylight hours the lidar operators
can visually determine if the steam plume is
detached from the stack outlet. During
nighttime hours a high-intensity spotlight,
night vision scope, low light level TV, etc.,
can be used as an aid in determining if the
steam plume is detached. If visual
determination is ineffective, the lidar may be
used to determine if the steam plume is
detached by repeatedly measuring plume
opacity from the outlet to the steam plume
along the plume's longitudinal axis or center
line. The lidar operator should also observe
color differences and plume reflectivity to
detect a detached plume. If the operator doe»
not obtain a clear indication of the location of
the detached plume, this method shall not be
used to make opacity measurements between
the outlet and the detached plume.
Once the determination of a detached
steam plume has been confirmed, the laser
shall be aimed into the region of highest
opacity In the plume between the outlet and
the formation of the steam plume. Aiming
adjustments shall be made to the lidar's Line-
of-sight within the plume to correct for
changes in the location of the most dense
.region of the plume due to changes in wind
direction and speed or if the detached steam
plume moves closer to the source outlet
encroaching on the most dense region of the
plume. If the detached steam plume should '
movt too close to the source outlet for the
lidar to make interference-free opacity
measurements, this method shall not be used.
2.5 Field Records. In addition to the
recording recommendations listed in other
sections of this method the following records
should be maintained. Each plume measured
should be uniquely identified. The name of
the facility, type of facility, emission source
type, geographic location of the lidar with
respect to the plume, and phune
characteristics should be recorded. The date
of the teat, the time period that a source was
monitored, the time (to the nearest second) ol
each opacity measurement, and the sample
interval should al«o be recorded. The wind
speed, wind direction, air temperature,
relative humidity, visibility (measured at the
lidar's position), and cloud cover should be
recorded at the beginning an'd end of each
time period for a given source. A small sketch
depicting the location of the laser beam
within the plume should be recorded.
If a detached or attached steam plume is
present at the emissions source, this fact
should be recorded. Figures AMl-I and AMl-
II are examples of logbook forms that may be
used to record this type of data. Magnetic
tape or paper tape may also be used to record
data.
Ill-Appendix A-41
-------
H
H
H
I
(D
H-
X
I
4*
KJ
MDAR UK, CONTROL H'MRER T4BILATION (r«m')
(Istii* • CONTIOL NUMIER ti tick iMiviluil siiret iMir tist]
LIDAR IOC, CONTROL M^IBtH TARILATION
I,U|{ B»»L Number.
|Assi|* • CONTROl NUMIER ti tick inlivifiil siirtl n««r tut)
CONTROL
NUMIER
CONTROL
NUMIER
DITE
ASSIGNED
PROJECT
CITY. STATE
DATE
ASSISNED
PROJECT
! *ITYl STATE
CIltiMlf II lilt Plfl
Nut U| Ink Nmkir-.
Figure AM1-1 Lidar Log Control Number Tabulation
-------
i in IK i IM. or opt:imio>>
•••• ••< Ue«tUl:
im»k.T:
I.IU4K OPIH4TOITS NOTES
Ilillill Mlitili it lull III* •ittil »!•••— lltllkll |ll«l III I
tl lit fl«U lilt i
iMtttel •( 111*1:
U.
. (Itlll tlBll
Illltllll tl 11111(1.
linn " siuiee
lull iicliiilin I* iifli is «» kiiitntil is 0 I
•••MI lip* Mi (Mlilil 4>il|»tUi:
H
n>
ikinitlillllll (ilUi, iklft. HUB friiiil, «l( I :
QJ
H-
X
"** Ml ll*M»ll'l Illll
| P 1 _—
LO (!••< KKI: tl|IH
• ttllUIC TWS
li»«« tiled = lilii
I II
1' - 1"
• ITIIlt IIBIilUII:
C.nl C lil.ili. t.»Klir t>|in °. ml
• nl »l.;kllht l»|in In «n» >n
nil
I
• 1TI
l»tl
inti m«(Tio»
III! ll lilt tlllllltlll
Cililnlil i|icit|
Cilcilitil lpi(il| _^
licirlil ii fill
Sn'ci uticii imiitii I I iciiiii I I
.Till lilt iiculll II tl|l> IIICM
14 » I J I
• Itllll SIMMUII:
.Mil:
. Mil:
Figure AM1-II Lidar Log Of Operations
-------
0)
•o
Q.
(a) Reference Signal, 1/R Corrected
Convergence Point
J - •—
(Near Region)
Rn
(Far Region)
Rf
0)
Time or Range
(b) Plume Signal. 1/R2 Corrected
'Plume Spike
Time or Range
o
(a) Reference signal, l/R -corrected. This reference signal is for
plume signal (b). R , Rf are chosen to coincide with I , 1^.
r\
(b) Plume signal, 1/R -corrected. The plume spike and the decrease
in the backscatter signal amplitude in the far region are due to
the opacity of the plume. I , If are chosen as indicated in
Section 2.6.
Figure AM1-III. Plots of Lidar Backscatter Signals
Ill-Appendix A-44
-------
2.6 Opacity Calculation and Data
Analysis. Referring to the reference signal
and plume signal in Figure AMl-III. the
measured opacity (Op) in percent for each
lidar measurement is calculated using
Equation AM1-2. (O,=l-Tp; Tp is the plume
transmittance.)
(AM1-2)
where:
!„ = near-region pick interval signal'
amplitude, plume signal, 1/R* corrected.
If = far-region pick interval signal amplitude.
plume signal, 1/R1 corrected.
Rn = near-region pick interval signal
amplitude, reference signal. 1/R1
corrected, and
Rr= far-region pick interval signal amplitude,
reference signal, 1/R5 corrected.
The 1/R "correction to the plume and
reference signal amplitudes is made by
multiplying the amplitude for each successive
sample interval from the time reference, by
the square of the lidar time (or range)
associated with that sample interval
[Reference S.I].
The first step in selecting the pick intervals
for Equation AMl-2 is to divide the plume
signal amplitude by the reference signal
amplitude at the same respective ranges to
obtain a "normalized" signal. The pick
intervals selected using this normalized
signal, are a minimum of 15 m (100
nanoseconds) in length and consist of at least
S contiguous sample intervals. In addition.
the following criteria, listed in order of
importance, govern pick interval selection. (1)
The intervals shall be in a region of the
normalized signal where the reference signal
meets the requirements of Section 2.3 and is
everywhere greater than zero. (2) The
intervals (near and far) with the minimum
average amplitude are chosen. (3) If more
than one interval with the same minimum
average amplitude is found, the interval
closest to the plume is chosen. (4) The
standard deviation. S0. for the calculated
opacity shall be 8% or less. (S0 is calculated
by Equation AM1-7).
If S0 is greater than 8%. then the far pick
interval shall be changed to the next interval
of minimal average amplitude. If S, is still
greater than 8%, then this procedure is
repeated for the far pick interval. This
procedure may be repeated once again for the
near pick interval, but if S0 remains greater
than 8%, the plume signal shall be discarded.
The reference signal pick intervals. Rn and
Rf, must be chosen over the same time
I =
1 m
- I I
*
The standard deviation, S,n. of the set of
amplitudes for the near-region pick interval
In, shall be calculated using Equation
(AMl-5).
(AMl-5)
Similarly, the standard deviations Su, SRn,
and SRJ are calculated with the three
expressions in Equation (AMl-6).
fi
B--5R
Kn m ' Kni •
.
B-i
Nf m
'Rn
Rf
[I ( Rni ' Rn )21 * f
[i=l (m-1) J
I"; (R"• Rf >*]**
Li=l (m-1) J
_ I £ fi ^ I The standard deviation, S,, for ea
If I ._. ( ,. I ' associated opacity value. Op, shall I
t 1-1 im-ij J calculated using Equation (AMl-7).
for each
shall be
The calculated values of !„, I,, Rn, Rf, S|n. Sn,
Sun. SRf, Op, and S, should be recorded. Any
plume-signal with an S0 greater than 8% shall
be discarded.
2.8.1 Azimuth Angle Correction. If the
azimuth angle correction to opacity specified
in this section is performed, then the
elevation angle correction specified in
Section 2.8.2 shall not be performed. When
opacity is measured in the residual region of
an attached steam plume, and the lidar line-
(AM1-7)
of-sight is not perpendicular to the plume, it
may be necessary to correct the opacity
measured by the lidar to obtain the opacity
that would be measured on a path
perpendicular to the plume. The following
method, or any other method which produces
equivalent results, shall be used to determine
the need for a correction, to calculate the
correction, and to document the point within
the plume at which the opacity was
measured.
interval as the plume signal pick intervals, In
and I,, respectively [Figure AMI-HI). Other
methods of selecting pick intervals may be
used if they give equivalent results. Field-
oriented examples of pick interval selection
are available in Reference 5.1.
The average amplitudes for each of the
pick intervals. !„, I,. Rn, Rf, shall be calculated
by averaging the respective individual
amplitudes of the sample intervals from the
plume signal and the associated reference
signal each corrected for 1/R2. The amplitude
of In shall be calculated according to
Equation (AM-3).
»n =
'„
(AMI-3)
where:
Im = the amplitude of the ith sample interval
(near-region),
2-sum of the individual amplitudes for the
sample intervals,
m = number of sample intervals in the pick
interval, and
!„ = average amplitude of the near-region pick
interval.
Similarly, the amplitudes for Ir, Rn, and R(
are calculated with the three expressions in
Equation (AM1-4).
m
2
1=1
"fi '
(AM1-4)
(AM1-6) '
Figure AMl-tV(b) shows the geometry of
the opacity correction. L' is the path through
the plume along which the opacity
measurement is made. P' is the path
perpendicular to the plume at the same point.
The angle £ is the angle between L' and the
plume center line. The angle (ir/2-t), is the
angle between the L' and P. The measured
opacity, O,, measured along the path L' shall
be corrected to obtain the corrected opacity,
, for the path P', using Equation (AMl-8).
opc »
- op)
Cos (n/2-e)
= 1 - (1 - 0 )
p
Sin e
(AMI-8)
The correction in Equation (AMl-8) shall
be performed if the inequality in Equation
(AM1-9) is true.
e > Sin
.1 I" In (1.01 - Op)
L 1n (1 ' °p>
(AM1-9)
Figure AMl-IV(a) shows-4he geometry
used to calculate t and the position in the
plume at which the lidar measurement is
made. This analysis assumes that for a given
lidar measurement, the range from the lidar
to the plume, the elevation angle of the lidar
from the horizontal plane, and the azimuth
angle of the lidar from an arbitrary fixed
reference in the horizontal plane can all be
obtained directly.
Ill-Appendix A-45
-------
k
V
tt>
3
QJ
H-
X
Projection of P onto the yz-plane, P "
Plume measurement position P (R , «|»', p )
Stack outlet P. (R_, 0, p )
| 9 3 *
I
I
•
-1 —7
Lldar Position
••ii I/Projection of P onto th«
Plume Drift
(a)
Plume drift angle position
pa (Ra' *' * "'• PiJ • ' '
xy-plane, P '
Lidar Line-of-Sight.
Position fn
(b) P
Projection of P onto the xy-plane, P '
o a
Figure AMI - IV. Correction in Opacity for Drift of the
Residual Region of an Attached Steam Plume.
-------
R. = range .from lidar to source*
0, = elevation angle of R5*
R0 = range from lidar to plume al the opacity
measurement point*
/}„ = elevation angle of Rp*
R. = range from lidar to plume at some
arbitrary point, P., so the drift angle of
the plume can be determined*
/3, = elevation angle of R.*
a = angle between RD and R.
The correction angle t shall be determined
using Equation AM1-10.
where:
a =Cos~' (Cos/3p Cos/3. Cosa'-t-SinfiD Sin/},).
and
R'. = projection of R, in the horizontal plane
R'p = projection of Rp in the horizontal plane
R', = projection of R. in the horizontal plane
Cos -'
lnd.01 - Op)
- Op)
(AMI-13)
The measured opacity, Op. along the lidar opacity. Ope. for the actual plume (horizontal)
path L, is adjusted to obtain the corrected path. P. by using Equation (AMl-14).
V = *-
- op)
(AM1-14)
where:
/30 = lidar elevation or inclination angle,
Op=measured opacity along path L, and
Ooc=corrected opacity for the actual plume
thickness P.
The values for /}„. Op and OK should be
recorded.
'Obtained directly from lidar. These values
should be recorded.
Ill-Appendix A-47
-------
Stack's Vertical Axis
Vertical Smoke Plume
M
H
•s
V
n>
p-
x
>
*»
00
Horizontal Plane —
__ E
Lidar Line-of-Sight
Referenced to Level Ground
(Horizontal Plane)
8 , Lidar Elevation or
p Inclination Angle
pc
= Effective Plume Thickness
= Actual Plume Thickness
= LCosi-,p
= Opacity measured along path L
= Opacity value corrected to the
actual plume thickness, P
Figure AM1-V. Elevation Angle Correction for Vertical Plumes.
-------
2.6.3 Determination of Actual Plume
Opacity. Actual opacity of the plume shall be
determined by Equation AMI-IS.
pa
pc
(AMI-IS)
2.6.4 Calculation of Average Actual Plume
Opacity. The average of the actual plume
opacity. Op,, shall be calculated as the
average of the consecutive individual actual
opacity values. Op., by Equation AM1-16.
1 "
~ i
n k=l
(AM1-16)
where:
(OB.)k=the kth actual opacity value in an
averaging interval containing n opacity
values; k is a summing index.
2 = the sum of the individual actual opacity
values.
n=the number of individual actual opacity
values contained in the averaging
interval.
dM=average actual opacity calculated over
the averaging interval.
3. Lidar Performance Verification. The
lidar shall be subjected to two types of
performance verifications that shall be
peformed in the field. The annual calibration,
conducted at least once a year, shall be used
to directly verify operation and performance
of the entire lidar system. The routine
verification, conducted for each emission
source measured, shall be used to insure
proper performance of the optical receiver
and associated electronics.
3.1 Annual Calibration Procedures. Either
a plume from a smoke generator or screen
target* shall be used to conduct this
calibration.
If the screen target method is selected, five
screens shall be fabricated by placing an
opaque mesh material over a narrow frame
(wood, metal extrusion, etc.). The screen
shall have a surface area of at least one
square meter. The screen material should be
chosen for precise optical opacities of about
10,20,40, 60, and 80%. Opacity of each target
shall be optically determined and should be
recorded. If a smoke generator plume is
selected, it shall meet the requirements of
Section 3.3 of Reference Method 9. This
calibration shall be performed in the Meld
during calm (as practical) atmospheric
conditions. The lidar shall be positioned in
accordance with Section 2.1.
The screen targets must be placed
perpendicular to and coincident with the
lidar line-of-sight at sufficient height above
the ground (suggest about 30 ft) to avoid
ground-level dust contamination. Reference
signals shall be obtained just prior to
conducting the calibratfon test.
The lidar shall be aimed through the center
of the plume within 1 stack diameter of the
exit, or through the geometric center of the
screen target selected. The lidar shall be set
in operation for a 6-minute data run at a
nominal pulse rate of 1 pulse every 10
seconds. Each backscarter return signal and
each respective opacity value obtained from
the smoke generator transraissometer. shall
be obtained in temporal coincidence. The
data shall be analyzed and reduced in
accordance with Section 2.6 of this method.
This calibration shall be performed for 0%
(clean air), and at least five other opacities
(nominally 10, 20. 40, 60, and 80%).
The average of the lidar opacity values
obtained during a 6-minute calibration run
shall be calculated and should be recorded.
Also the average of the opacity values
obtained from the smoke generator
transmissometer for the same 6-minute run
shall be calculated and should be recorded.
Alternate calibration procedures that do
not meet the above requirements but produce
equivalent results may be used.
3.2 Routine Verification Procedures.
Either one of two techniques shall be used to
conduct this verification. It shall be
performed at least once every 4 hours for
each emission source measured The
following parameters shall be directly
verified.
1) The opacity value of 0% plus a minimum
of 5 (nominally 10, 20, 40, 60, and 80%)
opacity values shall be verified through the
PMT detector and data processing
electronics.
2) The zero-signal level (receiver signal
with no optical signal from the source
present) shall be inspected to insure that no
spurious noise is present in the signal. With
the entire lidar receiver and analog/digital
electronics turned on and adjusted for normal
operating performance, the following
procedures shall be used for Techniques 1
and 2, respectively.
3.2.1 Procedure for Technique 1. This test
shall be performed with no ambient or stray
light reaching the PMT detector. The narrow
band filter (694.3 nanometers peak) shall be
removed from its position in front of the PMT
detector. Neutral density filters of nominal
opacities of 10, 20, 40,60, and 80% shall be
used. The recommended test configuration is
depicted in Figure AM1-VI.
Ill-Appendix A-49
-------
PMT Entrance
Window Completely
Covered
[
Lidar Receiver
Photomultiplier
Detector
(a) Zero'-Signal Level Test
CW Laser or
Light-Emitting Diode
(Light Source)
light path
Lidar Receiver
Photomultipiier
Detector
(b) Clear-Air or 0% Opacity Test
Neutral-density
optical filter
CW Laser or
Light-Emitting Diode
(Light Source)
light path
Lidar Receiver
Photomultip!ier
Detector
(c) Optical Filter Test (simulated opacity values)
*Tests shall be performed with no ambient or stray light reaching the
detector.
figure AM1-VI. Test Configuration for Technique 1
Ill-Appendix A-50
-------
The zero-signal level shall be measured
IMC! should bo recorded, as indicated in
Figure AMl-VI(a). This simulated clear-air or
;)"u opacity value shall be tested in using the
selected light source depicted in Figure AMl-
The light source either shall be a
continuous wave (CW) laser with the beam
mechanically chopped or a light emitting
diode controlled with a pulse generator
(rectangular pulse). (A laser beam may have
to be attenuated so as not to saturate the
PMT detector). This signal level shall be
measured and should be recorded. The
opacity value is calculated by taking two pick
intervals (Section 2.6] about 1 microsecond
apart in time and using Equation (AMl-2)
setting the ratio Rn/R(=l. This calculated
value should be recorded.
The simulated clear-air signal level is also
employed in the optical test using the neutral
density filters. Using the test configuration in
Figure AMl-VI(c), each neutral density filter
shall be separately placed into the light path
from the light source to the PMT detector.
The signal level shall be measured and
should be recorded. The opacity value for
each filter is calculated by taking the signal
level for that respective Filter (I,), dividing it
by the 0% opacity signal level (!„) and
performing the remainder of the calculation
by Equation (AMl-2) with R0/R,=1. The
calculated opacity value for each filter should
be recorded.
The neutral density filters used for
Technique \ shall be calibrated for actual
opacity with accuracy of ±2% or better. This
calibration shall be done monthly while the
filters are in use and the calibrated values
should be recorded,
3.2.2 Procedure for Technique 2. An
optical generator (built-in calibration
mechanism) that contains a light-emitting
diode (red light for a lidar containing a ruby
laser) is used. By injecting an optical signal
into the lidar receiver immediately ahead of
the PMT detector, a backscatter signal is
simulated. With the entire lidar receiver
electronics turned on and adjusted for normal
operating performance, the optical generator
is turned on and the simulation signal
(corrected for 1/RJ) is selected with no plume
spike signal and with the opacity Value equal
to 0%. This simulated clear-air atmospheric
return signal is displayed on the system's
video display. The lidar operator then makes
any fine adjustments that may be necessary
to maintain the system's normal operating
range.
The opacity values of 0% and the other five
values are selected one at a time in any
order. The simulated return signal data
should be recorded. The opacity value shall
be calculated. This measurement/calculation
shall be performed at least three times for
each selected opacity value. While the order
is not important, each of the opacity values
from the optical generator shall be verified.
The calibrated optical generator opacity
value for each selection should be recorded.
The optical generator used for Technique 2
shall be calibrated for actual opacity with an
accuracy of ±1% or better. This calibration
shall be done monthly while the generator is
in use and calibrated value should be
recorded.
Alternate verification procedures that do
not meet the above requirements but produce
equivalent results may be used.
3.3 Deviation. The permissible error for
the annual calibration and routine
verification are:
3.3.1 Annual Calibration Deviation.
3.3.1.1 Smoke Generator. If the lidar
measured average opacity for each data run
is not within ±5% (full scale) of the
respective smoke generator's average opacity
over the range of 0% through 80%. then the
lidar shall be considered out of calibration.
3.3.1.2 Screens. If the lidar-measured
average opacity for each data run is not
within ±3% (full scale) of the laboratory-
determined opacity for each respective
simulation screen target over the range of 0%
through 60%, then the lidar shall be
considered out of calibration.
3.3.2 Routine Verification Error. If the
lidar-measured average opacity for each
neutral density filter (Technique 1) or optical
generator selection (Technique 2) is not
within ±3% (full scale) of the respective
laboratory calibration value then the lidar
shall be considered non-operational.
4. Performance/Design Specification for
Basic Lidar System.
4.1 Lidar Design Specification. The
essential components of the basic lidar
system are a pulsed laser (transmitter),
optical receiver, detector, signal processor.
recorder, and an aiming device that is used in
aiming the lidar transmitter and receiver.
Figure AMl-VII shows a functional block
diagram of a basic lidar system.
Ill-Appendix A-51
-------
H
H
k
H-
X
Transmitted Light Pulse)
Backscatter Return Signal
Pulsed
Laser
1 Clock 1
Narrow Band Optical Filter
Optical
Receivet
,
Aiming Device
4 1
J| 1 Video Signal
Steerabie Mount I
Signal Processor
I
Recorder
Video
Display
Ul
to
figure AM I-VII. functional Blotk Diagram of a Bosic lie/or System
-------
-1.2 Performance Evaluation Tests. The
owner of a lidar system shall subject such a
lidar system to the performance verification
tests described in Section 3. The anrSial
calibration shall be performed for three
separate, complete runs and the results of
each should be recorded. The requirements of
Section 3.3.1 must be fulfilled for each of the
three runs.
Once the conditions of the annual
calibration are fulfilled the lidar shall be
subjected to the routine verification for three
separate complete runs. The requirements of
Section 3.3.2 must be fulfilled for each of the
three runs and the results should be recorded.
The Administrator may request that the
results of the performance evaluation be
submitted for review.
5. References.
5.1 The Use of Lidar for Emissions Source
Opacity Determination, U.S. Environmental
Protection Agency, National Enforcement
Investigations Center, Denver. CO, EPA-330/
1-79-003-R, Arthur W. Dybdahl. current
edition [NTIS No. PB81-246662).
5.2 Field Evaluation of Mobile Lidar for
the Measurement of Smoke Plume Opacity,
U.S. Environmental Protection Agency.
National Enforcement Investigations Center.
Denver, CO, EPA/NEIC-TS-128, February
1976.
5.3 Remote Measurement of Smoke Plume
Transmittance Using Lidar, C. S. Cook, G. W.
Bethke. W. D. Conner (EPA/RTP). Applied
Optics 11. pg 1742, August 1972.
5.4 Lidar Studies of Stack Plumes in Rural
and Urban Environments, EPA-650/4-73-002.
October 1973.
5.5 American National Standard for the
Safe Use of Lasers ANSI Z 136.1-176. 8 March
1976.
5.6 U.S. Army Technical Manual TB MED
279. Control of Hazards to Health from Laser
Radiation, February 1969.
5.7 Laser Institute of America Laser
Safety Manual, 4th Edition.
5.8 U.S. Department of Health. Education
and Welfare. Regulations for the
Administration and Enforcement of the
Radiation Control for Health and Safety Act
of 1968. January 1976.
5.9 Laser Safety Handbook. Alex Mallow.
Leon Chabot Van Nostrand Reinhold Co..
1978.
Ill-Appendix A-53
-------
METHOD 10—DETERMINATION OF CARBOH MON-
OXIDE EMISSIONS IROM STATIONARY SOURCES 5
1. Principle and Applicability.
1.1 Principle. An Integrated or continuous
gas sample is extracted from a sampling point
and analyzed for carbon monoxide (CO) con-
tent using a'Luft-type nondlsperslve Infra-
red analyzer (NDIR) or equivalent.
1.2 Applicability. This method Is appli-
cable for the determination of carbon 'mon-
oxide emissions from stationary sources only
when specified by the test procedures for
determining compliance with new source
performance standards. The test procedure
will Indicate whether a continuous or an
integrated sample is to be used.
2. Range and sensitivity.
2.1 Range. 0 to 1,000 ppm.
22 Sensitivity. Minimum detectable con-
centration is 20 ppm for a 0 to 1,000 ppm
span.
3. Interferences. Any substance having a
strong absorption of Infrared energy will
interfere to some-extent. For example, dis-
crimination ratios for water (H.O) and car-
bon dioxide (CO,) are 3.5 percent H,O per
7 ppm CO and 10 percent CO, per 10 ppm
CO, respectively, for devices measuring in the
1.500 to 3,000 ppm range. For devices meas-
uring in the 0 to 100 ppm range, Interference
ratios can be as high as 3.5 percent H,O per
25 ppm CO and 10 percent CO, per 50 ppm
CO. The use of silica gel and ascarlte traps
will alleviate the major Interference prob-
lems. The measured gas volume must be
corrected if these traps are used.
4. Precision and accuracy.
4.1 Precision. The precision of most NDIR
analyzers' is approximately ±2 percent of
span.
4.2 Accuracy. The accuracy of most NDIR
analyzers is approximately ±5 percent of
span after calibration.
6. Apparatus.
6.1 Continuous sample (Figure 10-1).
' 5.1.1 Probe. Stainless steel or sheathed
Pyrex * glass, equipped with a filter to remove
partlculate matter. • . - -
5.1.2 Air-cooled condenser or equivalent.
To remove any excess moisture.
52 Integrated sample (Figure 10-2).
52.1 Probe. Stainless steel or sheathed
Pyrex glass, equipped with a filter to remove
partlculate matter.
522 Air-cooled, condenser or equivalent.
To remove any excess moisture.
52.3 Valve. Needle valve, or equivalent, to
to adjust flow rate.
52.4 Pump. Leak-free diaphragm type, or
equivalent, to transport gas.
52.5 Rate meter. Botameter, or equivalent,
to measure a flow range from 0 to 1.0 liter
per m\n (0.035 cfm).
52.6 Flexible bag. Tedlar, or equivalent,
with a capacity of 60 to 90 liters (2 to 3 ft >).
Leak-test the bag In the laboratory before
using by evacuating bag with- a pump fol-
lowed by a dry gas meter. When evacuation
is complete, there should be no flow through
the meter.
6.2.7 Pitot tube. Type S, or equivalent, at-
tached to the probe so that the sampling
rate can be regulated proportional to the
stack gas velocity when velocity Is varying
with the time or a sample traverse la con-
ducted. .
6.3 Analysis (Figure 10-3).
TABU 10-1.—Field data
Location.
Test _.
Date
Operator.
Comments:
Clock time
Rotameter setting, liters per minute
(cubic feet per minute)
Fljw«1W.
63.1 Carbon monoxide analyzer. Nondlsper-
slve Infrared spectrometer, or equivalent.
This Instrument should be demonstrated,
preferably by the manufacturer, to meet or
exceed ' manufacturer's specifications- and
• those described in this method.
5.3.2 Drying tube. To contain approxi-
mately 200 g of silica gel.
5.3.3 Calibration gas. Refer to paragraph
6.1.
52.4 Filter. As recommended by NDIR
manufacturer.
53.5 CO, removal tube. To contain approxi-
mately 500 g of ascarite.
5.3.6 Ice water bath. For ascarlte and silica
gel tubes.
5.3.7 Valve. Needle valve, or equivalent, to
adjust flow rate
5.3.8 Rate meter. Rotameter or equivalent
to measure gas flow rate of 0 to 1.0 liter per
mln. (0.035 cfm) through NDIR.
6.3.9 Recorder (optional). To provide per-
manent record of NDIR readings..
6. Reagents:
1 Mention of trade names or specific prod-
ucts does not constitute endorsement by the
Environmental Protection Agency.
Ffen MM. Aiuljtal MulpM.
6.1 Calibration gases. Known concentration
of CO in nitrogen (N,) for Instrument span,
prepurified grade of N] for zero, and two addi-
tional concentrations corresponding approxi-
mately to 60 percent and 30 percent span. The
.span concentration shall not exceed 1.5 times
the applicable source performance standard.
The calibration gases shall be certified by
the manufacturer to be within ±2 percent
of the specified concentration.
62 Silica gel. Indicating type, 6 to 16 mesh,
dried at 175° C (347- F) for 2 hours.
6.3 Ascarite. Commercially available.
7. Procedure.
7.1 Sampling.
7.1.1 Continuous sampling. Set up the
equipment as shown In Figure 10-1 making
sure all connections are leak free. Place too
probe in the stack at a sampling point and
purge the sampling line. Connect the ana-
lyzer and begin drawing sample into the
analyzer., Allow 5 minutes for the system
xto stabilize, then record the analyzer read*
Ing as required by the test procedure. (See
1 72 and 8). CO, content of the gas may be
determined by using the Method 3 Inte-
grated sample procedure (36 FR 24886), ot
by weighing the ascarlte CO, removal tube
and computing CO, concentration from the
gas volume sampled and the- weight gain
of the tube.
-7.12 Integrated sampling. Evacuate the
flexible bag. Set up the equipment as shown
In Figure 10-2 with the bag disconnected.
Place the probe in the stack and purge the
sampling line. Connect the bag, making sure
that all connections are leak free. Sample at
a rate proportional to the stack velocity.
CO, content of the gas may be determined
by using the Method 3 integrated sample-
procedures (36 FR 24886), or by weighing
the ascarite CO., removal tube and comput-
ing CO, concentration from the gas volume
sampled and the weight gain of the tube.
72 CO Analysis. Assemble the apparatus aa
shown In Figure- 10-3, calibrate the instru-
ment, and perform other required operations
as described in paragraph 8. Purge analyzer
with Nj prior to Introduction of each sample.
Direct the sample stream through the instru-
ment for the test period, recording the read-
ings. Check the zero and span again after tha
test to assure that any drift or malfunction
is detected. Record the sample data on Table
10-1. • .-_ .
8. Calibration. Assemble the apparatus ac-
cording to Figure 10-3. Generally an Instru-
ment requires a warm-up period before sta-
bility is obtained. Follow the manufacturer's
Instructions for specific procedure. Allow a
minimum time of one hour for warm-up.
During this time check the sample condi-
tioning apparatus, i.e., filter, condenser, dry-
ing tube, and CO> removal tube, to ensure
that each component is In good operating
condition. Zero and calibrate the instrument
according to the manufacturer's procedures
using, respectively, nitrogen and the calibra-
tion gases.
Ill-Appendix A-54
-------
9. Calculation—Concentration of carbon monoxide. Calculate the concentration of carbon
monoxide In the stack using equation 10-1.
where:
equation 10-1
Cco.,..k=concentration of CO In stack, ppm by volume (dry bads).
= concentration of CO measured by NDIR analyzer, ppm by volume (dry
basis). 6
—volume fraction of COj in sample, I.e., percent COt from Gnat analyst*
divided by 100. *., , *~
10. Bibliography-
10.1 McElroy, Frank, The Intertech NDIB-CO
Analyzer, Presented at llth Methods
•Conference on Air Pollution, University
of California, Berkeley, Calif.. April 1,
1970.
'-10 J Jacobs, M. B., et al.. Continuous Deter-
mination of Carbon Monoxide and Hy-
drocarbons In Air by a Modified Infra-
red Analyzer, -J. Air Pollution Control
Association, 9(2): 110-114, August 1959.
103 MSA LIRA Infrared Oas and Liquid
Analyzer Instruction Book, Mine Safety
Appliances Co, Technical Products Di-
vision, Pittsburgh, Fa.
10.4 Models 215A, 316A, and 416A Infrared
Analyzers, Beckman Instruments, Inc,
Beckman Instructions 1635-B, Puller-
ton, Calif, October 1967.
10.5 Continuous CO Monitoring System,
Model A5611, Intertech Corp, Princeton,
N.J.
10.6 TTNOB Infrared Gas Analyzers, Bendlz
Corp., Ronceverte, West Virginia.
ADDENDA
" A. Performance Specifications for NDIR Carbon Monoxide Analyzers.
Range (minimum). »: '., . 0—lOOOppm.
Output (minimum) '—'. 0-10mV.
Minimum detectable sensitivity—. . 20 ppm.
Rise time, 90 percent (maximum).—. 30seconds.
fall time, 90 percent (TVftgiTwuTirt). .___ 30 seconds.
Zero drift {maximum) . * 10% In 8 hours.
Span drift {rwnfiw'*") ,:. 10% in 8 hours.
Precision (minimum) : ... ± 2% of full scale.
Noise (maximum) : ± 1% of full scale.
Linearity (maximum deviation) — 2% of full scale.
Interference rejection ratio COf—1000 to 1, BiO—600 to 1.
B. Definitions of Performance Specifica-
tions.
Range—The minimum and maximum
measurement limits.
Output—Electrical signal which is propor-
tional to the measurement; intended for con-
nection to readout or data processing devices.
Usually expressed ns millivolts or milliamps
full scale at a given impedance.
Full scale—The maximum measuring limit
for a given range.
Minimum detectable sensitivity—The
smallest amount of input concentration that
can be detected as the concentration ap-
proaches zero..
Accuracy—The degree of agreement be-
tween a measured value and the true value;
usually expressed as ± percent of full scale.
Time to SO percent response—The time in-
terval from a step change In the input con-
centration at the instrument inlet to a read-
Ing of 90 percent of the ultimate recorded
concentration.
Rise Time (SO percent)—The interval be-
tween Initial response time and'time to 90
percent response after a step Increase In the
inlet concentration.
Fall Time (90 percent)—The interval be-
tween Initial response time and time to 90
percent response after a step decrease in the
Inlet concentration.
Zero Drift—The change in instrument out-
put over a stated time -period, usually 24
hours,-of unadjusted continuous operation
when the input concentration is zero; usually
expressed as percent full scale.
Span Drift—The change in Instrument out-
put over a stated time period, usually 24
hours, of unadjusted continuous operation
when the input concentration is a stated
upscale value; usually expressed as percent
full scale.
Precision—The degree of agreement be-
tween repeated measurements of the same
concentration, expressed as the average de-
viation of the single results from the mean.
Noise—Spontaneous deviations from a
mean output not caused by input concen-
tration changes.
Linearity—The maximum deviation be-
tween an actual instrument reading and the
reading predicted by a straight line drawn
between upper and lower calibration points.
Ill-Appendix A-55
-------
METHOD Jl—DETERMINATION OF HYDROGEN
SULFIDE CONTENT OF FUEL GAS STREAMS IN
PETROLEUM REFINERIES 79
1. Principle and applicability. 1.1 Princi-
ple. Hydrogen sulfide (H.S) is collected from
a source in a series of midget impingers and
absorbed in pH 3.0 cadmium sulfate (CdSO.)
solution to form cadmium sulfide (CdS).
The latter compound is then measured iodo-
metrically. An impinger containing hydro-
gen peroxide is included to remove SO, as
an Interfering species. This method is a revi-
sion of the H>S method originally published
in the FEDERAL REGISTER, Volume 39, No. 47,
dated Friday, March 8. 1974.
1.2 Applicability. This method is applica-
ble for the determination of the hydrogen
sulfide content of fuel gas streams at petro-
leum refineries.
2. Range and sensitivity. The lower limit
of detection is approximately 8 mg/m« (6
ppm). The maximum of the range Is 740
mg/m' (520 ppm).
3. Interferences. Any compound that re-
duces iodine or oxidizes iodide ion will Inter-
fere in this procedure, provide it is collected
In the cadmium sulfate impingers. Sulfur
dioxide in concentrations of up to 2.600 mg/
m' is eliminated by the hydrogen peroxide
solution. Thiols precipitate with hydrogen
sulfide. In the absence of HiS, only co-traces
of thiols are collected. When methane- and
ethane-thiols at a total level of 300 mg/m3
are present in addition to H,S, the results
vary from 2 percent low at an HiS conce'n-
tration of 400 mg/ms to 14 percent high at
an H»S concentration of 100 mg/mj. Carbon
oxysulfide at a concentration of 20 percent
does not interfere. Certain carbonyl-con-
taining compounds react with iodine and
produce recurring end points. However, ac-
etaldehyde and acetone at concentrations of
1 and 3 percent, respectively, do not inter-
fere.
Entrained hydrogen peroxide produces a
negative interference equivalent to 100 per-
cent of that of an equimolar quantity of hy-
drogen sulfide. Avoid the ejection of hydro-
gen peroxide into the cadmium sulfate im-
pingers.
4. Precision and accuracy. Collaborative
testing has shown the within-laboratory co-
efficient of variation to be 2.2 percent and
the overall coefficient of variation to be 5
percent. The method bias was shown to be
—4.8 percent when only H,S was present. In
the presence of the interferences cited in
section 3, the bias was positive at low H.S
concentrations and negative at higher con-
centrations. At 230 mg H^S/m', the level of
the compliance standard, the bias was +2.7
percent. Thiols had no effect on the preci-
sion.
5. Apparatus.
6.1 Sampling apparatus.
5.1.1 Sampling line. Six to 7 mm
-------
NOTE.—A 0.01 N phenylarslne oxide solu-
tion may be prepared instead of 0.01 N thio-
Bulfate (see section 6.3.3).
6.3.3 Phenylarslne oxide solution, stan-
dard 0.01 N. Dissolve 1.80 g of phenylarsine
oxide (C.H.AsD) in 150 ml of 0.3 N sodium
hydroxide. After settling, decant 140 ml of
this solution into 800 ml of distilled water.
Bring the solution to pH 6-7 with 6N hydro-
chloric acid and dilute to 1 liter. Standard-
ize as in section 8.1.3.
6.3.4 Starch indicator solution. Suspend
10 g of soluble starch in 100 ml of delonized,
distilled water and add 15 g of potassium
hydroxide (KOH) pellets. Stir until dis-
solved, dilute with 900 ml of delonized dis-
tilled water and let stand'for 1 hour. Neu-
tralize the alkali with concentrated hydro-
chloric acid, using an indicator paper similar
to Alkacid test ribbon, then add 2 ml of gla-
cial acetic acid as a preservative.
NOTE.—Test starch indicator solution for
decomposition by . titrating, with 0.01 N
Iodine solution, 4 ml of starch solution in
200 ml of distilled water that contains 1 g
potassium iodide. If more than 4 drops of
the 0.01 N Iodine solution are required to
obtain the blue color, a fresh solution must
be prepared.
7. Procedure.
7.1 Sampling.
7.1.1 Assemble the sampling train as
shown in figure 11-1, connecting the five
midget Impingers in series. Place 15 ml of 3
percent hydrogen peroxide solution in the
first impinger. Leave the second impinger
empty. Place 15 ml of the cadmium sulfate
absorbing solution in the third, fourth, and
fifth Impingers. Place the Impinger assem-
bly in an ice bath container and place
crushed ice around the impingers. Add more
Ice during the run, if needed.
7.1.2 Connect the rubber bulb and mano-
meter to first Impinger. as shown in figure
11-1. Close the petcock on the dry gas meter
outlet. Pressurize the train to 25-cm water
pressure with the bulb and close off tubing
connected to rubber bulb. The train must
hold a 25-cm water pressure with not more
than a 1-cm drop in pressure in a 1-minute
Interval. Stopcock grease is acceptable for
sealing ground glass joints.
NOTE.—This leak check procedure is op-
tional at the beginning of the sample run,
but Is mandatory at the conclusion. Note
also that if the pump is used for sampling, it
Is recommended (but not required) that the
pump be leak-checked separately, using a
method consistent with the leak-check pro-
cedure for diaphragm pumps outlined in
section 4.1.2 of reference method 6. 40 CFR
Part 60, Appendix A.
7.1.3 Purge the connecting line between
the sampling valve and first impinger, by
disconnecting the line from the first im-
pinger, opening the sampling valve, and al-
lowing process gas to flow through the line
for a minute or two. Then, close the sam-
pling valve and reconnect the line to the im-
pinger train. Open the petcock on the dry
gas meter outlet. Record the initial dry pa>
meter reading.
7.1.4 Open the sampling valve and then
adjust the valve to obtain a rate of approxi-
mately 1 liter/min. Maintain a constant
(±10 percent) flow rate during the test.
Record the meter temperature.
7.1.5 Sample for at least 10 mln. At the
end of the sampling time, close the sam-
pling valve and record the final volume and
temperature readings. Conduct a leak check
as described in Section 7.1.2 above.
7.1.6 Disconnect the impinger train from
the sampling line. Connect the charcoal
tube and the pump, as shown in figure 11-1.
Purge the train (at a rate of 1 liter/mini
with clean ambient air fpr 15 minutes to
ensure that all H.S is removed from the hy-
drogen peroxide. For sample recovery, cap
the open ends and remove the impinger
train to a clean area that is away from
sources of heat. The area should be well
lighted, but not exposed to direct sunlight.
7.2 Sample recovery.
7.2.1 Discard the contents of the hydro-
gen peroxide impinger. Carefully rinse the
contents of the third, fourth, and fifth im-
pingers into a 500 ml iodine flask.
...... ..... fW in. TEFLON SAMPLING," MIDGET
S IIB", LINE '' IMPINGERS
SILICA GEL TUBE
VALVE
(FOR AIR PURGE)
PUMP
Figure 11-1. H2S sampling train.
Ill-Appendix A-57
-------
NOTE.—The impingers normally have only
a thin film of cadmium sulfide remaining
"after a water rinse. If Antifoam B was not
used or if significant quantities of yellow
cadmium sulfide remain in the impingers,
the alternate recovery procedure described
below must be used.
7.2.2 Pipette exactly 50 ml of 0.01 N
Iodine solution into a 125 ml Erlenmeyer
flask. Add 10 ml of 3 M HC1 to the solution.
Quantitatively rinse the acidified" iodine
into the iodine flask. Stopper the flask im-
mediately and shake briefly.
7.2.2 (Alternate). Extract the remaining
cadmium sulfide from the third, fourth, and
fifth impingers using the acidified iodine so-
lution. Immediately after pouring the acidi-
fied iodine into an impinger, stopper it and
shake for a few moments, then transfer the
liquid to the iodine flask. Do not transfer
any rinse portion from one Impinger to an-
other, transfer it directly to the iodine flask.
Once the acidified iodine solution has been
poured into any glassware containing cadmi-
um sulfide, the container must be tightly
stoppered at all times except when adding
more solution, and this must be done as
quickly and carefully as possible. After
adding any acidified iodine solution to the
iodine flask, allow a few minutes for absorp-
tion of the H.S before adding any further
rinses. Repeat the iodine extraction until all
cadmium sulfide is removed from the im-
pingers. Extract that part of the connecting
glassware that contains visible cadmium sul-
fide.
Quantitatively rinse all of the iodine from
the impingers, connectors, and the beaker
into the iodine flask using deionized, dis-
tilled water. Stopper the flask and shake
briefly.
7.2.3 Allow the iodine flask to stand
about 30 minutes in the dark for absorption
of the H,S into the iodine, then complete
the titration analysis as in section 7.3.
NOTE.—Caution! Iodine evaporates from
acidified iodine solutions. Samples to which
jicidified iodine have been added may not be
stored, but must be analyzed in the time
schedule stated in section 7.2.3.
7.2.4 Prepare a blank by adding 45 ml of
cadmium sulfate absorbing solution to an
iodine flask. Pipette exactly 50 ml of 0.01 N
iodine solution into a 125-ml Erlenmeyer
flask. Add 10 ml of 3 M HC1. Follow the
same Impinger extracting and quantitative
rinsing procedure carried out in sample
analysis. Stopper the flask, shake briefly,
let stand 30 minutes In the dark, and titrate
with the samples.
NOTE.—The blank must be handled by ex-
actly the same procedure as that used for
the samples.
7.3 Analysis.
NOTE.—Titration analyses should be con-
rfucted at the sample-cleanup area in order
to prevent loss of iodine from the sample.
Titration should never be made in direct
sunlight.
7.3.1 Using 0.01 N sodium thiosulfate so-
lution (or 0.01 N phenylarsine oxide. If ap-
plicable), rapidly titrate each sample in an
iodine flask using gentle mixing, until solu-
tion is light yellow. Add 4 ml of starch indi-
cator solution and continue titrating slowly
until the blue color just disappears. Record
VTT. the volume of sodium thiosulfate solu-
tion used, or VAT, the volume of phenylar-
stne oxide solution used (ml).
7.3.2 Titrate the blanks in the game
manner as the samples. Run blanks each
day until replicate values agree within 0.05
ml. Average the replicate titration values
which agree within 0.05 ml.
8. Calibration and standards.
8.1 Standardizations.
8.1.1 Standardize the 0.01 N iodine solu-
tion daily as follows: Pipette 25 ml of the
iodine solution into a 125 ml Erlenmeyer
flask. Add 2 ml of 3 M HC1. Titrate rapidly
with standard 0.01 N thiosulfate solution or
with 0.01 N phenylarsine oxide until the so-
lution is light yellow, using gentle mixing.
Add four drops of starch indicator solution
and continue titrating slowly until the blue
color just disappears. Record VT, the volume
of thiosulfate solution used, or Vu, the
volume of phenylarsine oxide solution used
(ml). Repeat until replicate values agree
within 0.05 ml. Average the replicate titra-
tion values which agree within 0.05 ml and
calculate the exact normality of the iodine
solution using equation 9.3. Repeat the
standardization daily.
8.1.2 Standardize the 0.1 N thiosulfate
solution as follows: Oven-dry potassium di-
chromate (K,Cr,O,) at 180 to 200* C (360 to
390* F). Weigh to the nearest milligram, 2 g
of potassium dichromate. Transfer the di-
chromate to a 500 ml volumetric flask, dis-
solve in deionized, distilled water and dilute
to exactly 500 ml. In a 500 ml iodine flask,
dissolve approximately 3 g of potassium
iodide (KI) in 45 ml of deionized, distilled
water, then add 10 ml of 3 M hydrochloric
acid solution. Pipette 50 ml of the dichro-
mate solution into this mixture. Gently
swirl the solution once and allow It to stand
in the dark for 5 minutes. Dilute the solu-
tion with 100 to 200 ml of deionized distilled
water, washing down the sides of the flask
with part of the water. Titrate with 0.1 N
thiosulfate until the solution is light yellow.
Add 4 ml of starch indicator and continue ti-
trating slowly to a green end point. Record
V,, the volume of thiosulfate solution used
(ml). Repeat until replicate analyses agree
within 0.05 ml. Calculate the normality
using equation 9.1. Repeat the standardiza-
tion each week, or after each test series,
' whichever time is shorter.
8.1.3 Standardize the 0.01 N Phenylar-
sine oxide (if applicable) as follows: oven
dry potassium dichromate
-------
(6 eq. I,/mole K.Cr.O,) (1.000 ml/liter)/
(249.2 g K,Cr,O,/mole) (100 aliquot
factor)
0.3 Normality of Standard Iodine Solu-
tion.
N,=NTVT/V,
where:
Ni=Normality of standard Iodine solution.
g-eq/liter.
V,«=Volume of standard Iodine solution
used. ml.
NT=Normality of standard (-0,01 N) thio-
sulfate solution; assumed to be 0.1 Nt. g-
eq/liter.
VT=Volume of thiosulfate solution used. ml.
NOTE.—If phenylarsine oxide is used
intead of thiosulfate, replace NT and VT In
Equation 9.3 with NA and V«, respectively
(see sections 8.1.1 and 8.1.3).
9.4 Dry Gas Volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (20* C) and 760 nun Hg.
V.ta->=V.Y {(T^/T.) (Pu,/P«)J
where:
V»(.,d>=Volume at standard conditions of gas
sample through the dry gas meter, stan-
dard liters.
V«, = Volume of gas sample through the dry
gas meter (meter conditions), liters.
T.UI = Absolute temperature at standard con-
ditions. 293' K.
T,=Average dry gas meter temperature. 'K.
PM> = Barometric pressure at the sampling
site, mm Hg.
P.U = Absolute pressure at standard condi-
tions. 760 mm Hg.
V = Dry gas meter calibration factor.
9.5 Concentration of H>S. Calculate the
concentration of H,S in the gas stream at
standard conditions using the following
equation:
CH« = K[(V,7N,-VT,NT) sample—
(VrTN.-VrrN,) blank]/V...u.
where (metric units):
CHn- Concentration of H>S at standard con-
ditions, mg/dscm.
K = Conversion factor= 17.04x10'
(34.07 g/mole H,S> (1.000 liters/in') (1.000
mg/g>/ = ( 1.000 ml/liter) (2H.S eq/mole)
Vrr = Volume of standard Iodine solu-
tion =50.0 ml.
N, = Normality of standard iodine solution,
g-eq/liter.
VTT = Volume of standard (-0.01 N) sodium
thiosulfate solution, ml.
N, = Normality of standard sodium thiosul-
fate solution, g-eq/liter.
V.(,uji=Dry gas volume at standard condi-
tions, liters.
NOTE-'If phenylarsine oxide is used In-
stead of thiosulfate, replace NT and Vn in
Equation 9.5 with NA and VAT, respectively
(see Sections 7.3.1 and 8.1.3).
10. Stability. The absorbing solution is
stable for at least 1 month. Sample recovery
and analysis should begin within 1 hour of
sampling to minimize oxidation of the acidi-
fied cadmium sulfide. Once Iodine has been
added to the sample, the remainder of the
analysis procedure must be completed ac-
cording to sections 7.2.2 through 7.3.2.
11. Bibliography.
11.1 Determination of Hydrogen Sulfide.
Ammoniacal Cadmium Chloride Method.
API Method 772-54. In: Manual on Disposal
of Refinery Wastes, Vol. V: Sampling and
Analysis of Waste Cases and Partlculate
Matter. American Petroleum Institute,
Washington. D.C.. 1954.
11.2 Tentative Method of Determination
of Hydrogen Sulfide and Mercaptan Sulfur
in Natural Oas, Natural Oas Processors As-
sociation, Tulsa. Okla., NOPA Publication
No. 2265-65. 1965.
11.3 Knoll. J. E.. and M. R. Midgett. De-
termination of Hydrogen Sulfide in Refin-
ery Fuel Gases, Environmental Monitoring
Series, Office of Research and Develop-
ment. USEPA, Research Triangle Park, N.C.
27711. EPA 600/4-77-007.
11.4 Scheill. G. W.. and M. C. Sharp.
Standardization of Method 11 at a Petro-
leum Refinery. Midwest Research Institute
Draft Report for USEPA. Office of Re-
search and Development. Research Triangle
Park. N.C. 27711, EPA Contract No. 68-02-
1098. August 1976. EPA 600/4-77-088a
(Volume 1) and EPA 600/4-77-088b (Volume
2).
(Sees. Ill, 114. 301(a). Clean Air Act as
amended (42 U.S.C. 7411. 7414. 7601).)
Ill-Appendix A-59
-------
Method 12. Determination of Inorganic Lead
Emissions From Stationary Source* 145
1. Applicability and Principle.
1.1 Applicability. This method applies to
the determination of inorganic lead (Pb)
emissions from specified stationary sources
only.
1.2 Principle. Paniculate and gaseous Pb
emissions are withdrawn isokinetically from
the source and collected on a filter and in
dilute nitric acid. Hie collected samples are
digested in acid solution and analyzed by
atomic absorption spectrometry using an air
acetylene flame.
2. Range, Sensitivity. Precision, and
Interferences.
2.1 Range. For a minimum analytical
accuracy of ±10 percent, the lower limit of
the range is 100 fig. The upper limit can be
considerably extended by dilution.
2.2 Analytical Sensitivity. Typical
sensitivities for a 1-percent change in
absorption (0.0044 absorbance units) are 0.2
and 0.5 fig Pb/ml for the 217.0 and 283.3 nm
lines, respectively.
2.3 Precision. The within-laboratory
precision, as measured by the coefficient of
variation ranges from 0.2 to 9.5 percent
relative to a run-mean concentration. These
values were based on tests conducted at a
gray iron foundry, a lead storage battery
manufacturing plant, a secondary lead
smelter, and a lead recovery furnace of an
alkyl lead manufacturing plant. The
concentrations encountered during these
tests ranged from 0.61 to 123.3 mg Pb/m1.
2.4 Interferences. Sample matrix effects
may interfere with the analysis for Pb by
flame atomic absorption. If this interference
is suspected, the analyst may confirm the
presence of these matrix effects and
frequently eliminate the interference by using
the Method of Standard Additions.
High concentrations of copper may
interfere with the analysis of Pb at 217.0 run.
This interference can be avoided by
analyzing the samples at 283.3 nm.
3. Apparatus.
3.1 Sampling Train. A schematic of the
sampling train is shown in Figure 12-1; it is
similar to the Method 5 train. The sampling
train consists of the following components:
3.1.1 Probe Nozzle, Probe Liner. Pitot
Tube, Differential Pressure Gauge, Filter
Holder. Filter Heating System. Metering
System. Barometer, and Gas Density
Determination Equipment. Same as Method 5.
Sections 2.1.1 to 2.1.6 and 2.1.8 to 2.1.10,
. respectively.
3.1.2 Impingers. Four impingers connected
in series with leak-free ground glass fittings
or any similar leak-free noncontaminating
fittings. For the first, third, and fourth
impingers, use the Greenburg-Smith design,
modified by replacing the tip with a 1.3 cm
(Vi in.) ID glass tube extending to about 1.3
cm (VS> in.) from the bottom of the flask. For
the second impinger, use the Greenburg-
Smith design with the standard tip. Place a
thermometer, capable of measuring
temperature to within 1°C (2°F) at the outlet
of the fourth impinger for monitoring
purposes.
Ill-Appendix A-60
-------
H
(D
3
a
p-
x
CTi
a:
PITOTTUBE
TEMPERATURE SENSOR
- PROBE
TEMPERATURE
SENSOR
HEATED AREA THERMOMETER
THERMOMETER
PROBE /ff STACK
/ [J—
REVERSE-TYPE
PITOTTUBE *
\T} BY PASS VALVE
^LXISL
VACUUM
GAUGE
THERMOMETERS
MAIN VALVE
DRY GAS METER
AIRTIGHT
PUMP
CHECK
VALVE
VACUUM
LINE
Figure 12-1. Inorganic lead sampling train.
-------
3.2 Sample Recovery. The following items
are needed:
3.2.1 Probe-Liner and Probe-Nozzle
Brushes, Petri Dishes, Plastic Storage
Containers, and Funnel and Rubber
Policeman. Same as Method S, Sections 2.2.1,
2.2.4, Z.2.B, and £2.7. respectively.
S.2.Z Wash Bottles. Glass (2).
3.2.3 Sample Storage Containers.
Chemically resistant borosilicate glass
bottles, for 0.1 nitric acid (HNO,) impinger
and probe solutions and washes. lOOO-ml.
Use screw-cap liners that are either rubber-
backed Teflon* or leak-free and resistant to
chemical attack by 0.1 N HNO.. (Narrow
mouth glass bottles have been found to be
less prone to leakage.)
1.2.4 Graduated Cylinder and/or Balance
To measure condensed water to within 2 ml
or 1 a. Use a graduated cylinder that has a
minimum capacity of 500 ml and
subdivisions no greater than 5 ml. (Most
laboratory balances are capable of weighing
to the nearest 0.5 g or less.)
8.2.5 Funnel. Glass, to aid in sample
recovery.
3.3 Analysis. The following equipment is
needed:
3.3.1 Atomic Absorption
Spectrophotometer. With lead hollow
cathode lamp and burner for air/acetylene
flame.
3.3.2 Hot Plate.
3.3.3 Erlenmeyer Flasks. 125-mL 24/40 &
3.3.4 Membrane Filters. Miilipore SCWPO
4700 or equivalent.
3.3.5 Filtration Apparatus. Miilipore
vacuum filtration unit, or equivalent, far use
with the above membrane filter.
13.6 Volumetric Flasks. 100-ml. 250-ml
4. Reagents.
4.1 Sampling. The reagents used in
sampling are as follows:
4.1.1 Filter. Caiman Spectre Grade, Reeve
Angel 934 AH. MSA 1106 BH all with lot
assay for Pb, or other high-purity glass fiber
filters, without organic' binder, exhibiting at
least 99.95 percent efficiency (<0.05 percent
penetration) on 03 micron dioctyl phthalate
smoke particles. Conduct the filter efficiency
test using ASTM Standard Method D 2986-71
or use test data from the supplier's quality
control program.
4.1.2 Silica GeL Crushed Ice, and
Stopcock Grease. Same as Method 5, Section
3.1.2. 3.1.4, and 3.1.5, respectively.
4.1.3 Water. Deionized distilled, to
conform lo ASTM Specification 0 1193-74.
Type 3. If high concentrations of organic
matter are not expected lo be present, the
analyst may delete the potassium
permanganate test for oxidizable organic
matter.
4.1.4 Nitric Acid, 0.1 N. Dilute 6.5 ml of
concentrated HNO, to 1 liter with deionized
distilled water, fit may te desirable to ran
blanks before field use to eliminate a high
blank on test samples.)
4.2 Pretest Preparation. 6 N HNO, is
needed. Drhite 390 ml of concentrated HNOa
to 1 liter with deionized distilled water.
'Mention of trade names «r specific products
dots not omwKtTrte endorsement by the U.S.
Environment*! Protection Agency.
4.3 Sample Recovery, at N HNO, (same
as 4.1.4 above) te needed for (ample recovery.
4.4 Analysis. The following reagents are
needed for analysis («te ACS reagent grade
chemicals or equivalent unless otherwise
specified):
4.4.1 Water. Same as 4.14 above.
4.4.2 NhTic Acid. Concentrated.
4.4.3 Nitric Acid. SO percent (V/V). Dilute
500 ml of concentrated HNO, to 1 liter with
deionized distilled water.
4.4.4 Stock Lead Standard Solution. 1000
' fig Pb/ml. Dissolve 0.1596 g of lead nitrate
[Pb(NO,),] hi about 60 ml of deionized
distilled water, add 2 ml concentrated HNO*
and dilute to 100 ml with deionized distilled
water.
4.4.5 Working Lead Standard*. Pipet 0.0,
1.0.2.0. 3.0,4.0, and 5.0 ml of the stock lead
standard solution (4.4.4) into 250-ml
volumetric flasks. Add 5 ml of concentrated
HNO, to each flask and dilute to volume with
deionized distilled water. These working
standards contain 0.0,4.0,8.0,12.0,16.0, and
20.0 fig Pb/ml, respectively. Prepare, as
needed, additional standards at other
concentrations in a similar manner.
4.4.6 Air. Suitable quality for atomic
absorption analysis.
4.4.7 Acetylene. Suitable quality for
atomic absorption analysis.
4.4.8 Hydrogen Peroxide, 3 percent IV/V).
Dilute 10 ml of 30 percent H.O, to 100 ml with
deionized distilled water.
5. Procedure.
5.1 Sampling. The complexity of this
method is such that, in order to obtain
reliable results, testers should be trained and
experienced with the test procedures.
5.1.1 A-eiest Preparation. Follow the same
general procedure given in Method 5. Section
4.1.1, except the filter need not be weighed.
5.1.2 Preliminary Determination*. Follow
the same general procedure given in Method
5, Section 4.1.2.
5.1.3 Preparation of Collection Train.
Follow the same general procedure given in
Method 5. Section 443, except place 100 ml
of 0.1 HNO, in each of the Erst two
impingets, leave the third impinger empty.
and transfer approximately 200 to 300 g of
pre weighed silica gel from its container to the
fourth impinger. Set up the train as shown in
Figure 12-L
5.1.4 Leak-Check Procedures. Follow the
general leak-check procedures given in
Method 5. Sections 4.1.4.1. (Pretest Leak-
Check). 4.1.4.2 (Leak-Checks During the
Sample RunJ. and 4.L4J (Post-Test Leak-
Check).
5.1.5 Sampling Train Operation. Follow
the same general procedure given in Method
5, Section 4.I.S. For each ran, record toe data
required on a data sheet •noh as the one
shown in EPA Method S. Figure S-£.
5.1« Calculation of Percent Isokinetic.
Same as Method S, Section 4.1.6.
5.2 Sample Recovery. Begin proper
cleanup procedure as soon as the probe is
removed from the stack at the end of the
sampling period.
Allow the probe to cool. When ft can be
safely handled, wipe oEf all external
particulate matter near the tip of the probe
nozzle and place a cap over it. Do not cap off
the probe tip tightly while the sampling train
is cooling down as (his would create a
vacuum in the filter holder, thus drawing
liquid from the impingers into the filter.
Before moving the sampling train to the
cleanup site, remove the probe from the
sapling train, wipe off the silicon* grease, and
cap the open outlet of the probe. Be careful
not to lose any condensate that might be
present. Wipe off the silicone grease from the
glassware inlet where the probe was fastened
and cap the inlet. Remove the umbilical cord
from the last impinger and cap die impinger.
The tester may use ground-glass stoppers,
plastic caps, or serum caps to dose these
openings.
Transfer the probe and filter-unpinger
assembly to a cleanup area, which is clean
and protected from (he wind so that the
chances of contaminating or losing the
sample are minimized.
Inspect the train prior to and during
disassembly and note any abnormal
conditions. Treat the samples as follows:
5.2.1 Container No. 1 (Filter), Carefully
remove the filter from the filter holder and
place it in its identified petri dish container. If
it is necessary to fold the filter, do so such
that the sample-exposed side is inside the
fold. Carefully transfer to the petri dish any
visible sample matter and/or filter fibers that
adhere to the filter holder gasket by using a
dry Nylon bristle brush and/or a sharp-edged
blade. Seal the container.
5.2.2 Container No. 2 (Probe). Taking care
that dust on the outside of the probe or other
exterior surfaces does not get into the
sample, quantitatively recover sample matter
or any condensate from the probe nozzle.
probe fitting, probe liner, and front half of the
filter holder by washing these components
with 0.1 N HNO, and placing the wash into a
glass sample storage container. Measure and
record (to the nearest 2-ml) the total amount
of 0.1 N HNO. used for each rinse. Perform
the 0.1 N HNO1 rinses as follows:
Carefully remove the probe nozzle and
rinse the inside surfaces with 0.1 N HNO9
from a wash bottle while brushing with a
stainless steel. Nylon-bristle brush. Brush
until the 0.1 N HNO, rinse shows no visible
particles, then make a final rinse of die inside
surface.
Brush and rinse with 0.1 N HNOa the inside
parts of the Swagelok fitting in a similar way
until no visible particles remain.
Rinse the probe liner with 0.1 N HNO,.
While rotating the probe so that ull inside
surfaces will be rinsed with 0.1 N HNO.. tilt
the probe and squirt 0.1 N HNO, into its
upper end. Let the 0.1 N HNO* drain from the
lower end into the sample container. The
tester may use a glass runnel to aid in
transferring liquid washes to the container.
Follow the rinse with • probe brush. Hold the
probe in an inclined position, squirt 0.1 N
HNO. into the upper end of the probe as the
probe brash is being pushed with • twisting
action through the probe: hold the sample
container underneath the lower ead of the
probe and catch any 0.1 N HNO, and sample
matter that is brushed from the probe. Run
the brash through the probe three times or
more until no risible sample matter is carried
out with the 0.1 N HNO, and none remains on
the probe liner on visual inspection. With
Ill-Appendix A-62
-------
stainless steel or other metal probes, run the
brush through in the above prescribed
manner at least six times, since metal probes
have small crevices in which sample matter
can be entrapped. Rinse the brush with 0.1 N
HNO, and quantitatively collect these
washings in the sample container. After the
brushing make a final rinse of the probe as
described above.
It is recommended that two people clean
the probe to minimize loss of sample,
Between sampling runs, keep brushes clean
and protected from contamination.
After insuring that all joints are wiped
clean of silicone grease, brush and rinse with
0.1 N HNO, the inside of the front half of the
filter holder. Brush and rinse each suface
three times or more, if needed, to remove
visible sample matter. Make a final rinse of
the brush and filter holder. After all 0.1 N
HNOj washings and sample matter are
collected in the sample container, tighten the
lid on the sample container so that the fluid
will not leak out when it is shipped to the
laboratory. Mark the height of the fluid level
to determine whether leakage occurs during
transport. Label the container to clearly
identify its contents.
5.2.3 Container No. 3 (Silica Gel). Check
the color of the indicating silica gel to
determine if it has been completely spent and
make a notation of its condition. Transfer the
silica gel from the fourth impinger to the
original container and seal. The tester may
use a funnel to pour the silica gel and a
rubber policeman to remove the silica gel
from the impinger. It is not necessary to
remove the small amount of particles that
may adhere to the walls and are difficult to
remove. Since the gain in weight is to be used
for moisture calculations, do not use any
water or other liquids to transfer the silica
gel. If a balance is available in the field, the
tester may follow procedure for Container
No. 3 under Section 5.4 (Analysis).
5.2.4 Container No. 4 (Impingers). Due to
the large quantity of liquid involved, the
tester may place the impinger solutions in
several containers. Clean each of the first
three impingera and connecting glassware in
the following manner
1. Wipe the impinger ball joints free of
silicone grease and cap the joints.
2. Rotate and agitate each impinger, so that
the impinger contents might serve as a rinse
solution.
3. Transfer the contents of the Impingers to
a 500-ml graduated cylinder. Remove the
outlet ball joint cap and drain the contents
through this opening. Do not separate the
impinger parts (inner and outer tubes) while
transferring their contents to the cylinder.
Measure the liquid volume to within ±2 ml.
Alternatively, determine the weight of the
liquid to within ±0.5 g. Record in the log the
volume or weight of the liquid present, along
with a notation of any color or film observed
in the impinger catch. The liquid volume or
weight is needed, along with the silica gel
data, to calculate the stack gas moisture
content (see Method 5, Figure 5-3).
4. Transfer the contents to Container No. 4.
5. Note: In steps 5 and 6 below, measure
and record the total amount of 0.1 N HNO*
used for rinsing. Pour approximately 30 ml of
0.1 N HNO, into each of the first three
impingera and agitate the impingere. Drain
the 0.1 N HNO, through the outlet arm of
each impinger into Container No. 4. Repeat
this operation a second time; inspect the
impingera for any abnormal conditions.
6. Wipe the ball joints of the glassware
connecting the impingers free of silicone
grease and rinse each piece of glassware
twice with 0.1 N HNO,; transfer this rinse
into Container No. 4. (Do not rinse or brush
the glass-fritted filter support.} Mark the
height of the fluid level to determine whether
leakage occurs during transport. Label the
container to clearly identify its contents.
5.2.5 Blanks. Save 200 ml of the 0.1 N
HNO, used for sampling and cleanup as a
blank. Take the solution directly from the
bottle being used and place into a glass
sample container labeled "0.1 N HNO,
blank."
5.3 Sample Preparation.
5.3.1 Container No. 1 (Filter). Cut the filter
into strips and transfer the strips and all
loose particulate matter into a 125-ml
Erlenmeyer flask. Rinse the petri dish with 10
ml of 50 percent HNO, to insure a
quantitative transfer and add to the flask.
(Note: If the total volume required in Section
5.3.3 is expected to exceed 80 ml, use a 250-ml.
Erlenmeyer flask in place of the 125-ml flask.)
5.3.2 Containers No. 2 and No. 4 (Probe
and Impingers). (Check the liquid level in
Containers No. 2 and/or No. 4 and confirm as
to whether or not leakage occurred during
transport; note observation on the analysis
sheet. If a noticeable amount of leakage had
occurred, either void the sample or take
steps, subject to the approval of the
Administrator, to adjust the final results.)
Combine the contents of Containers No. 2
and No. 4 and take to dryness on a hot plate.
5.3.3 Sample Extraction for lead. Based on
the approximate stack gas particulate
concentration and the total volume of stack
gas sampled, estimate the total weight of
particulate sample collected. Then transfer
the residue from Containers No. 2 and No. 4
to the 125-ml Erlenmeyer flask that contains
the filter using rubber policeman and 10 ml of
50 percent HNO, for every 100 mg of sample
collected in the train or a minimum of 30 ml
of 50 percent HNO, whichever is larger.
Place the Erlenmeyer flask on a hot plate
and heat with periodic stirring for 30 min at a
temperature just below boiling. If the sample
volume falls below 15 ml, add more 50
percent HNO,. Add 10 ml of 3 percent H,O,
and continue heating for 10 min. Add 50 ml of
hot (SO'C) deionized distilled water and heat
for. 20 min. Remove the flask from the hot
plate and allow to cool. Filter the sample
through a Millipore membrane filter or
equivalent and transfer the filtrate to a 250-
ml volumetric flask. Dilute to volume with
deionized distilled water.
5.3.4 Filter Blank. Determine a filter blank
using two filters from each lot of filters used
in the sampling train. Cut each filter into
strips and place each filter in a separate 125-
ml Erlenmeyer flask. Add 15 ml of 50 percent
HNO! and treat as described in Section 5.3.3
using 10 ml of 3 percent HiO, and 50 ml of
hot, deionized distilled water. Filter and
dilute to a toal volume of 100 ml using
deionized distilled water.
5.3.5 0.1 N HNO. Blank. Take the entire
200 ml of 0.1 N HNO, to dryness on a steam
bath, add 15 ml of 50 percent HNO,. and treat
as described in Section 5.3.3 using 10 ml of 3
percent H,O, and 50 ml of hot, deionized
distilled water. Dilute to a total volume of 100
ml using deionized distilled water.
5.4 Analysis.
5.4.1 Lead Determination. Calibrate the
spectrophotometer as described in Section 6.2
and determine the absorbance for each
source sample, the filter blank, and 0.1 N
HNOi blank. Analyze each sample three
times in this manner. Make appropriate
dilutions, as required, to bring all sample Pb
concentrations into the linear absorbance
range of the spectrophotometer.
If the Pb concentration of a sample is at the
low end of the calibration curve and high
accuracy is required, the sample can be taken
to dryness on a hot plate and the residue
dissolved in the appropriate volume of water
to bring it into the optimum range of the
calibration curve.
5.4.2 Mandatory Check for Matrix Effects
on the Lead Results. The analysis for Pb by
atomic absorption is sensitive to the chemical
compositon and to the physical properties
(viscosity. pH) of the sample (matrix effects).
Since the Pb procedure described here will be
applied to many different sources, many
sample matrices will be encountered. Thus,
check (mandatory) at least one sample from
each source using the Method of Additions to
ascertain that the chemical composition and
physical properties of the sample did not
cause erroneous analytical results.
Three acceptable "Method of Additions"
procedures are described in the General
Procedure Section of the Perkin Elmer
Corporation Manual (see Citation 9.1). If the
results of the Method of Additions procedure
on the source sample do not agree within 5
percent of the value obtained by the
conventional atomic absorption analysis,
then the tester must reanalyze all samples
from the source using the Method of
Additions procedure.
5.4.3 Container No. 3 (Silica Gel). The
tester may conduct this step in the field.
Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g; record this
weight.
6. Calibration.
Maintain a laboratory log of all
calibrations.
6.1 Sampling Train Calibration. Calibrate
the sampling train components according to
the indicated sections of Method 5: Probe
Nozzle (Section 5.1); Pilot Tube (Section 5.2);
Metering System (Section 5.3); Probe Heater
(Section 5.4); Temperature Gauges (Section
5.5); Leak-Check of the Metering System
(Section 5.6); and Barometer (Section 5.7).
6.2 Spectrophotometer. Measure the
absorbance of the standard solutions using
the instrument settings recommended by the
spectrophotometer manufacturer. Repeat
until good agreement (±3 percent) is
obtained between two consecutive readings.
Plot the absorbance (y-axis) versus
concentration in fig Pb/ml (x-axis). Draw or
compute a straight line through the linear
portion of the curve. Do not force the
calibration curve through zero, but if the
curve does not pass through the origin or at
least lie closer to the origin than ±0.003
Ill-Appendix A-63
-------
absorbance units, check for incorrectly
prepared standards and for curvature in the
calibration curve.
To determine stability of the calibration
curve, run a blank and a standard after every
five samples and recalibrate, as necessary.
7. Calculations.
7.1 Dry Gas Volume. Using the data from
this test, calculate Vm(«4), the total volume of
dry gas metered corrected to standard
conditions (20*C and 760 mm Hg), by using
Equation 5-1 of Method 5. If necessary, adjust
VnUuD for leakages as outlined in Section 6.3
of Method 5. See the field data sheet for the
average dry gas meter temperature and
average orifice pressure drop.
72 Volume of Water Vapor and Moisture
Content. Using data obtained in this test and
Equations 5-2 and 5-3 of Method 5, calculate
the volume of water vapor V^^mi) and the
moisture content B,, of the stack gas.
7.3 Total Lead in Source Sample. For each
source sample correct the average
absorbance for the contribution of the filter
blank and the 0.1 N HNO, blank. Use the
calibration curve and this corrected
absorbance to determine the fig Pb
concentration in the sample aspirated into
the spectrophotometer. Calculate the total Pb
content C°n (in ;ig) in the original source
sample; correct for all the dilutions that were
made to bring the Pb concentration of the
sample into the linear range of the
spectrophotometer.
7.4 Lead Concentration. Calculate the
stack gas Pb concentration CM in mg/dscm
at follows:
i(nd)
Where:
K=0.001 mg/fig for metric units.
=2.205 lb/fig for English units.
7.5 Isokinetic Variation and Acceptable
Results. Same as Method 5, Sections 6.11 and
6.12. respectively. To calculate v.. the average
stack gas velocity, use Equation 2-9 of
Method 2 and the data from this field test.
8. Alternative Test Methods for Inorganic
Lead.
ai Simultaneous Determination of
Particulate and Lead Emissions. The tester
may use Method 5 to simultaneously
determine Pb provided that (1) he uses
acetone to remove particulate from the probe
and inside of the filter holder as specified by
Method 5, (2) he uses 0.1 N HNO, in the
impingers. (3) he uses a glass fiber filter with
a low Pb background, and (4) he treats and
analyzes the entire train contents, including
the impingers, for Pb as described in Section
5 of this method. >
8.2 Filter Location. The tester may use a
filter between the third and fourth impinger
provided that he includes the filter in the
analysis for Pb.
8.3 In-stack Filter. The tester may use an
in-stack filter provided that (1) he uses a
glass-lined probe and at least two impingers.
each containing 100 ml of 0.1 N HNO,. after
the in-stack filter and (2) he recovers and
analyzes the probe and impinger contents for
Pb. Recover sample from the nozzle with
acetone if a particulate analysis is to be
made.
9. Bibliography
9.1 Perkin Elmer Corporation. Analytical
Methods for Atomic Absorption
Spectrophotometry. Norwalk, Connecticut.
September 1976.
9.2 American Society for Testing and
Materials. Annual Book of ASTM Standards.
Part 31; Water, Atmospheric Analysis.
Philadelphia, Pa. 1974. p. 40-42.
9.3 Klein, R. and C. Hach. Standard
Additions—Uses and Limitations in
Spectrophotometric Analysis. Amer. Lab.
£21-27.1977.
9.4 Mitchell. W.J. and M.R. Midgett.
Determining Inorganic and Alkyl Lead
Emissions from Stationary Sources. U.S.
Environmental Protection Agency, Emission
Monitoring and Support Laboratory. Research
Triangle Park. N.C. (Presented at National
APCA Meeting. Houston. June 26.1978).
9.5 Same as Method 5, Citations 2 to 5
and 7 of Section 7.
*****
(Sees. 111. 114. and 301(a) of the Clean Air
Act as amended (42 U.S.C. 7411. 7414. and
7601(a)))
|FR Doc. R2-10481 Tiled t-15-81 8:45 am]
Ill-Appendix A-64
-------
Method 13A. Determination of Total Fluoride
Emissions From Stationary Sources; SPADNS
Zirconium Lake Method14'"3
1. Applicability and Principle
1.1 Applicability. This method applies to
the determination of fluoride (F) emissions
from sources as specified in the regulations. It
does not measure fluorocarbons, such aa
fa-eons.
1.2 Principle. Caseous and paniculate F
are withdrawn isokinetically from the source
and collected in water and on a filter. The
total F is then determined by the SPADNS
Zirconium Lake colorimetric method.
2. Range and Sensitivity
The range of this method is 0 to 1.4 pg F/
ml. Sensitivity has not been determined.
3. Interferences
Large quantities of chloride will interfere
with the analysis, but this interference can be
prevented by adding silver sulfate into the
distillation flask (see Section 7.3.4J. If
chloride ion is present, it may be easier to use
the Specific Ion Electrode Method (Method
13B). Grease on sample-exposed surfaces
may cause low F results due to adsorption.
4. Precision, Accuracy, and Stability
4.1 Precision. The following estimates
are based on a collaborative test done at a
primary aluminum smelter. In the test, six
laboratories each sampled the stack
simultaneously using two sampling trains for
a total of 12 samples per sampling run.
Fluoride concentrations encountered during
the test ranged from 0.1 to 1.4 mg F/m3. The
within-laboratory and between-laboratory
standard deviations, which include sampling
and analysis errors, were 0.044 mg F/m3 with
60 degrees of freedom and 0.064 mg F/ms
with five degrees of freedom, respectively.
4.2 Accuracy. The collaborative test did
not Find any bias in the analytical method.
4.3 Stability. After the sample and
colorimetric reagent are mixed, the color
formed is stable for approximately 2 hours. A
3°C temperature difference between the
sample and standard solutions produces an
error of approximately 0.005 mg F/liter. To
avoid this error, the absorbances of the
sample and standard solutions must be
measured at the same temperature.
5. Apparatus
5.1 Sampling Train. A schematic of the
sampling train is shown in Figure 13A-1; it is
similar to the Method 5 train except the filter
position is interchangeable. The sampling
train consists of the following components:
5.1.1 Probe Nozzle, Pilot Tube,
Differential Pressure Gauge, Filter Heating
System, Metering System, Barometer, and
Gas Density Determination Equipment.
Same as Method 5, Sections 2.1.1, 2.1.3, 2.1.4,
2.1.6, 2.1.8, 2.1.9, and 2.1.10. When moisture
condensation is a problem, the filter heating
system is used.
5.1.2 Probe Liner. Borosilicate glass or
316 stainless steel. When the filter is located
immediately after the probe, the tester may
use a probe heating system to prevent filter
plugging resulting from moisture
condensation, but the tester shall not allow
the temperature in the probe to exceed
120±14°C (248±25°F).
5.1.3 Filter Holder. With positive seal
against leakage from the outside or around
the filter. If the filter is located between the
probe and first impinger, use borosilicate
glass or stainless steel with a 20-mesh
stainless steel screen filter support and a
silicone rubber gasket; do not use a glass frit
or a sintered metal filter support. If the filler
is located between the third and fourth
impingers, the tester may use borosilicate
glass with a glass frit filter support and a
silicone rubber gasket. The tester may also
use other materials of construction with
approval from the Administrator.
5.1.4 Impingers. Four impingers
connected as shown in Figure 13A-1 with
ground-glass (or equivalent), vacuum-tight
fittings. For the first, third, and fourth
impingers, use the Greenburg-Smith design,
modified by replacing the tip with a 1.3-cm-
inside-diameter (V4 in.) glass tube extending
to 1.3 cm (V: in.) from the bottom of the flask.
For the second impinger, use a Greenburg-
Smith impinger with the standard tip. The
tester may use modifications (e.g., flexible
connections between the impingers or
materials other than glass), subject to the
approval of the Administrator. Place a
thermometer, capable of measuring
temperature to within 1°C (2°F), at the outlet
of the fourth impinger for monitoring
purposes.
5.2 Sample Recovery. The following
items are needed:
5.2.1 Probe-Liner and Probe-Nozzle
Brushes, Wash Bottles, Graduated Cylinder
and/or Balance, Plastic Storage Containers,
Rubber Policeman, Funnel. Same as Method
5, Sections 2.2.1 to 2.2.2 and 2.2.5 to 2.2.8,
respectively.
5.2.2 Sample Storage Container. Wide-
mouth, high-density-polyethylene bottles for
impinger water samples, 1-liter.
5.3 Analysis. The following equipment is
needed:
5.3.1 Distillation Apparatus. Glass
distillation apparatus assembled as shown in
Figure 13A-2.
5.3.2 Bunsen Burner.
5.3.3 Electric Muffle Furnace. Capable of
heating to 600°C.
5.3.4 Crucibles. Nickel, 75- to 100-ml.
5.3.5 Beakers. 500-ml and 1500-ml.
5.3.6 Volumetric Flasks. 50-ml.
5.3.7 Erlenmeyer Flasks.or Plastic Bottles.
500-ml.
5.3.8 Constant Temperature Bath.
Capable of maintaining a constant
temperature of ±1.0°C at room temperature
conditions.
5.3.9 Balance. 300-g capacity to measure
to ±0.5 g.
5.3.10 Spectrophotometer. Instrument
that measures absorbance at 570 run and
provides at least a 1-cm light path.
5.3.11 Spectrophotometer Cells. 1-cm
pathlength.
6. Reagents
6.1 Sampling. Use ACS reagent-grade
chemicals or equivalent, unless otherwise
specified. The reagents used in sampling are
as follows:
6.1.1 Filters.
6.1.1.1 If the filter is located between the
third and fourth impingers, use a Whatman '
No. 1 filter, or equivalent, sized to fit the filter
holder.
1 Mention of company or product names doei not
constitute endorsement by the U.S. Environmental
Protection Agency.
Ill-Appendix A-65
-------
TEMPERATURE
SENSOR
I I 1
STACK WALL « OPTIONAL FILTER
L~-"~ iHOLOER LOCATION;
' PROBE J
3 .if >
THERMOMETER
AIR TIGHT PUMP
DRV TEST METER
Figure 13A 1. Fluoride sampling train.
CONNECTING TUBE •
12-mm ID
{24/40
THERMOMETER
£—124/40
CONDENSER
CHECK VALVE
VACUUM LINE
VACUUM GAUGE
Figure 13A-2. Fluoride distillation apparatus.
Ill-Appendix A-66
-------
6.1.1.2 If the filter is located between the
probe and first impinger, use any suitable
medium (e.g., paper.organic membrane) that
conforms to the following specifications: (1)
The filter can withstand prolonged exposure
to temperatures up to 135°C (275°F). (2) The
filter has at least 95 percent collection
efficiency (<5 percent penetration) for 0.3 /xm
dioctyl phlhalate smoke particles. Conduct
the filter efficiency test before the test series.
using ASTJvi Standard Method D 2986-71, or
use test data from the supplier's quality
control program. (3) The filter has a low F
blank value (<0.015 mg F/cm'of filter area).
Before the test series, determine the average
F blank value of at least three filters (from
the lot to be used for sampling) using the
applicable procedures described in Sections
7.3 and 7A of this method. In general, glass
fiber filters have high and/or variable F
blank values, and will not be acceptable for
I^Q r
use. '"
6.1.2 Water. Deionized distilled, to
conform to ASTM Specification D 1193-74,
Type 3. If high concentrations of organic
matter are-not expected to be present, the
analyst may delete the potassium
permanganate test for oxidizable organic
matter.
6.1.3 Silica Gel, Crushed Ice. and
Stopcock Grease. Same as Method 5,
Section 3.1.2, 3.1.4. and 3.1.5, respectively.
6.2 Sample Recovery. Water, from same
container as described in Section 6.1.2, is
needed for sample recovery.
6.3 Sample Preparation and Analysis.
The reagents needed for sample preparation
and analysis are as follows:
6.3.1 Calcium Oxide (CaO). Certified
grade containing 0.005 percent F or less.
6.3.2 Phenolphthalein Indicator.
Dissolve 0.1 g of phenolphthalein in a mixture
of 50 ml of 90 percent ethanol and SO ml of
deionized distilled water.
6.3.3 Silver Sulfate (Ag,SO«).
6.3.4 Sodium Hydroxide (NaOH).
Pellets.
6.3.5 Sulfuric Acid (I-USO.), Concentrated.
6.3.6 Sulfuric Acid, 25 percent (V/V).
Mix 1 part of concentrated H.SO, with 3
parts of deionized distilled water.
6.3.7 Filters. Whatman No. 541. or
equivalent.
6.3.8 Hydrochloric Acid (HC1).
Concentrated.
6.3.9 Water. From same container as
described in Section 6.1.2.
6.3.10 Fluoride Standard Solution. 0.01 mg
F/ml. Dry in an oven at 110'C for at least 2
hours. Dissolve 0.2210 g of NaF in 1 liter of
deionized distilled water. Dilute 100 ml of this
solution to 1 liter with deionized distilled
water.
6.3.11 SPADNS Solution |4, 5 dihydroxy-3-
(p-8uIfophenylazo)-2.7-naphthalene-disulionic
acid trisodium salt]. Dissolve 0.960 ± 0.010
g of SPADNS reagent in SCO ml deionized
distilled water. If stored in a well-sealed
bottle protected from the sunlight, this
solution is stable for at least 1 month.
6.3.12 Spectrophotometer Zero Reference
Solution. Prepare daily. Add 10 ml of
SPADNS solution (6.3.11) to 100 ml deionized
distilled water, and acidify with a solution
prepared by diluting 7 ml of concentrated HC1
to 10 ml with deionized distilled water.
6.3.13 SPADNS Mixed Reagent. Dissolve
0.135 ± 0.005 g of zirconyl chloride
octahydrate (ZrOCU. 8H,O) in 25 ml of
deionized distilled water. Add 350 ml of
concentrated HC1. and dilute to 500 ml with
deionized distilled water. Mix equal volumes
of this solution and SPADNS solution to form
a single reagent. This reagent is stable for at
least 2 months.
7. Procedure
7.1 Sampling. Because of the complexity
of this method, testers should be trained and
experienced with the test procedures to
assure reliable results.'"
7.1.1 Pretest Preparation. Follow the
general procedure given in Method 5, Section
4.1.1, except the filter need not be weighed.
- 7.1.2 Preliminary Determinations.
Follow the general procedure given in
Method 5, Section 4.1.2., except the nozzle
size selected must maintain isokinetic
sampling rates below 28 liters/min (1.0 cfm).
7.1.3 Preparation of Collection Train.
Follow the general procedure given in
Method 5, Section 4.1.3, except for the
following variations:
Place 100 ml of deionized distilled water in
each of the first two impingers, and leave the
third impinger empty. Transfer approximately
200 to 300 g of preweighed silica gel from its
container to the fourth impinger.
Assemble the train as shown in Figure
13A-1 with the filter between the third and
fourth impingers. Alternatively, if a 20-mesh
stainless steel screen is used for the filter
support, the tester may place the filter
between the probe and first impinger. The
tester may also use a filter heating system to
prevent moisture condensation, but shall not
allow the temperature around the filter holder
to exceed 120 + 1
-------
Rinse the inside surface of each of the first
three impingers (and connecting glassware]
three separate times. Use a small portion of
deionized distilled water for each rinse, and
brush each sample-exposed surface with a
Nylon bristle brush, to ensure recovery of
fine particulate matter. Make a final rinse of
each surface and of the brush.
After ensuring that all joints have been
wiped clean of the silicone grease, brush and
rinse with deionized distilled water the inside
of the filter holder (front-half only, if filter is
positioned between the third and fourth
impingers). Brush and rinse each surface
three times or more if needed. Make a final
rinse of the brush and filter holder.
After all water washings and particulate
matter have been collected in the sample
container, tighten the lid so that water will
not leak out when it is shipped to the
laboratory. Mark the height of the fluid level
to determine whether leakage occurs during
transport. Label the container clearly to
identify its contents.
7.2.2 Container No. 2 (Sample Blank).
Prepare a blank by placing an unused filter in
a polyethylene container and adding a
volume of water equal to the total volume in
Container No. 1. Process the blank in the
same manner as for Container No. 1.
7.2.3 Container No. 3 (Silica Gel). Note
the color of the indicating silica gel to
determine whether it has been completely
spent and make a notation of its condition.
Transfer the silica gel from the fourth
impinger to its original container and seal.
The tester may use a funnel to pour the silica
gel and a rubber policeman to remove the
silica gel from the impinger. It is not
necessary to remove the small amount of dust
particles that may adhere to the impinger
wall and are difficult to remove. Since the
gain in weight is to be used for moisture
calculations, do not use any water or other
liquids to transfer the silica gel. If a balance
is available in the field, the tester may follow
the analytical procedure for Container No. 3
in Section 7.4.2.
7.3 Sample Preparation and Distillation.
(Note the liquid levels in Containers No. 1
and No. 2 and confirm on the analysis sheet
whether or not leakage occurred during
transport. If noticeable leakage had occurred,
either void the sample or use methods,
subject to the approval of the Administrator,
to correct the final results.) Treat the contents
of each sample container as described below:
7.3.1 Container No. 1 (Probe, Filter, and
Impinger Catches). Filter this container's
contents, including the sampling filter,
through Whatman No. Ml filter paper, or
equivalent, into a'l500-ml beaker.
7.3.1.1 If the filtrate volume exceeds 900
ml, make the filtrate basic (red to
phenolphthalein) with NaOH, and evaporate
to less than 900 ml.
7.3.1.2 Place the filtered material
(including sampling filter) in a nickel crucible,
add a few ml of deionized distilled water,
and macerate the filters with a glass rod.
Add 100 mg CaO to the crucible, and mix
the contents thoroughly to form a slurry. Add
two drops of phenolphthalein indicator. Place
the crucible in a hood under infrared lamps
or on a hot plate at low heat. Evaporate the
water completely. During the evaporation of
the water, keep the slurry basic (red to
phenolphthalein) to avoid loss of F. If the
indicator turns colorless (acidic) during the
evaporation, add CaO until the color turns
red again.
After evaporation of the water, place the
crucible on a hot plate under a hood and
slowly increase the temperature until the
Whatman No. Ml and sampling filters char. It
may take several hours to completely char
the filters.
Place the crucible in a cold muffle furnace.
Gradually (to prevent smoking) increase the
temperature to 600°C, and maintain until the
contents are reduced to an ash. Remove the
crucible from the furnace and allow to cool.
Add approximately 4 g of crushed NaOH to
the crucible and mix. Return the crucible to
the muffle furnace, and fuse the sample for 10
minutes at 600°C.
Remove the sample from the furnace, and
cool to ambient temperature. Using several
rinsings of warm deionized distilled water,
transfer the contents of the crucible to the
beaker containing the filtrate. To assure
complete sample removal, rinse finally with
two 20-ml portions of 25 percent H2SO4, and
carefully add to the beaker. Mix well, and
transfer to a 1-liter volumetric flask. Dilute to
volume with deionized distilled water, and
mix thoroughly. Allow any undissolved solids
to settle.
7.3.2 Container No. 2 (Sample Blank).
Treat in the same manner as described in
Section 7.3.1 above.
7.3.3 Adjustment of Acid/Water Ratio in
Distillation Flask. (Use a protective shield
when carrying out this procedure.) Place 400
ml of deionized distilled water in the
distillation flask, and add 200 ml of
concentrated HaSO4. (Caution: Observe
standard precautions when mixing HaSO4
with water. Slowly add the acid to the flask
with constant swirling.) Add some soft glass
beads and several small pieces of broken
glass tubing, and assemble the apparatus as
shown in Figure 13A-2. Heat the flask until it
reaches a temperature of 175°C to adjust the
acid/water ratio for subsequent distillations.
Discard the distillate.
7.3.4 Distillation. Cool the contents of
the distillation flask to below 80°C. Pipet an
aliquot of sample containing less than 10.0 mg
F directly into the distillation flask, and add
deionized distilled water to make a total
volume of 220 ml added to the distillation
flask. (To estimate the appropriate aliquot
size, select an aliquot of the solution and
treat as described in Section 7.4.1. This will
be an approximation of the F content because
of possible interfering ions.) Note: If the
sample contains chloride, add 5 mg of Ag2SO«
to the flask for every mg of chloride.
Place a 250-ml volumetric flask at the
condenser exit. Heat the flask as rapidly as
possible with a Bunsen burner, and collect all
the distillate up to 175"C. During hearup, play
the burner flame up and down the side of the
flask to prevent bumping. Conduct the
distillation as rapidly as possible (15 minutes
or less). Slow distillations have been found to
produce low F recoveries. Caution: Be careful
not to exceed 175°C to avoid causing H,SO«
to distill over.
If F distillation in the mg range is to be
followed by a distillation in the fractional mg
range, add 220 ml of deionized distilled water
and distill it over as in the acid adjustment
step to remove residual F from the distillation
system.
The tester may use the acid in the
distillation flask until there is carry-over of
interferences or poor F recovery. Check for
these every tenth distillation using a
deionized distilled water blank and a
standard solution. Change the acid whenever
the F recovery is less than 90 percent or the
blank value exceeds 0.1 jig/ml.
7.4 Analysis.
7.4.1 Containers No. 1 and No. 2. After
distilling suitable aliquots from Containers
No. 1 and No. 2 according to Section 7.3.4,
dilute the distillate in the volumetric flasks to
exactly 250 ml with deionized distilled water,
and mix thoroughly. Pipet a suitable aliquot
of each sample distillate (containing 10 to 40
fig F/ml) into a beaker, and dilute to 50 ml
with deionized distilled water. Use the same
aliquot size for the blank. Add 10 ml of
SPADNS mixed reagent (6.3.13), and mix
thoroughly.
After mixing, place the sample in_a
constant-temperature bath containing the
standard solutions (see Section 8.2) for 30
minutes before reading the absorbance on the
spectrophotometer.
Set the spectrophotometer to zero
absorbance at 570 nm with the reference
solution (6.3.12), and check the
spectrophotometer calibration with the
standard solution. Determine the absorbance
of the samples, and determine the
concentration from the calibration curve. If
the concentration does not fall within the
range of the calibration curve, repeat the
procedure using a different size aliquot.
7.4.2 Container No. 3 (Silica Gel). Weigh
the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g using a balance.
The tester may conduct this step in the field.
A Calibration
Maintain a laboratory log of all
calibrations.
8.1 Sampling Train. Calibrate the
sampling train components according to the
indicated sections in Method 5: Probe Nozzle
(Section 5.1); Pitot Tube (Section 5.2);
Metering System (Section 5.3); Probe heater
(Section 5.4); Temperature Gauges (Section
6.5); Leak Check of Metering System (Section
5.6); and Barometer (Section 5.7).
8.2 Spectrophotometer. Prepare the
blank standard by adding 10 ml of SPADNS
mixed reagent to 50 ml of deionized distilled
water. Accurately prepare a series of
standards from the 0.01 mg F/ml standard
fluoride solution (6.3.10) by diluting 0, 2,4,6,
8,10,12, and 14 ml to 100 ml with deionized
distilled water. Pipet 50 ml from each solution
and transfer each to a separate 100-ml
beaker. Then add 10 ml of SPADNS mixed
reagent to each. These standards will contain
0,10, 20, 30, 40 50,60, and 70 fig F (0 to 1.4 fig/
ml], respectively.
After mixing, place the reference standards
and reference solution in a constant
temperature bath for 30 minutes before
reading the absorbance with the
spectrophotometer. Adjust all samples to this
same temperature before analyzing.
Ill-Appendix A-68
-------
With the spectrophotometer at 570 nm, use
the reference solution (6.3.12) to set the
absorbance to zero.
Determine the absorbance of the
standards. Prepare a calibration curve by
plotting fig F/50 ml versus absorbance on
linear graph paper. Prepare the standard
curve initially and thereafter whenever the
SPADNS mixed reagent is newly made. Also,
run a calibration standard with each set of
samples and if it differs from the calibration
curve by ±2 percent, prepare a new standard
curve.
9. Calculations
Carry out calculations, retaining at least
one extra decimal figure beyond that of the
acquired data. Round off figures after final
calculation. Other forms of the equations may
be used, provided that they yield equivalent
results.
9.1 Nomenclature.
A
-------
Method 13B. Determination of Total Fluoride
Emissions From Stationary Sources; Specific
Ion Electrode Method14'"3
1. Applicability and Principle
1.1 Applicability. This method applies to
the determination of fluoride (F) emissions
from stationary sources as specified in the
regulations. It does not measure
fluorocarbons. such as freons.
1.2 Principle. Gaseous and paniculate F
are withdrawn isokinetically from the source
and collected in water and on a filter. The
total F is then determined by the specific ion
electrode method.
2. Range and Sensitivity
The range of this method is 0.02 to 2.000 fig
F/ml; however, measurements of less than 0.1
Mg F/ml require extra care. Sensitivity has
not been determined.
3. Interferences
Crease on sample-exposed surfaces may
cause low F results because of adsorption.
4. Precision and Accuracy
4.1 Precision. The following estimates
are based on a collaborative test done at a
primary aluminum smelter. In the test, six
laboratories each sampled the stack
simultaneously using two sampling trains for
a total of 12 samples per sampling run.
Fluoride concentrations encountered during
the test ranged from 0.1 to 1.4 mg F/ms. The
within-laboratory and between-laboratory
standard deviations, which include sampling
and analysis errors, are 0.037 mg F/m3 with
60 degrees of freedom and 0.056 mg F/m9
with five degrees of freedom, respectively.
4.2 Accuracy. The collaborative test did
not find any bias in the analytical method.
5. Apparatus
5.1 Sampling Train and Sample Recovery.
Same as Method 13A, Sections 5.1 and 5.2.
respectively.
5.2 Analysis. The following items are
needed:
5.2.1 Distillation Apparatus, Bunsen
Burner, Electric Muffle Furnace, Crucibles.
Beakers, Volumetric Flasks. Erlenmeyer
Flasks or Plastic Bottles. Constant
Temperature Bath, and Balance. Same as
Method 13A, Sections 5.3.1 to 5.3.9,
respectively, except include also 100-cnl
polyethylene beakers.
5.2.2 Fluoride Ion Activity Sensing
Electrode.
5.2.3 Reference Electrode. Single
junction, sleeve type.
5.2.4 Electrometer. A pH meter with
millivolt-scale capable of ±0.1-mv resolution.
or a specific ion meter made specifically for
specific ion use.
5.2.5 Magnetic Stirrer and TFE *
Fluorocarbon-Coated Stirring Bars.
'Mention of any trade name or specific product
does not constitute endorsement by the U.S.
Environmental Protection Agency. 123
6. Reagents
6.1 Sampling and Sample Recovery.
Same as Method 13A. Sections 6.1 and 6.2.
respectively.
6.2 Analysis. Use ACS reagent grade
chemicals (or equivalent), unless otherwise
specified. The reagents needed for analysis
are as follows:
6.2.1 Calcium Oxide (CaO). Certified
grade containing 0.005 percent F or less.
6.2.2 Phenolphthalein Indicator.
Dissolve 0.1 g of phenolphthalein in a mixture
of 50 ml of 90 percent ethanol and 50 ml
deionized distilled water.
6.2.3 Sodium Hydroxide (N'aOH).
Pellets.
6.2.4 Sulfuric Acid (HZSO<). Concentrated.
6.2.5 Filters. Whatman No. 541. or
equivalent.
6.2.6 Water. From same container as
6.1.2 of Method 13A.
6.2.7 Sodium Hydroxide. 5 M. Dissolve
20 g of NaOH in 100 ml of deionized distilled
water.
6.2.8 Sulfuric Acid. 25 percent (V/V).
Mix 1 part of concentrated HjSO, with 3
parts of deionized distilled water.
6.2.9 Total Ionic Strength Adjustment
Buffer (T1SAB). Place approximately 500 ml
of deionized distilled water in a 1-liter
beaker. Add 57 ml of glacial acetic acid, 58 g
of sodium chloride, and 4 g of cyclohexylene
dinitrilo tetraacetic acid. Stir to dissolve.
Place the beaker in a water bath to cool it
Slowly add 5 M NaOH to the solution,
measuring the pH continuously with a
calibrated pH/reference electrode pair, until
the pH is 5.3. Cool to room temperature. Pour
into a 1-liter volumetric flask, and dilute to
volume with deionized distilled water.
Commercially prepared TISAB may be
substituted for the above.
6.2.10 Fluoride Standard Solution. 0.1 M.
Oven dry some sodium fluoride (NaF) for a
minimum of 2 hours at 110°C, and store in a
desiccator. Then add 4.2 g of NaF to a 1-liter
volumetric flask, and add enough deionized
distilled water to dissolve. Dilute to volume
with deionized distilled water.
7. Procedure
7.1 Sampling, Sample Recovery, and
Sample Preparation and Distillation. Same
as Method 13A, Sections 7.1, 7.2, and 7.3,
respectively, except the notes concerning
chloride and sulfate interferences are not
applicable.
7.2 Analysis.
7.2.1 Containers No. 1 and No. 2. Distill
suitable aliquots from Containers No. 1 and
No. 2. Dilute the distillate in the volumetric
flasks to exactly 250 ml with deionized
distilled water and mix thoroughly. Pipet a
25-ml aliquot from each of the distillate and
separate beakers. Add an equal volume of
TISAB, and mix. The sample should be at the
same temperature as the calibration
standards when measurements are made. If
ambient laboratory temperature fluctuates
more than ±2°C from the temperature at
which the calibration standards were
measured, condition samples and standards
in a constant-temperature bath before
measurement. Stir the sample with a
magnetic stirrer during measurement to
minimize electrode response time. If the
stirrer generates enough heat to change
solution temperature, place a piece of
temperature insulating material such as cork,
between the stirrer and the beaker. Hold
dilute samples (below 10" 4M fluoride ion
content) in polyethylene beakers during
measurement. '
Insert the fluoride and reference electrodes
into the solution. When a steady millivolt
reading is obtained, record it. This may take
several minutes. Determine concentration
from the-calibration curve. Between electrode
measurements, rinse the electrode with -
deionized distilled water. '"
7.2.2 Container No. 3 (Silica Gel). Same
as Method 13A. Section 7.4.2.
8. Calibration
Maintain a laboratory log of all
calibrations.
8.1 Sampling Train. Same as Method
13A.
8.2 Fluoride Electrode. Prepare fluoride
standardizing solutions by serial dilution of
the 0.1 M fluoride standard solution. Pipet 10
ml of 0.1 M fluoride standard solution into a
100-ml volumetric flask, and make up to the
mark with deionized distilled water for a 10"*
M standard solution. Use 10 ml of 10"» M
solution to make a 10"s M solution in the
same manner. Repeat the dilution procedure
and make 10"4and 10'5solutions.
Pipet 50 ml of each standard into a
separate beaker. Add 50 ml of TISAB to each
beaker. Place the electrode in the most dilute
standard solution. When a steady millivolt
reading is obtained, plot the value on the
linear axis of semilog graph paper versus
concentration on the log axis. Plot the
nominal value for concentration of the
standard on the log axis, e.g., when 50 ml of
10" 2M standard is diluted with 50 ml of
TISAB, the concentration is still designated
"10-2M."
Between measurements soak the fluoride
sensing electrode in deionized distilled water
for 30 seconds, and then remove and blot dry.
Analyze the standards going from dilute to
concentrated standards. A straight-line
calibration curve will be obtained, with
nominal concentrations of 10"', 10"*, 10"*,
and 10"' fluoride molarity on the log axis
plotted versus electrode potential (in mv) on
the linear scale. Some electrodes may be
slightly nonlinear between 10"* and 10"4 M. If
this occurs, use additional standards between
these two concentrations.
Calibrate the fluoride electrode daily, and
check it hourly. Prepare fresh fluoride
standardizing solutions daily (10"*M or less).
Store fluoride standardizing solutions in
polyethylene or polypropylene containers.
(Note: Certain specific ion meters have been
designed specifically for fluoride electrode
use and give a direct readout of fluoride ion
concentration. These meters may be used in
lieu of calibration curves for fluoride
measurements over narrow concentration
ranges. Calibrate the meter according to the
manufacturer's instructions.)
Ill-Appendix A-70
-------
9. Calculations
Carry out calculations, retaining at least
one extra decimal figure beyond that of the
acquired data. Round off figures after final
calculation.
0.1 Nomenclature. Same as Method 13A,
Section 9.1. In addition:
M = F concentration from calibration curve,
molarity.
9.2 Average Dry Gas Meter Temperature
and Average Orifice Pressure Drop, Dry Gas
Volume, Volume of Water Vapor and
Moisture Content, Fluoride Concentration in
Stack Gas, and Isokinetic Variation and
Acceptable Results. Same as Method 13 A, .
Section 9.2 to 9.4, 9.5.2, and 9.6, respectively. 3
9.3 Fluoride in Sample. Calculate the
amount of F in the sample using the
following:
-------
METHOD 14—DETERMINATION OF
FLUORIDE EMISSIONS FROM POTROOM
ROOF MONITORS FOR PRIMARY
ALUMINUM PLANTS27.114
1. Applicability and Principle.
1.1 Applicability. This method is
applicable for the determination of fluoride
emissions from stationary sources only when
specified by the test procedures for
•determining compliance with new source
performance standards.
1.2 Principle. Gaseous and particulate
fluoride roof monitor emissions are drawn
into a permanent sampling manifold through
several large nozzles. The sample is
transported from the sampling manifold to
ground level through a duct. The gas in the
duct is sampled using Method 13A or 13B—
Determination of Total Fluoride Emissions
from Stationary Sources. Effluent velocity
and volumetric flow rate are determined with
anemometers located in the roof monitor.
2. Apparatus.
2.1 Velocity measurement apparatus.
2.1.1 Anemometers. Propeller
anemometers, or equivalent. Each
Bnemometer^shall meet the following _
specifications: (1) Its propeller shall be madr
'of polystyrene, or similar material of uniform
density. To insure uniformity of perfurmunr.i:
among propellers, it is desirable thfil all
propellers be made from the same mold; (2)
The propeller shall be properly balanced, to
optimize performance: (3) When the
anemometer is mounted horizontally, its
threshold velocity shall not exceed 15 m/min
(50 fpm); (4) The measurement range of the
anemometer shall extend to at least 600 m/
min (2,000 fpm): (5) The anemometer shall hi'
able to withstand prolonged exposure to
dusty and corrosive environments: one way
of achieving this is to continuously purge the
bearings of the anemometer with filtered air
during operation; (6) All anemometer
components shall be properly shielded or
encased, such that the performance of the
anemometer is uninfluenced by potroom
magnetic field effects; (7) A known
relationship shall exist between the electrical
output signal from the anemometer generator
and the propeller shaft rpm, at a minimum of
three evenly spaced rpm settings between 60
and 1800 rpm; for the 3 settings, use 60±15.
000±100, and 1800±100 rpm. Anemometers
having other types of output signals (e.g.,
optical) may be used, subject to the approval
of the Administrator. If other types of
anemometers are used, there must be a
known relationship (as described above)
between output signal and shaft rpm; also.
each anemometer must be equipped with a
suitable readout system (See Section 2.1.3).
2.1.2 Installation of anemometers.
2.1.2.1 If the affected facility consists of u
single, isolated potroom (or potroom
segment), install at least one anemometer for
every 85 m of roof monitor length. If the
length of the roof monitor divided by 85 m is
not a whole number, round the fraction to the
nearest whole number to determine the
number of anemometers needed. For
monitors that are less than 130 m in length.
use at least two anemometers. Divide the
monitor cross-section into as many equal
areas as anemometers and locate an
anemometer at the centroid of each equal
area. See exception in Section 2.1.2.3.
2.1.2.2 If the affected facility consists of
two or more potrooms (or potroom segments)
ducted to a common control device, install
anemometers in each potroom (or segment)
that contains a sampling manifold. Install at
least one anemometer for every 85 m of roof
monitor length of the potroom (or segment). If
the potroom (or segment) length divided by 85
is not a whole number, round the fraction to
the nearest whole number to determine the
number of anemometers needed. If the
potroom (or segment) length is less than 130
m. use at least two anemometers. Divide the
potroom (or segment) monitor cross-section
into as many equal areas as anemometers
and locate'an anemometer at the centroid of
each equal area. See exception in Section
2.1.2.3.
2.1.2.3 At least one anemometer shall bu
installed in the immediate vicinity (i.e..
within 10 m) of the center of the manifold
(See Section 2.2.1). For its placement in
relation to the width of the monitor, there are
two alternatives. The first is'to make a
velocity traverse of the width of the roof
monitdr where an anemometer is to be placed
and install the anemometer at a point of
average velocity along this traverse. The
traverse may be made with any suitable low
velocity measuring device, and shall be made
during normal process operating conditions.
The second alternative, at the option of the
tester, is to install the anemometer halfway
across the width of the roof monitor. In this
latter case, the velocity traverse need not be
conducted.
2.1.3 Recorders. Recorders, equipped with
suitable auxiliary equipment (e.g.
transducers) for converting the output signal
from each anemometer to a continuous
recording of air flow velocity, or to an
integrated measure of volumetric flowrate. A
suitable recorder is one that allows the
output signal from the propeller anemometer
to be read to within 1 percent when the
velocity is between 100 and 120 m/min (350
and 400 fpm). For the purpose of recording
velocity, "continuous" shall mean one
readout per 15-minute or shorter time
interval. A constant amount of time shall
elapse between readings. Volumetric flow
rate may be determined by an electrical
count of anemometer revolutions. The
recorders or counters shall permit
identification of the velocities or flowrate
measured by each individual anemometer.
2.1.4 Pitot tube. Standard-type pilot tube.
as described in Section 2.7 of Method 2. and
having a coefficient of 0.99±0.01.
2.1.5 Pitot tube (optional). Isolated. Type
S pilot, as described in Section 2.1 of Method
2. The pitot tube shall have a known
coefficient, determined as outlined in Section
4.1 of Method 2.
2.1.6 Differential pressure gauge. Inclined
manometer or equivalent, as described in
Section 2.1.2 of Method 2.
2.2 Roof monitor air sampling system.
2.2.1 Sampling ductwork. A minimum of
one manifold system shall be installed for
each potroom group (as defined in Subpart S.
Section 60.191). The manifold system and
connecting duct shall be permanently
installed to draw an air sample from the roof
monitor to ground level. A typical installation
of a duct for drawing a sample from a roof
monitor to ground level is shown in Figure
14-1. A plan of a manifold system that is
located in a roof monitor is shown in Figure
14.2. These drawings represent a typical
installation for a generalized roof monitor.
The dimensions on these figures may be
altered slightly to make the manifold system
fit into a particular roof monitor, but the
general configuration shall be followed.
There shall be eight nozzles, each having a
diameter of 0.40 to 0.50 m. Unless otherwise
specified by the Admini»trator, the length of
the manifold system from the first nozzle to
the eighth shall be 35 m or eight percent of
the length of the potroom (or potroom
segment) roof monitor, whichever is greater.
The duct leading from the roof monitor
manifold shall be round with a diameter of
0.30 to 0.40 m. As shown in Figure 14-2. each
of the sample legs of the manifold shall have
a device, such as a blast gale or valve, to
enable adjustment of the flow into each
sample nozzle.
The manifold shall be located in the
immediate vicinity of one of the propeller
anemometers (see Section 2.1.2.3) and as
close as possible to the midseclion of the
potroom (or potroom segment). Avoid
locating the manifold near the end of a
potroom or in a section where the aluminum
reduction pot arrangement is not typical of
the rest of the potroom (or potroom segment).
Center the sample nozzles in the throat of the
roof monitor (see Figure 14-1). Construct all
sample-exposed surfaces within the nozzles.
manifold and sample duct of 316 stainless
steel. Aluminum may be used if a new
ductwork system is conditioned with
fluoride-laden roof monitor air for a period of
six weeks prior to initial testing. Other
materials of construction may be uied if it is
demonstrated through comparative testing
that there is no loss of flourides in the
system. All connections in the ductwork shall
be leak free.
Locate two sample ports in a vertical
section of the duct between the roof monitor
and exhaus.1 fan. The sample ports shall be at
least 10 duct diameters downstream and
three diameters upstream from any flow
disturbance such as a bend or contraction.
The two sample ports shall be situated 90°
apart. One of the sample ports shall be
situated so that the duct can be traversed in
the plane of the nearest upstream duct bend.
2.2.2 Exhaust fan. An industrial fan or
blower shall be attached to the sample duct
at ground level (see Figure 14-1). This
exhaust fan shall have a capacity such that a
large enough volume of air can be pulled
through the.ductwork to maintain an
isokinetic sampling rate in all the sample
nozzles for all flow rates normally
encountered in the roof monitor.
The exhaust fan volumetric flow rate shall
be adjustable so that the roof monitor air can
be drawn isokinetically into the sample
nozzles. This control of flow may be achieved
by a damper on the inlet to the exhauster or
by any other workable method.
2.3 Temperature measurement apparatus.
2.3.1 Thermocouple. Install a
thermocouple in the roof monitor near tb«
Ill-Appendix A-72
-------
SAMPLE
MANIFOLD
W/8 NOZZLES
ROOF MONITOR
SAMPLE EXTRACTION
DUCT
35 cm I.D.
H
13
(D
3
O.
H-
^4
to
SAMPLE PORTS IN
VERTICAL DUCT
SECTION AS SHOWN
EXHAUST BLOWER
Figure 14-1. Roof monitor sampling system.
-------
0.025 DIA
CALIBRATION
HOLE
DIMENSIONS IN METERS
NOT TO SCALE
Figure 14 2. Sampling manifold and nozzles.
Ill-Appendix A-74
-------
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sample duct. The thermocouple shall conform
to the specifications outlined in Section 2.3 of
Method 2.
2.3.2 Signal transducer. Transducer, to
change the thermocouple voltage output to •
temperature readout.
2.3.3 Thermocouple wire. To reach from
roof monitor to signal transducer and
recorder.
2.3.4 Recorder. Suitable recorder to
monitor the output from the'thermocouple
signal transducer.
2.4 Fluoride sampling train. Use the train
described in Method 13A or 13B.
3. Reagents.
3.1 Sampling and analysis. Use reagents
described in Method 13A or 13B.
4. Calibration.
4.1 Initial performance checks. Conduct
these checks within 60 days prior to the first
performance test.
4.1.1 Propeller anemometers.
Anemometers which meet the specifications
outlined in Section 2.1.1 need not be
calibrated, provided that a reference
performance curve relating anemometer
Signal output to air velocilj (covering tho
velocity range of interest) is available from
the manufacturer. For the purpose of this
method, a "reference" performance curve Is
defined as one that has been derived from
primary standard calibration data, with the
anemometer mounted vertically. "Primary
standard" data are obtainable by: (1) Direct
calibration of one or more of the
anemometers by the National Bureau of
Standards (NBS); (2) NBS-traceable
calibration; or (3) Calibration by direct
measurement of fundamental parameters
such as length and time (e.g., by moving the
anemometers through still air at measured
rates of speed, and recording the output
signals). If a reference performance curve is
not available from the manufacturer, such a
curve shall be generated, using one of the
three methods described as above. Conduct a
performance-check as outlined in Section
4.1.1.1 through 4.1.1.3, below. Alternatively.
the tester may use any other suitable method.
subject to the approval of the Administrator.
that takes into account the signal output.
propeller condition and threshold velocity of
the anemometer.
4.1.1.1 Check the signal output of the
anemometer by using an accurate rpm
generator (see Figure 14-3) or synchronous
motors to spin the propeller shaft at each of
the three rpm settings described in Section
2.1.1 above (specification No. 7), and
measuring the output signal at. each setting. If.
at each setting, the output signal is within ±
5 percent of the manufacturer's value, the
anemometer can be used. If the anemometer
performance is unsatisfactory, the
anemometer shall either be replaced or
repaired.
4.1.1.2 Check the propeller condition, by
visually inspecting the propeller, making note
of any significant damage or warpage;
damaged or deformed propellers shall be
replaced.
Ill-Appendix A-75
-------
SIDE
(A)
FRONT
SIDE
(B)
FRONT
Figure 14-4. Check of anemometer starting torque. A "y" gram weight placed "x" centimeters
from center of propeller shaft produces a torque of "xy" g-cm. The minimum torque which pro-
duces a 90° (approximately) rotation of the propeller is the "starting torque."
4.1.1.8 Check the anemometer threshold
velocity as follows: With the anemometer
mounted as thown in Figure 14-4(A). fasten B
known weight (a frraight-pin will suffice) to
tb« anemometer propeller at a fixed distance
from the center of the propeller shaft. This
will generate a known torque: for example, a
0.1 g weight, placed 10 cm from the center of
the (haft will generate a torque of 1.0 g-cn. If
the known torqut causes the propeller to
rotate downward, approximately 90° [see
Figure 14-4(B)j, then the known torque is
greater than or equal to the starting torque: if
the propeller fails to rotate approximately
90°, the known torque is less than the starting
torque. By trying different combinations of
weight and distance, the starting torque of a
particular anemometer can be satisfactorily
estimated. Once an estimate of the starting
torque has been obtained, the threshold
velocity of the anemometer (for horizontal
mounting) can be estimated from a graph
such as Figure 14-5 (obtained from the
manufacturer). If the horizontal threshold
velocity is acceptable |<15 m/min (50 fpm),
when this technique is used], the anemometer
can be used. If the threshold velocity of an
anemometer is found to be unacceptably
high, the anemometer shall either be replaced
or repaired.
Ill-Appendix A-76
-------
y
O
ec
o
o
z
rniiiii
FPM
(m/min)
20
(6)
40
(12)
60
(18)
80
(24)
100
(30)
120
(36)
140
(42)
THESHOLD VELOCITY FOR HORIZONTAL MOUNTING
Figure 145. Typical curve of starting torque vs horizontal threshold velocity for propeller
anemometers. Based on data obtained by R.M. Young Company, May, 1977.'
Ill-Appendix A-7 7
-------
4.1.2 Thermocouple. Check the calibration
of the thermocouple-potentiometer system,
using the procedures outlined in Section 4.3
of Method 2. at temperatures of 0.100, and
150'C. If the calibration is off by more than
S'C at any of the temperatures, repair or
replace the system: otherwise, the system can
be used.
4.1.3 Recorders and/or counters. Check
the calibration of each recorder and/or
counter (see Section 2.1.3) at a minimum of
three points, approximately spanning the
expected range of velocities. Use the
calibration procedures recommended by the
manufacturer, or other suitable procedures
(subject to the approval of the
Administrator). If a recorder or counter is
found to be out of calibration, by an average
amount greater than S percent for the three
calibration points, replace or repair the
system: otherwise, the system can be used.
4.1.4 Manifold Intake Nozzles. In order to
balance the flow rates in the eight individual
nozzles, proceed as follows: Adjust the
exhaust fan to draw a volumetric flow rate
(refer to Equation 14-1) such that the
entrance velocity into each manifold nozzle
approximates the average effluent velocity in
the roof monitor. Measure the velocity of the
air entering each nozzle by inserting a
standard pilot tube into a 2.5 cm or less
diameter hole (see Figure 14-2) located in the
manifold between each blast gate (or valve)
and nozzle. Note that a standard pilot tube is
used, rather than a type S, to eliminate
possible velocity measurement errors due to
cross-section blockage in the small (0.13 m
diameter) manifold leg ducts. The pilol lube
tip shall be posilioned al Ihe center of each
manifold leg duel. Take care lo insure that
there is no leakage around the pilot tube,
which could affect the indicated velocity in
the manifold leg. If the velocity of air being
drawn into each nozzle is not the same, open
or dose each blast gate (or valve) until the
velocity in each nozzle is the same. Fasten
each blast gate (or valve) so thai it will
remain in this position and close the pilot
port holes. This calibration shall be
performed when the manifold system is
installed. Alternatively. Ihe manifold may be
preassembled and the flow rales balanced on
the ground, before being installed.
4.2 Periodical performance checks.
Twelve months after their initial installation,
check the calibration of the propeller
anemometers, thermocouple-potentiometer
system, and the recorders and/or counters as
in Section 4.1. If the above systems pass the
performance checks, (i.e.. if no repair or
replacement of any component is necessary),
continue with the performance checks on a
12-month interval basis. However, if any of
the above systems fail Ihe performance
checks, repair or replace the syslem(s) that
failed and conduct Ihe periodical
performance checks on a 3-mohlh interval
basis, until sufficient information (consult
with the Administrator) is obtained to
establish a modified performance check
schedule and calculation procedure.
Note.-—If any of Ihe above systems fafl Ihe
initial performance checks, the data for the
past year need not be recalculated.
5. Procedure.
5.1 Roof Monitor Velocity Determination.
5.1.1 Velocity estimate(s) for setting
isokinetic flow. To assist in setting isokinetic
flow in the manifold sample nozzles, Ihe
anticipated average velocity in the section of
the roof monitor containing the sampling
manifold shall be estimated prior to each test
run. The tester may use any convenient
means to make this estimate (e.g.. the
velocity indicated by the anemometer in the
section of Ihe roof monitor containing the
sampling manifold may be continuously
monitored during the 24-hour period prior to
the test run).
If there is question as to whether a single
estimate of average velocity is adequate for
an entire test run (e.g.. if velocities are
anticipated to be significantly different
during different potroom operations), the
tester may opt to divide Ihe test run into two
or more "sub-runs," and to use a different
estimated average velocity for each sub-run
(see Section 5.3.2.2.)
5.1.2 Velocity determination during a test
run. During the actual test run, record the
velocity or volumetric flowrate readings of
each propeller anemometer in the roof
monitor. Readings shall be taken for each
anemometer every 15 minutes or at shorter
equal time intervals (or continuously).
5.2 Temperature recording. Record the
temperature of the roof monitor every 2 hours
during the test run.
5.3 Sampling.
5.3.1 Preliminary air flow in duct. During
24 hours preceding the jest, turn on the
exhaust fan and draw roof monitor air
through the manifold duct to condition the
ductwork. Adjust the fan to draw a
volumetric flow through the duct such that
the velocity of gas entering the manifold
nozzles approximates the average velocity of
the air exiting the roof monitor in the vicinity
of the sampling manifold.
5.3.2 Manifold isokinetic sample rate
adjustment(s).
5.3.2.1 Initial adjustment. Prior to the test
run (or first sub-run, if applicable: see Section
5.1.1 and 5.3.2.2), adjust the fan to provide the
necessary volumetric flowrate in the
sampling duct, so that air enters the manifold
sample nozzles at a velocity equal to the
appropriate estimated average velocity
determined under Section 5.1.1. Equation 14-1
gives the correct stream velocity needed in
the duct at the sampling location, in order for
sample gas to be drawn isokinetically into
the manifold nozzles. Next, verify that the
correct stream velocity has been achieved, by
performing a pilot tube traverse of the sample
duct (using either a standard or type S pilot
tube); use the procedure outlined in Method 2.
8 (0.)' ~ 1 mtn
».= (vj ._ .(Equation 14-1)
(D«C 60 sec
Where:
va = Desired velocity in duct al sampling
location, m/sec.
Dn —Diameter of a roof monitor manifold
nozzle, m.
D0 = Diameter of duel at sampling location.
m.
vm = Average velocity of the air stream in
the roof monitor, m/min. as determined
under Section 5.1.1.
5.3.2.2 Adjustments during run. If the test
run is divided into two or more "sub-runs"
(see Section 5.1.1), additional isokint-tic rule
adjustment(s) may become necessary during
the run. Any such adjustment shall be made
just before the start of a sub-run, using the
procedure outlined in Section 5.3.2.1 above.
Nole.—Isokinetic rale adjustments are not
permissible during a sub-run.
5.3.3 Sample train operation. Sample the
duct using the standard fluoride train and
methods described in Methods 13A and 13B.
Determine the number and location of the
sampling points in accordance with Method
1. A single train shall be used for the entire
sampling run. Alternatively, if two or more
sub-runs are performed, a separate train may
be used for each sub-run: note, however, that
if this option is chosen, the area of the
sampling nozzle shall be the same (± 2
percent) for each train. If the test run is
divided into sub-runs, a complete traverse of
the duct shall be performed during each sub-
run.
5.3.4 Time per run. Each tesl run shall last
8 hours or more; if more than one run is to be
performed, all runs shall be of approximately
the same (± 10 percent) length. If question
exists as to the representativeness of an 8-
hour test, a longer period should be selected.
Conduct each run during a period when all
normal operations are performed underneath
the sampling manifold. For most recently-
constructed plants. 24 hours are required for
all potroom operations and events to occur in
the area beneath the sampling manifold.
During the test period, all pots in the potroom
group shall be operated such that emissions
are representative of normal operating
conditions in the potroom group.
5.3.5 Sample recovery. Use the sample
recovery procedure described in Method 13A
or 13B.
5.4 Analysis. Use the analysis procedures
described in Method 13A or 13B.
6. Calculations.
6.1 Isokinetic sampling check.
6.1.1 Calculate the mean velocity (vm) for
the sampling run. as measured by the
anemometer in the section of the roof monitor
containing the sampling manifold. If two or
more sub-runs have been performed, the
tester may opt to calculate the mean velocity
for each sub-run.
6.1.2 Using Equalion 14-1. calculate the
expected average velocity (vd) in the
sampling duct, corresponding to each value of
vm obtained under Section 6.1.1.
6.1.3 Calculate the actual average velocity
(vj in the sampling duct for each run or sub-
run, according to Equation 2-9 of Method 2.
and using data obtained from Method 13.
6.1.4 Express each value v. from Seclion
6.1.3 as a percentage of the corresponding vd
value from Section 8.1.2.
Ill-Appendix A-78
-------
6.1.4.1 If v. .is less than or equal to 120
percent of vd. the results are acceptable (note
that in cases where the above calculations
have been performed for each sub-run, the
results are acceptable if the average
percentage for all sub-runs is less than or
equal to 120 percent).
6.1.4.2 If v, is more than 120 percent of vd,
multiply the reported emission rate by the
following factor.
(100 y./vj -120
200
6.2 Average velocity of roof monitor
gases. Calculate the average roof monitor-
n
(Ft).
j,
velocity using all the velocity or volumetric
flow readings from Section 5.1.2.
6.3 Roof monitor temperature. Calculate
the mean value of the temperatures recorded
in Section 5.2.
6.4 Concentration of fluorides in roof
monitor air (in mg F/m3).
6.4.1 If a single sampling train was used
throughout the run. calculate the average
fluoride concentration for the roof monitor
using Equation 13A-2 of Method 13A.
6.4.2 If two or more sampling trains were
used (i.e., one per sub-run), calculate the
average fluoride concentration for the run, as
follows:
(Equation 14^2)
Where:
C.=Average fluoride concentration in roof
monitor air, mg F/dscm.
• Ft=Total fluoride mass collected during a
particular sub-run, mg F (from Equation
13A-1 of Method 13A or Equation 13B-1
of MethodlSB).
Vro(tul)=Tolal volume of sample gas
passing through the dry gas meter during
a particular sub-run, dscm (see Equation
5-1 of Method 5).
n=Total number of sub-runs.
6.5 Average volumetric flow from the roof
monitor of the potroom(s) (or potroom
segment(s)) containing the anemometers is
given in Equation 14-3.
-------
METHOD 15. DETERMINATION OF HYDROGEN
SULFIDE. CARBONYL SULFIDE, AND CARBON
DISULPIDE EMISSIONS PROM STATIONARY
SOURCES 86
INTRODUCTION
The method described below uses the
principle of gas chromatographic separation
and flame photometric detection (FPD).
Since there are many systems or sets of op-
erating conditions that represent usable
methods of determining sulfur emissions, all
systems which employ this principle, but
differ only in details of equipment and oper-
ation, may be used as alternative methods,
provided that the criteria set below are met.
1. Principle and applicability
1.1 Principle. A gas sample is extracted
from the emission source and diluted with
clean dry air. An aliquot of the diluted
sample is then analyzed for hydrogen sul-
fide (H.S). carbonyl sulfide (COS), and
carbon disulfide (CS>) by gas chromatogra-
phic (GO separation and flame photomet-
ric detection (FPD).
1.2 Applicability. This method is applica-
ble for determination of the above sulfur
compounds from tail gas control units of
sulfur recovery plants.
2. Range and sensitivity
2.1 Range. Coupled with a gas chromto-
graphic system utilizing a l-milliliter sample
size, the maximum limit of the FPD for
each sulfur compound Is approximately 10
ppm. It may be necessary to dilute gas sam-
ples from sulfur recovery plants hundred-
fold (99:1) resulting In an upper limit of
about 1000 ppm for each compound.
2.2 The minimum detectable concentra-
tion of the FPD is also dependent on sample
size and would be about 0.5 ppm for a 1 ml
sample.
3. Interferences
3.1 Moisture Condensation. Moisture con-
densation in the sample delivery system, the
analytical column, or the FPD burner block
can cause losses or Interferences. This po-
tential is eliminated by heating the sample
line, and by conditioning the sample with
dry dilution air to lower its dew point below
the operating temperature of the OC/FPD
analytical system prior to analysis.
3.2 Carbon Monoxide and Carbon Dioxide.
CO and CO, have substantial desensitizing
effects on the flame photometric detector
. even after 9:1 dilution. (Acceptable systems
must demonstrate that they have eliminat-
ed this interference by some procedure such
as eluding CO and CO, before any of the
sulfur compounds to be measured.) Compli-
ance with this requirement can be demon-
strated by submitting chromatograms of
calibration gases with and without CO, in
the diluent gas. The CO, level should be ap-
proximately 10 percent for the case with
CO. present. The two chromatographs
should show agreement within the precision
limits of, section 4.1.
3.3 Elemental Sulfur. The condensation of
sulfur vapor in the sampling line can lead to
eventual coating and even blockage of the
sample line. This problem can be eliminated
along with the moisture problem by heating
the sample line.
4. Precision
4.1 Calibration Precision. A series of three
consecutive injections of the same calibra-
tion gas, at any dilution, shall produce re-
sults which do not vary by more than ±13
percent from the mean of the three injec-
tions.
4.2 Calibration Drift. The calibration drift
determined from the mean of three injec-
tions made at the beginning and end of any
8-hour period shall not exceed ±5 percent.
5. Apparatus
5.1.1 Probe. The probe must be made of
inert material such as stainless steel or
glass. It should be designed to incorporate a
, filter and to allow calibration gas to enter
the probe at or near the sample entry point.
Any portion of the probe not exposed to the
stack gas must be heated to prevent mois-
ture condensation.
5.1.2 The sample line must be made of
Teflon,'no greater than 1.3 cm (Vz in) inside
diameter. All parts from the probe to the di-
lution system must be thermostatically
heated to 120* C.
5.1.3 Sample Pump. The sample pump
shall be a leakless Teflon coated diaphragm
type or equivalent. If the pump is upstream
of the dilution system, the pump head must
be heated to 120' C.
5.2 Dilution System. The dilution system
must be constructed such that all sample
contacts are made of inert material (e.g.
stainless steel or Teflon). It must be heated
to 120* C and be capable of approximately a
9:1 dilution of the sample.
5.3 Gas Chromatograph. The gas chroma-
tograph must have at least the following
components:
5.3.1 Oven. Capable of maintaining the
separation column at the proper operating
temperature ±1* C.
5.3.2 Temperature Gauge. To monitor
column oven, detector, and exhaust tem-
perature ±r C.
5.3.3 Flow System. Gas metering system to
measure sample, fuel, combustion gas, and
carrier gas flows.
5.3.4 Flame Photometric Detector.
5.3.4.1 Electrometer. Capable of full scale
amplification of linear ranges of 10''to 10'•
amperes full scale.
5.3.4.2 Power Supply. Capable of deliver-
ing up to 750 volts.
5.3.4.3 Recorder. Compatible with the
output voltage range of the electrometer.
5.4 Gas Chromatograph Columns. The
column system must be demonstrated to be
capable of resolving three major reduced
sulfur compounds: H.S, COS, and CS>.
To demonstrate that adequate resolution
has been achieved the tester must submit a
Chromatograph of a calibration gas contain-
ing all three reduced sulfur compounds In
the concentration range of the applicable
standard. Adequate resolution will be de-
fined as base line separation of adjacent
peaks when the amplifier attenuation is set
so that the smaller peak is at least 50 per-
cent of full scale. Base line separation is de-
fined as a return to zero ±5 percent in the
Interval between peaks. Systems not meet-
ing this criteria may be considered alternate
methods subject to the approval of the Ad-
ministrator.
5.5.1 Calibration System. The calibration
system must contain the following compo-
nents.
5.5.2 Flow System. To measure air flow
over permeation tubes at ±2 percent. Each
flowmeter shall be calibrated after a com-
plete test series with a wet test meter. If the
flow measuring device differs jfrom the wet
test meter by 5 percent, the completed test
shall be discarded. Alternatively, the tester
may elect to use the flow data that would
yield the lowest flow measurement. Calibra-
tion with a wet test meter before a test is
optional.
'Mention of trade names or specific prod-
ucts does not constitute an endorsement by
the Environmental Protection Agency.
5.5.3 Constant Temperature Bath. Device
capable of maintaining the permeation
tubes at the calibration temperature within
±1.1" C.
5.5.4 Temperature Gauge. Thermometer
or equivalent to monitor bath temperature
within ±r C.
6. Reagents
6.1 Fuel. Hydrogen (H,) prepurified grade
or better.
6.2 Combustion Gas. Oxygen (O,) or air,
research purity or better.
6.3 Carrier Gas. Prepurified grade or
better.
6.4 Diluent. Air containing less than 0.5
ppm total sulfur compounds and less than
10 ppm each of moisture and total hydro-
carbons.
6.5 Calibration Gases. Permeation tubes,
one each of H,S, COS, and CS,, gravimetri-
cally calibrated and certified at some conve-
nient operating temperature. These tubes
consist of hermetically sealed FEP Teflon
tubing In which a liquified gaseous sub-
stance is enclosed. The enclosed gas perme-
ates through the tubing wall at a constant
rate. When the temperature is constant,
calibration gases covering a wide range of
known concentrations can be generated by
varying and accurately measuring the flow
rate of diluent gas passing over the tubes.
These calibration gases are used to calibrate
the GC/FPD system and the dilution
system.
7. Pretest Procedures
The following procedures are optional but
would be helpful in preventing any problem
which might occur later and Invalidate the
entire test.
7.1 After the complete measurement
system has been set up at the site and
deemed to be operational, the following pro-
cedures should be completed before sam-
pling is initiated.
7.1.1 Leak Test. Appropriate leak test pro-
cedures should be employed to verify the In-
tegrity of all components, sample lines, and
connections. The following leak test proce-
dure is suggested: For components upstream
of the sample pump, attach the probe end
of the sample line to a manometer or
vacuum gauge, start the pump and pull
greater than 50 mm (2 in.) Mg vacuum, close
off the pump outlet, and then stop the
pump and ascertain that there is no leak for
1 minute. For components after the pump,
apply a slight positive pressure and check
for leaks by applying a liquid (detergent in
water, for example) at each joint. Bubbling
indicates the presence of a leak.
7.1.2 System Performance. Since the com-
plete system is calibrated following each
test, the precise calibration of each compo-
nent is not critical. However, these compo-
nents should be verified to be operating.
properly. This verification can be performed
by observing the response of flowmeters or
of the GC output to changes in flow rates or
calibration gas concentrations and ascer-
taining the response to be within predicted
limits. If any component or the complete
system fails to respond in a normal and pre-
dictable manner, the source of the discrep-
ancy should be identifed and corrected
before proceeding.
8. Calibration
Prior to any sampling run. calibrate the
system using the following procedures. (If
more than one run is performed during any
24-hour period, a calibration need not be
performed prior to the second and any sub-
sequent runs. The calibration must, howev-
er, be verified as prescribed in section 10,
after the last run made •within the 24-hour
Ill-Appendix A-80
-------
period.)
8.1 General Considerations. This section
outlines steps to be followed for use of the
GC/FPD and the dilution system. The pro-
cedure does not include detailed instruc-
tions because the operation of these systems
is complex, and it requires an understanding
of the individual system being used. Each
system should include a written operating
manual describing in detail the operating
procedures associated with each component
in the measurement system. In addition, the
operator shuld be familiar with the operat-
ing principles of the components; particular-
ly the GC/PPD. The citations in the Bib-
liography at the end of this method are rec-
ommended for review for this purpose.
8.2 Calibration Procedure. Insert the per-
meation tubes into the tube chamber. Check
the bath temperature to assure agreement
with the calibration temperature of the
tubes within ±0.1°C. Allow 24 hours for the
tubes to equilibrate. Alternatively equilibra-
tion may be verified by injecting samples of
calibration gas at 1-hour intervals. The per-
meation tubes can be assumed to have
reached equilibrium when consecutive
hourly samples agree within the precision
limits of section 4.1.
Vary the amount of air flowing over the
tubes to produce the desired concentrations
for calibrating the analytical and dilution
systems. The air flow across the tubes must
at all times exceed the flow requirement of
the analytical systems. The concentration in
parts per million generated by a bube con-
taining a specific permeant can be calculat-
ed as follows:
Equation 15-1
where:
C= Concentration of permeant produced
in ppm.
P,= Permeation rate of the tube in us/
mln.
M = Molecular weight of the permeant: g/
g-mole.
L=Flow rate. 1/min, of air over permeant
@ 20'C, 760 mm Hg.
K = Gas constant at 20'C and 760 mm
Hg= 24.04 1/g mole.
8.3 Calibration of analysis system. Gener-
ate a series of three or more known concen-
trations spanning the linear range of the
FPD (approximately O.OS to 1.0 ppm) for
each of the four major sulfur compounds.
Bypassing the dilution system, Inject these
standards in to the GC/FPD analyzers and
monitor the responses. Three injects for
each concentration must yield the precision
described in section 4.1. Failure to attain
this precision is an Indication -of a problem
in the calibration or analytical system. Any
such problem must be identified and cor-
rected before proceeding.
8.4 Calibration Curves. Plot the GC/FPD
response in current (amperes) versus their
causative concentrations in ppm on log-log
coordinate graph paper for each sulfur com-
pound. Alternatively, a least squares equa-
tion may be generated from the calibration
data.
8.S Calibration of Dilution System. Gener-
ate a know concentration of hydrogen sul-
fied using the permeation tube system.
Adjust the flow rate of diluent air for the
first dilution stage so that the desired level
of dilution is approximated. Inject the dilut-
ed calibration gas into the GC/FPD system
and monitor its response. Three injections
for each dilution must yield the precision
described in section 4.1. Failure to attain
this precision in this step is an indication of
a problem in the dilution system. Any such
problem must be identified and corrected
before proceeding. Using the calibration
data for H»S (developed under 8.3) deter-
mine the diluted calibration gas concentra-
tion in ppm. Then calculate the dilution
factor as the ratio of the calibration gas
concentration before dilution to the diluted
calibration gas concentration determined
under this paragraph. Repeat this proce-
dure for each stage of dilution required. Al-
ternatively, the GC/FPD system may be
calibrated by generating a series of three or
more concentrations of each sulfur com-
pound and diluting these samples before in-
jecting them into the OC/FPD system. This
data will then serve as the calibration data
for the unknown samples and a separate de-
termination of the dilution factor will not
be necessary. However, the precision re-
quirements of section 4.1 are still applicable.
9. Sampling and Analysis Procedure
9.1 Sampling. Insert the sampling probe
into the test port making certain that no di-
lution air enters the stack through the port.
Begin sampling and dilute the sample ap-
proximately 9:1 using the dilution system.
Note that the precise dilution factor Is that
which is determined in paragraph 8.5. Con-
dition the entire system with sample for a
minimum of 15 minutes prior to commenc-
ing analysis.
9.2 Analysis. Aliquots of diluted sample
are injected into the GC/FPD analyzer for
analysis.
9.2.1 Sample Run. A sample run is com-
posed of 16 individual analyses (injects) per-
formed over a period of not less than 3
hours or more than 6 hours.
9.2.2 Observation for Clogging of Probe. If
reductions in sample concentrations are ob-
served during a sample run that cannot be
explained by process conditions, the sam-
pling must be interrupted to determine if
the sample probe is clogged with paniculate
matter. If the probe Is found to be clogged,
the test must be stopped and the results up
to that point discarded. Testing may resume
after cleaning the probe or replacing it with
a clean one. After each run, the sample
probe must be Inspected and. If necessary.
dismantled and cleaned.
10. Post-Test Procedures
10.1 Sample Line Loss. A known concen-
tration of hydrogen sulflde at the level of
the applicable standard. ±20 percent, must
be introduced into the sampling system at
the opening of the probe in sufficient quan-
tities to ensure that there is an excess of
sample which must be vented to the atmo-
sphere. The sample must be transported
through the entire sampling system to the
measurement system In the normal manner.
The resulting measured concentration
should be compared to the known value to
determine the sampling system loss. A sam-
pling system loss of more than 20 percent Is
unacceptable. Sampling losses of 0-20 per-
cent must be corrected by dividing the re-
sulting sample concentration by the frac-
tion of recovery. The known gas sample may
be generated using permeation tubes. Alter-
natively, cylinders of hydrogen sulfide
mixed in air may be used provided they are
traceable to permeation tubes. The optional
pretest procedures provide a good guideline
for determining if there are leaks in the
sampling system.
10.2 Recallbration. After each run. or
after a series of runs made within a 24-hour
period, perform a partial recalibration using
the procedures in section 8. Only H.S (or
other permeant) need be used to recalibrate
the GC/FPD analysis system (8.3) and the
dilution system (8.5).
10.3 Determination of Calibration Drift.
Compare the calibration curves obtained
prior to the runs, to the calibration curve*
obtained under paragraph 10.1. The calibra-
tion drift should not exceed the limits set
forth in paragraph 4.2. If the drift exceed*
this limit, the intervening run or run*
should be considered not valid. The tester,
however, may Instead have the option of
choosing the calibration data set which
would give the highest sample values.
11. Calculations
11.1 Determine the concentrations of each
reduced sulfur compound detected directly
from the calibration curves. Alternatively,
the concentrations may be calculated using
the equation for the least squares line.
11.2 Calculation of SO, Equivalent. SO,
equivalent will be determined for each anal-
ysis made by summing the concentrations of
each reduced sulfur compound resolved
during the given analysis.
SO. equivalent=2(H,S, COS. 2 CS,)d
Equation 15-2
where:
SOt equivalent=The sum of the concen-
tration of each of the measured com-
pounds (COS, H>S, CSt) expressed as
sulfur dioxide in ppm.
H.S=Hydrogen sulfide, ppm.
COS = Carbonyl sulfide, ppm.
CS,=Carbon disulfide, ppm.
d=Dilution factor, dimensionless.
11.3 Average SO, equivalent will be deter-
mined as follows:
Average SO^ equivalent
1
equtv.j
N (1 - Bwo)
Equation 15-.'
where:
Average SO, equivalent, = Average SO,
equivalent in ppm, dry basis.
Average SO, equivalent,=SO, in ppm as
• determined by Equation 15-2.
N=Number of analyses performed.
Bwo=Fraction of volume of water vapor
in the gas stream as determined by
Method 4—Determination of Moisture
in Stack Oases (36 FR 24887).
12. Example System
Described below Is a system utilized by
EPA in gathering NSPS data. This system
does not now reflect all the latest develop-
ments in equipment and column technology,
but It does represent one system that hat
been demonstrated to work.
12.1 Apparatus.
12.1.1 Sample System.
12.1.1.1 Probe. Stainless steel tubing, 6.35
mm (V< in.) outside diameter, packed with
glass wool.
12.1.1.2 Sample Line. Vi> inch inside diam-
eter Teflon tubing heated to 120* C. Thl«
temperature is controlled by a thermostatlc
heater.
12.1.1.3 Sample Pump. Leakless Teflon
coated diaphragm type or equivalent. The
pump head Is heated to 120* C by enclosing
It In the sample dilution box (12.2.4 below).
12.1.2 Dilution System. A schematic dia-
gram of the dynamic dilution system ii
given in Figure 15-2. The dilution system k
constructed such that all sample contact!
are made of Inert materials. The dilutior
Ill-Appendix A-81
-------
system which Is heated to 120* C must be ca-
pable of a minimum of 9:1 dilution of
sample. Equipment used In the dilution
system is listed below:
12.1.2.1 Dilution Pump. Model A-150 Koh-
tnyhr Teflon positive displacement type.
nonadjustable ISO cc/min. ±2.0 percent, or
equivalent, per dilution stage. A 9:1 dilution
of sample is accomplished by combining 150
cc of sample with 1350 cc of clean dry air as
shown In Figure 15-2.
12.1.2.2 Valves. Three-way Teflon solenoid
or manual type.
12.1.2.3 Tubing. Teflon tubing and fittings
«re used throughout from the sample probe
to the OC/FPD to present an inert surface
for sample gas.
12.1.2.4 Box. Insulated box, heated and
maintained at 120'C, of sufficient dimen-
sions to house dilution apparatus.
12.1.2.5 Flowmeters. Rotameters or equiv-
alent to measure flow from 0 to 1500 ml/
mln. ± 1 percent per dilution stage.
12.1.3.0 Oas Chromatograph.
12.1.3.1 Column—1.83 m (6 ft.) length of
Teflon tubing. 2.16 mm (0.085 in.) Inside di-
ameter, packed with deactivated silica gel.
or equivalent.
12.1.3.2 Sample Valve. Teflon six port gas
sampling valve, equipped with a 1 ml sample
loop, actuated by compressed air (Figure 15-
1).
12.1.3.3 Oven. For containing sample
valve, stripper column and separation
column. The oven should be capable of
maintaining an elevated temperature rang-
ing from ambient to 100* C. constant within
±1'C.
12.1.3.4 Temperature Monitor. Thermo-
couple pyrometer to measure column oven.
detector, and exhaust temperature ± r C.
12.1.3.5 Flow System. Oas metering
system to measure sample flow, hydrogen
flow, oxygen flow and nitrogen carrier gas
flow.
12.1.3.6 Detector. Flame photometric de-
tector.
12.1.3.7 Electrometer. Capable of full scale
amplification of linear ranges of 10'* to 10~*
amperes full scale.
12.1.3.8 Power Supply. Capable of deliver-
ing up to 750 volts.
12.1.3.9 Recorder. Compatible with the
output voltage range of the electrometer.
12.1.4 Calibration. Permeation tube
system (Figure 15-3).
12.1.4.1 Tube Chamber. Olass chamber of
sufficient dimensions to house permeation
tubes.
12.1.4.2 Mass Flowmeters. Two mass flow-
meters in the range 0-3 1/mln. and 0-10 I/
mln. to measure air flow over permeation
tubes at ±2 percent. These flowmeters shall
be cross-calibrated at the beginning of each
test. Using a convenient flow rate in the
measuring range of both flowmeters, set
and monitor the flow rate of gas over the
permeation tubes. Injection of calibration
gas generated at this flow rate as measured
by one flowmeter followed by injection of
calibration gas at the same flow rate as mea-
sured by the other flowmeter should agree
within the specified precision limits. If they
do not, then there is a problem with the
mass flow measurement. Each mass flow-
meter shall be calibrated prior to the first
test with a wet test meter and thereafter at
least once each year.
12.1.4.3 Constant Temperature Bath. Ca-
pable of maintaining permeation
-------
METHOD 16. SEMICONTIirUOUS DETERMINATION
Or SULFUR EMISSIONS FROM STATIONARY
SOURCES 62
Introduction
The method described below uses the
principle of gas chromatographic separation
and flame photometric detection. Since
there are many systems or sets of operating
conditions that represent usable methods of
determining sulfur emissions, all systems
which employ this principle, but differ only
In details of equipment and operation, may
be used as alternative methods, provided
that the criteria set below are met.
1. Principle and Applicability.
1.1 Principle. A gas sample is extracted
from the emission source and diluted with
clean dry air. An aliquot of the diluted
sample is then analyzed for hydrogen sul-
fide (H,S>, methyl mercaptan (MeSH), di-
methyl sulfide (DMS) and dimethyl disul-
fide (DMDS) by gas chromatographic (OC)
separation and flame photometric detection
(FPD). These four compounds are known
collectively as total reduced sulfur (TRS).
1.2 Applicability. This method Is applica-
ble for determination of TRS compounds
from recovery furnaces, lime kilns, and
smelt dissolving tanks at kraft pulp mills.
2. Range and Sensitivity.
2.1 Range. Coupled with a gas chromato-
graphic system utilizing a ten milllliter
sample size, the maximum limit of the PPD
for each sulfur compound is approximately
1 ppm. This limit is expanded by dilution of
the sample gas before analysis. Kraft mill
gas samples are normally diluted tenfold
(9:1), resulting in an upper limit of about 10
ppm for each compound.
For sources with emission levels between
10 and 100 ppm. the measuring range can be
best extended by reducing the sample size
to 1 milliliter.
2.2 Using the sample size, the minimum
detectable concentration is approximately
50 ppb.
3. Interferences.
3.1 Moisture Condensation. Moisture
condensation in the sample delivery system,
the analytical column, or the FPD burner
block can cause losses or interferences. This
potential is eliminated by heating the
sample line, and by conditioning the sample
with dry dilution air to lower its dew point
below the operating temperature of the
OC/FPD analytical system prior to analysis.
3.2 Carbon Monoxide and Carbon Diox-
ide. CO and CO, have substantial desensitiz-
ing effect on the flame photometric detec-
tor even after 9:1 dilution. Acceptable sys-
tems must demonstrate that they have
eliminated this interference by some proce-
dure such as eluting these compounds
before any of the compounds to be mea-
sured. Compliance with this requirement
can be demonstrated by submitting chroma-
tograms of calibration gases with and with-
out Cd In the diluent gas. The COt level
should be approximately 10 percent for the
case with CO, present. The two chromato-
graphs should show agreement within the
precision limits of Section 4.1.
3.3 Paniculate Matter. Particuiale
matter in gas samples can cause Interfer-
ence by eventual clogging of the analytical
system. This Interference must be eliminat-
ed by use of a probe filter.
3.4 Sulfur Dioxide. SO, is not a specific
Interferent but may be present in such large
amounts that it cannot be effectively sepa-
rated from other compounds of Interest.
The procedure must be designed to elimi-
nate this problem either by the choice of
separation columns or by removal of SO.
from the sample, in the example
system, SO, is removed by a citrate
buffer solution prior to GC injection.
This scrubber will be used when SO,
levels are high enough to prevent
baseline separation from the reduced
sulfur compounds. 93
Compliance with this section can be denv
onstrated by submitting chromatographs of
calibration gases with SO, present in the
same quantities expected from the emission
source to be tested. Acceptable systems
shall show baseline separation with the am-
plifier attenuation set so that the reduced
sulfur compound of concern Is at least SO
percent of full scale. Base line separation is
defined as a return to zero ± percent In the
Interval between peaks.
4. Precision and Accuracy.
4.1 OC/FPD and Dilution System Cali-
bration Precision. A series of three consecu-
tive Injections of the same calibration gas,
at any dilution, shall produce results which
do not vary by more than ± 6 percent from
the mean of the three injections.93
4.2 GC/FPD and Dilution System Cali-
bration Drift. The calibration drift deter-
mined from the mean of three injections
made at the beginning and end of any 8-
hour period shall not exceed ± percent.
4.3 System Calibration Accuracy.
Losses through the sample transport
system must be measured and a cor-
rection factor developed to adjust the
calibration accuracy to 100 percent.93
6. Apparatus (See Figure 16-1).
5.1. Sampling.93
5.1.1 Probe. The probe must be made of
Inert material such as stainless steel or
glass. It should be designed to incorporate a
filter and to allow calibration gas to enter
the probe at or near the sample entry point.
Any portion of the probe not exposed to the
stack gas must be heated to prevent mois-
ture condensation.
5.1.2 Sample Line. The sample line must
be made of Teflon,1 no greater than 1.3 cm
(V4) inside diameter. All parts from the
probe to the dilution system must be ther-
mostatically heated to 120' C.
5.1.3 Sample Pump. The sample pump
shall be a leakless Teflon-coated diaphragm
type or equivalent. If the pump is upstream
of the dilution system, the pump head must
be heated to 120' C.
5.2 Dilution System. The dilution system
must be constructed such that all sample
contacts are made of Inert materials (e.g..
stainless steel or Teflon). It must be heated
to 120* C. and be capable of approximately a
9:1 dilution of the sample.
5.3 SO, Scrubber. The
SOj scrubber is a midget impinger
packed with glass wool to eliminate
entrained mist and charged with po-
tassium citrate-citric acid buffer.93
5.4 Gas Chromatograph. The gas chro-
matograph must have at least the following
components: 93
5.4.1 Oven. Capable of maintaining the
separation column at the proper operating
temperature ±1' C.93
5.4.2 Temperature Gauge. To monitor
column oven, detector, and exhaust tem-
perature ±TC.93
5.4.3 Flow System. Gas metering system
to measure sample, fuel, combustion gas,
and carrier gas flows. 93
'Mention of trade names or-specific-pro*
ucts does not constitute endorsement by the
Environmental Protection Agency.
6.AA Flame Photometric Detector. 93
5.4.4.1 Electrometer. Capable of full scale
amplification of linear ranges of 10"' to 10**
amperes full scale.'3
6.4.4.2 Power Supply. Capable of deliver-
ing up to 750 volts. 93
5.4.4.3 Recorder. Compatible with the
output voltage range of the electrometer. 93
5.6 Gas Chromatograph Columns. The
column system must be demonstrated to be
capble of resolving the four major reduced
sulfur compounds: H»S, MeSH, DMS, and
DMDS. It must also demonstrate freedom
from known interferences. 93
To demonstrate that adequate resolution
has been achieved, the tester must submit a
Chromatograph of a calibration gas contain-
ing all four of the TRS compounds in the
concentration range of the applicable stan-
dard. Adequate resolution will be defined as
base line separation of adjacent peaks when
the amplifier attenuation is set so that the
smaller peak is at least 50 percent of full
scale. Base line separation is defined In Sec-
tion 3.4. Systems not meeting this criteria
may be considered alternate methods sub-
ject to the approval of the Administrator.93
5.5.1 Calibration System. The calibration
system must contain the following compo-
nents. 93
5.5.2 Tube Chamber. Chamber of glass or
Teflon of sufficient dimensions to house
permeation tubes. 93
.5.5.3 Flow System. To measure air flow
over permeation tubes at ±2 percent. Each
flowmeter shall be calibrated after a com-
plete test series with a wet test meter. If the
flow measuring device differs from the wet
test meter by 5 percent, the completed test
shall be discarded. Alternatively, the tester
may elect to use the flow data that would
yield the lower flow measurement. Calibra-
tion with a wet test meter before a test is
optional. 93
8.5.4 Constant Temperature Bath. Device
capable of maintaining the permeation
tubes at the calibration temperature within
±0.1'C.93
5.5.5 Temperature Gauge. Thermometer
or equivalent to monitor bath temperature
within ±1'C.93
6. Reagents.
6.1 Fuel. Hydrogen (H,) prepurified
grade or better.
6.2 Combustion Gas. Oxygen (O.) or air,
research purity or better.
6.3 Carrier Gas. Prepurified grade or
better.
6.4 Diluent. Air containing less than 50
ppb total sulfur compounds and less than 10
ppm each of moisture and total hydrocar-
bons. This gas must be heated prior to
mixing with the sample to avoid water con-
densation at the point of contact.
6.5 Calibration Gases. Permeation tubes.
one each of H.S, MeSH, DMS, and DMDS,
agravtmetrically calibrated and certified at
some convenient operating temperature.
These tubes consist of hermetically sealed
FEP Teflon tubing in which a liquified gas-
eous substance is enclosed. The enclosed gas
permeates through the tubing wall at a con-
stant rate. When the temperature is con-
stant, calibration gases Governing a wide
range of known concentrations can be gen-
erated by varying and accurately measuring
the flow rate of diluent gas passing over the
tubes. These calibration gases are used to
calibrate the GC/FPD system and the dilu-
tion system.
6.6 Citrate Buffer. Dis-
solve 300 grams ol potassium .citrate
and 41 grams of anhydrous citric acid
In 1 liter of deionized water. 284 grams
of sodium citrate may be substituted
for the potassium citrate. 93
Ill-Appendix A-83
-------
f. Pretest Procedure*. The following proce-
res are optional but would be helpful in
eventing any problem which might occur
-er and invalidate the entire test.
7.1 After the complete measurement
stem has been set up at the site and
etned to be operational, the following pro-
dures should be completed before satn-
Ing is initiated.
7.1.1 Leak Test. Appropriate leak test
ocedures should be employed to verify the
tegrity of all components, sample lines,
id connections. The following leak test
ocedure is suggested: For components up-
ream of the sample pump, attach the
obe end of the sample line to a ma- no-
eter or vacuum gauge, start the pump and
ill greater than SO mm (2 in.) Hg vacuum,
jse off the pump outlet, and then stop the
imp and ascertain that there is no leak for
minute. For components after the pump,
iply a slight positive pressure and check
r leaks by applying a liquid (detergent in
iter, for example) at each joint. Bubbling
dicates the presence of a leak.
7.1.2 System Performance. Since the
mplete system is calibrated following each
st, the precise calibration of each compo-
:nt is not critical. However, these compo-
«ts should be verified to be operating
•operly. This verification can be performed
' observing the response of flowmeters or
the GC output to changes In flow rates or
libration gas concentrations and ascer-
ining the response to be within predicted
nits. In any component, or if the complete
stem fails to respond in a normal and pre-
ctable manner, the source of the discrep-
icy should be identified and corrected
fore proceeding.
8. Calibration. Prior to any sampling run,
librate the system using the following
•ocedures. (If more than one run is per-
rmed during any 24-hour period, a calibra-
>n need not be performed prior to the
cond and any subsequent runs. The cali-
ation must, however, be verified as pre-
ribed In Section 10, after the last run
ade within the 24-hour period.)
B.I General Considerations. This section
itlines steps to be followed for use of the
C/FPD and the dilution system. The pro-
dure does not include detailed instruc-
>ns because the operation of these systems
complex, and it requires a understanding
the individual system being used. Each
stem should include a written operating
ajiual describing In detail the operating
ocedures associated with each component
the measurement system. In addition, the
•erator should be familiar with the operat-
g principles of the components; particular-
the GC/FPD. The citations in the Bib-
igraphy at the end of this method are rec-
omended for review for this purpose.
B.2 Calibration Procedure. Insert the per-
eation tubes into the tube chamber.
leek the bath temperature to assure
reement with the calibration temperature
the tubes within ±0.1' C. Allow 24 hours
r the tubes to equilibrate. Alternatively
uillbration may be verified by injecting
triples of calibration gas at 1-hour inter-
is. The permeation tubes can be assumed
have reached equilibrium when consecu-
re hourly samples agree within the preci-
>n limits of Section 4.1.
Vary the amount of air flowing over the
bes to produce the desired concentrations
r calibrating the analytical and dilution
stems. The air flow across the tubes must
all times exceed the flow requirement of
e analytical systems. The concentration In
xts per million generated by a tube con-
ining a specific permeant can be calculat-
as follows: p
r
c • "HE
Equation 16-)
where:
C= Concentration of permeant produced in
ppm.
Pr=Permeation rate of the tube in pg/min.
M=Molecular weight of the permeant (g/g-
mole).
L=Flow rate, 1/min, of air over permeant @
20' C, 760 mm Hg.
K=Gas constant at 20* C and 760 mm
Hg= 24.04 1/gmole.
8.3 Calibration of analysis system. Gen-
erate a series of three or more known con-
centrations spanning the linear range of the
FPD (approximately 0.05 to 1.0 ppm) for
each of the four major sulfur compounds.
Bypassing the dilution system, but using
the SOZ scrubber. Inject these
standards into the GC/FPD analyzers and
monitor the responses. Three injects for
each concentration must yield the precision
described in Section 4.1. Failure to attain
this precision is an indication of a problem
in the calibration or analytical system. Any
such problem must be identified and cor-
rected before proceeding.93
8.4 Calibration Curves. Plot the GC/FPD
response in current (amperes) versus their
causative concentrations in ppm on log-log
coordinate graph paper for each sulfur com-
pound. Alternatively, a least squares equa-
tion may be generated from the calibration
data.
8.5 Calibration of Dilution System. Gen-
erate a known concentration of hydrogen
sulfide using the permeation tube system.
Adjust the flow rate of diluent air for the
first dilution stage so that the desired level
of dilution is approximated. Inject the dilut-
ed calibration gas into the GC/FPD system
and monitor Its response. Three Injections
for each dilution must yield the precision
described In Section 4.1. Failure to attain
this precision in this step is an indication of
a problem in the dilution system. Any such
problem must be Identified and corrected
before proceeding. Using the calibration
data for H>S (developed under 8.3) deter-
mine the diluted calibration gas concentra-
tion in ppm. Then calculate the dilution
factor as the ratio of the calibration gas
concentration before dilution to the diluted
calibration gas concentration determined
under this paragraph. Repeat this proce-
dure for each stage of dilution required. Al-
ternatively, the GC/FPD system may be
calibrated by generating a series of three or
more concentrations of each sulfur com-
pound and diluting these samples before in-
jecting them into the GC/FPD system. This
data will then serve as the calibration data
for the unknown samples and a separate de-
termination of the dilution factor will not
be necessary. However, the precision re-
quirements of Section 4.1 are still applica-
ble.
9. Sampling and Analysis Procedure.
9.1 Sampling. Insert the sampling probe
into the test port making certain that no di-
lution air enters the stack through the port.
Begin sampling and dilute the sample ap-
proximtely 8:1 using the dilution system.
Note that the precise dilution factor is that
which is determined In paragraph 8.5. Con-
dition the entire system with sample for a
minimum of 15 minutes prior to commenc-
ing analysis.
9.2 Analysis. Aliquots of dilut-
ed sample pass through the SOi scrub-
ber, and then are injected into the
GC/FPD analyzer for analysis/?3
9.2.1 Sample Run. A sample "run is com-
posed of 16 individual analyses (injects) per
formed over a period of not less than 3
hours or more than 6 hours.
9.2.2 Observation for Clogging of Prjbt
If reductions in sample concentrations are
observed during a sample run that cannot
be explained by process conditions, the sam
pling must be interrupted to determine if
the sample probe is clogged with paniculate
matter. If the probe is found to be clogged.
the test must be stopped and the results up
to that point discarded. Testing may resume
after cleaning the probe or replacing it with
a clean one. After each run, the sample
probe must be inspected and, if necessary,
dismantled and cleaned.
10. Post-Test Procedures.
10.1 Sample line loss. A known concen-
tration of hydrogen sulfide at the level of
;•:: applicable standard, ± 20 percent, m >
be introduced into the sampling system in
sufficient quantities to insure that there is
an excess of sample which must be vented
to the atmosphere. The sample must be in-
troduced Immediately after the probe and
filter and transported through the remain-
der of the sampling system to the measure-
ment system in the normal manner. The re-
sulting measured concentration should be
compared to the known value to determine
the sampling system loss.91
For sampling losses greater than 20 per-
cent in a sample run, the sample run is not
to be used when determining the arithmetic
mean of the performance test. For sampling
losses of 0-20 percent, the sample concen-
tration must be corrected by dividing the
sample concentration by the fraction of re-
covery. The fraction of recovery is equal to
one minus the ratio of the measured con-
centration to the known concentration of
hydrogen sulfide in the sample line loss pro-
cedure. The known gas sample may be gen-
erated using permeation tubes. Alternative-
ly, cylinders of hydrogen sulfide mixed in
air may be used provided they are traceable.
to permeation tubes. The optional pretest
procedures provide a good guideline for de-
termining if there are leaks in the sampling
system.91
10.2 Recalibration. After each run, or
after a series of runs made within a 24-hour
period, perform a partial recalibration using
the procedures In Section 8. Only H,S *oi
other permeant) need be used to recalibrate
the GC/FPD analysis system (8.3) and the
dilution system (8.5).
10.3 Determination of Calibration Drift.
Compare the calibration curves obtained
prior to the runs, to the calibration cunes
obtained under paragraph 10.1. The calibra
tion drift should not exceed the limits set
forth Insubsection4.2. If the drift exceed*
this limit, the Intervening run or runs
should be considered not valid. The tester.
however, may instead have the option of
choosing the calibration data set which
would give the highest sample values. 93
11. Calculations.
11.1 Determine the concentrations of
each reduced sulfur compound detected di-
rectly from the calibration curves. Alterna-
tively, the concentrations may be calculated
using the equation for the least square line.
11.2 Calculation of TRS. Total reduced
sulfur will be determined for each anaylsis
made by summing the concentrations of
each reduced sulfur compound resolved
J i-ing a given analysis.
TRS = J (H.S. MeSH, DMS. 2DMDS)ci
Equation 16 2
Ill-Appendix A-84
-------
where:
TRS = Total reduced sulfur la ppm, wet
basis.
HdS = Hydrogen sulfide, ppm.
MeSH = Methyl mercaptan. ppm.
DMS = Dimethyl sulfide, ppm.
DMDS = Dimethyl disulfide. ppm.
d = Dilution factor, dlmensionless.
11.3 Average TRS. The average TRS will
be determined as follows:
N
r TRS
Average TRS=
Average TRS = Average total reduced suflur
in ppm, dry basis.
TRS,=Total reduced sulfur In ppm as deter-
mined by Equation 16-2.
N = Number of samples.
B,re=Praction of volume of water vapor in
the sas stream as determined by Refer
encemeli.ta t -Determination of 93
Moisture In Stack Gases (36 FR 24887).
11.4 Average concentration of Individual
reduced sulfur compounds.
N
I S-
i =
N
Equation 16-3
where:
S, = Concentration of any reduced sulfur
compound from the ith sample injec-
tion, ppm.
C = Average concentration of any one of the
reduced sulfur compounds for the entire
run, ppm.
N = Number of injections in any run period.
12. Example System. Described below is a
system utilized by EPA in gathering NSPS
data. This system does not now reflect all
the latest developments in equipment and
column technology, but it does represent
one system that has been demonstrated to
work.
12.1 Apparatus.
12.1.1 Sampling System.
12.1.1.1 Probe. Figure 16-1 Illustrates the
probe used in lime kilns and other sources
where significant amounts of particulate
matter are present, the probe is designed
with the deflector shield placed between the
sample and the gas inlet holes and the glass
wool plugs to reduce clogging of the filter
and possible adsorption of sample gas. The
exposed portion of the probe between the
sampling port and the sample line is heated
with heating tape.
12.1.1.2 Sample Lane Vi« inch inside diam-
eter TeHon tubing, heated to 120' C. This
temperature is controlled by a thennostatic
heater.
12.1.1.3 Sample Pump. Leakless Teflot
coated diaphragm type or equivalent. Th
pump head is heated to 120' C by enclosint
It in the sample dilution box (12.1.2.4below).
12.1.2 Dilution System. A schematic dia-
gram of the dynamic dilution system is
given in Figure 16-2. The dilution system is
constructed such that all sample contacts
are made of inert materials. The dilution
system which is heated to 120' C must be ca-
pable of a minimum of 9:1 dilution of
sample. Equipment used in the dilution
system Is listed below: 93
12.1.2.1 Dilution Pump. Model A-150
Kohmyhr Teflon positive displacement
type, nonadjustable 150 cc/mln. ±2.0 per-
cent, or equivalent, per dilution stage. A 9:1
dilution of sample is accomplished by com-
bining ISO cc of sample with 1,350 cc of
clean dry air as shown in Figure 16-2.
12.1.2.2 Valves. Three-way Teflon sole-
noid or manual type.
12.1.2.3 Tubing. Teflon tubing and fit-
tings are used throughout from the sample
probe to the OC/FPD to present an inert
surface for sample gas,
12.1.2.4 Box. Insulated "box, heated and
maintained at 120' C, of sufficient dimen-
sions to house dilution apparatus.
12.1.2.5 Flowmeters. Rotameters or
equivalent to measure flow from 0 to 1500
m! 'min ±1 percent per dilution stage.
i:.i.3 SO: Scrub-
ber. Midget impinger with 15 ml of po-
tassium citrate buffer to absorb SO, in
the sampJp. 93
12.1.4 Gas Chromatograph Column;-
Two types oi columns are used for separa
tlon of low and high molecular weigh;
sulfur compounds: 93
12.1.4.1 Low Molecular Weight Sulfur
Compounds Column GC/FPD-I.93
12.1.4.1.ISsparatlori Column. 11 m by 2.16
mm (36 ft by 0.085 in) inside diameter
Teflon tubing packed with 30/60 mesh
Teflon coated with 5 percent polyphenyl
ether and 0.05 percent orthophosphoric
acid, or equivalent (see Figure 16-3).
12.1.4.1.2 Stripper or Precolumn. 0.6 m
by 2.16 mm (2 ft by 0.085 in) inside diameter
Teflon tubing.93
12.1.4.1.3 Sample Valve. Teflon 10-port
gas sampling valve, equipped with a 10 ml
sample loop, actuated by compressed air
(Figure 16-3 ).93
12.1.4.1.4 Oven. For containing sample
valve, stripper column and separation
column. The oven should be capable of
maintaining an elevated temperature rang-
ing from ambient to 100' C, constant within
±rc. 93
12.1.4.1.5 Temperature Monitor. Thermo
couple pyrometer to measure column oven,
detector, and exhaust temperature ±1* C.93
12.1.4.1.6 Flow System. Gas metering
system to measure sample flow, hydrogen
flow, and oxygen flow (and nitrogen carrier
Bras flow).93
12.1.4.1.7 Detector. Flame photometric
detector.93
12.1.4.1.8 Electrometer. Capable of full
scale amplification of linear ranges of 10-°
to 10-' amperes full scale.93
12.1.4.1.9 Power Supply. Capable of deli-
vering up to 750 volts.93
12.1.4.1.10 Recorder. Compatible with
the output voltage range of the electrom-
eter.93
12.1.4.2 High Molecular Weight Com-
pounds Column (GC/FPD-II).93
12.1.4.2.1. Separation Column. 3.05 m by
2.16 mm (10 ft by 0.0885 in) inside diameter
Teflon tubing packed with 30/60 mesh
Teflon coated with 10 percent Triton Z-305.
or equivalent.93
12.1.4.2.2 Sample Valve. Teflon 6-port gas
sampling valve equipped with a 10 ml
sample loop, actuated by compressed air
(Figure 16-3).93
12.1.4.2.3 Other Components. All compo-
nents same as in 12.1.4.1 5 to 12.1.4.1.10.
12.J 5 Calibration Permeation tubp
system 'figure 16-4).93
12.1.5 1 Tube Chamber. Glass chamber
of suflicient dimensions to house perme-
ation tubes.93
12.1.5.2 Mass Flowmeters. Two mass
flowmeters in the range 0-3 1/min. and 0-10
1/min. to measure air flow over permeation
tubes at ±2 percent. These flowmeters shal
be cross-calibrated at the betjinnlns of eacl
test. Using a convenient flow rate In tn<
measuring range of both flowmeters, es
and monitor the flow rate of BBS over th<
permeation tubes. Injection of calibratlor
gas generated at this flow rate as measure*
by one flowmeter followed by Injection o:
calibration gas at the same flow rate as mea
sured by the other flowmeter should agret
within the specified precision limits. If the}
do not, then there is a problem with th«
mass flow measurement. Each mass flow
meter shall be calibrated prior to the first
test with a wet test meter and thereafter, at
least once each year.
12.1.5.3 Constant Temperature Bath. Ca-
pable of maintaining permeation tubes at
certification temperature of 30* C. within
±0.1' C.
13.2 Reagents
12.2.1 Fuel. Hydrogen (H«) prepurlfied
jrrade or better.
12.2.2. Combustion Gas. Oxygen (O.) re-
search purity or better.
12.2.3 Carrier Gas. Nitrogen (N,) prepuri-
f led grade or better.
12.2.4 Diluent. Air containing less than
50 ppb total sulfur compounds and less than
10 ppm each of moisture and total hydro-
carbons, and filtered using MSA filters
46727 and 79030, or equivalent. Removal of
sulfur compounds can be verified by inject-
ing dilution air only, described in Section
8.3.
12.2.5 Compressed Air. 80 psig for GC
valve actuation.
12.2.6 Calibrated Gases. Permeation
tubes gravimetrically calibrated and certi-
fied at 30.0' C.
12.2.7 Citrate
Buffer. Dissolve 300 grams of potas-
sium citrate and 41 grams of anhy-
drous citric acid in 1 liter of deionized
water. 284 grams of sodium citrate
may be substituted for the potassium
citrate. 93
12.3 Operating Parameters.
12.3.1 Low-Molecular Weight Sulfur
Compounds. The operating parameters for
the GC/FPD system used for low molecular
weight compounds are as follows: nitrogen
carrier gas flow rate of 50 cc/min, exhaust
temperature of 110' C, detector temperature
of 105' C, oven temperature of 40' C, hydro-
sen flow rate of 80 cc/min, oxygen flow rate
of 20 cc/mln, and sample flow rate between
20 and 80 cc/mln.
12.3.2 High-Molecular "Weight Sulfur
Compounds. The operating parameters for
the GC/FPD system for high molecular
weight compounds are the same as in 12.3.1
except: oven temperature of 70* C, and ni-
trogen carrier gas flow of 100 cc/min.
12.4 Analysis Procedure.
12.4.1 Analysis. Aliquots of diluted
sampje are injected simultaneously Into
both GC/FPD analyzers for analysis. GC/
FPD-I is used to measure the low-molecular
weight reduced sulfur compounds. The low
molecular weight compounds include hydro-
gen sulfide, methyl mercaptan, and di-
methyl sulfide. GC/FPD-II is used to re-
solve the high-molecular weight compound.
The high-molecular weight compound is di-
methyl disulfide.
12.4.1.1 Analysis of Low-Molecular
Weight Sulfur Compounds. The sample
valve is actuated for 3 minutes in which
time an aliquot of diluted sample is injected
Into the stripper column and analytical
column. The valve is then deactivated for
approximately 12 minutes In which time,
the analytical column continues to be fore-
Ill-Appendix A-85
-------
flushed, the stripper column is backflushed.
and the sample loop is refilled. Monitor the
responses. The elution time for each com-
pound will be determined during calibra-
tion.
12.4.1.2 Analysis of High-Molecular
Weight Sulfur Compounds. The procedure
Is essentially the same as above except that
no stripper column Is needed.
13. Bibliography.
13.1 O'Keeffe, A. E. and O. C. Ortman.
"Primary Standards for Trace Oas Analy-
sis." Analytical Chemical Journal, 38,760
(1966).
13.2 Stevens, R. K., A. E. O'Keeffe, and
O. C. Ortman. "Absolute Calibration of a
Flame Photometric Detector to Volatile
Sulfur Compounds at Sub-Part-Per-Mlllion
Levels." Environmental Science and Tech-
nology. 3:7 (July, 1969).
13.3 Mulick, J. D., R. K. Stevens, and R.
Baumgardner. "An Analytical System De-
signed to Measure Multiple Malodorous
Compounds Related to Kraft Mill Activi-
ties." Presented at the 12th Conference on
13.6 General Reference. Standard Meth-
ods of Chemical Analysis Volume III A and
B Instrumental Methods. Sixth Edition.
Van Nostrand Reinhold Co 93
Methods in Air Pollution and Industrial Hy
Siene Studies, University of Southern Cali
fornia, Los Angeles, CA. April 6-8. 1971.
13.4 Devonald, R. H., R. S. Serenius, and
A. D. Mclntyre. "Evaluation of the Flame
Photometric Detector for Analysis of Sulfur
Compounds." Pulp and Paper Magazine of
Canada. 73,3 (March. 1972).
13.5 Grimley, K. W., W. S. Smith, and R.
•A. Martin. "The Use of a Dynamic Dilution"
System in the Conditioning of Stack Gases
or Automated Analysis by a Mobile Sam-
>ling Van." Presented at the 63rd Annual
VPCA Meeting in St. Louis. Mo. June 14-19,
970.
en
•D
o
-------
~f
PROSE
FILTER
(GLASS WOOL)
*"%
X
SJACK TO GC/FPD ANALYZERS
10:1 10*:1
I
FILTER
i
i
i
£ HEATED |
H SAMPLE i
1 LINE 1
'O
3 \
&
H-
1
00
1
i
PuSi'fiVE
DISPLACEMENT
- PUMP
(1 50 ce/min) -~
| V
PERMEATION , |[
TUBE 1 **'
CALIBRATION i
GAS 1
II '
1
I
1
|
1
f \ ** 1
>~^ !
DIAPHRAGM 1
PUMP
(HEATED)
V,
i
-»S~*v
r
\
/
J V
N
C
r
v
/
i
^
•v
I
—
_
^
)
\
3
DILUENT AIR
-WAY
.v VALVE _
/ \s
or
I **
1350 ec/mir
1
n n
X I
till
l_J LJ
i
i*
25PSI
CLEAN
DRY AIR
~ DilUTicTBoTHEATED
TO 100°C
FLOWMETER
VENT
Figure 16-2.Sampling and dilution apparatus.
-------
SAMPLING VALVE
GC/FPD-I
H
H
I
(D
3
O-
H-
SAMPLE
LOOP
SAMPLE
OR
CALIBRATION
GAS
STRIPPER
MM!
•*5>-VENT
SEPARATION
COLUMN
"2 *»
OVEN
FLAME PHOTOMETRIC DETECTOR
EXHAUST
750V
POWER SUPPLY
00
00
SAMPLING VALVE FOR
GC/FPD-II
VACUUM
SAMPLE-"-:
03
CALIBRATION
GAS
N2
CARRIER
Figure 16-3. Gas chrcmatographic-f lame'photometric analyzers..
-------
TO INSTRUMENTS
AND
U 1 b U 1 1 U II
I
CONSTANT
TEMPERATURE
BATH
Q i O 1 CIVI
i
THERMOMETER
(L
^
\
>
\
VJjj,.
a
0
\
7
V.
— ^
•-^S
PERMEATION
TUBE
-^
1
i
1
<;
K^_
g
FLOWMETER
SI
IRRI
1® °"
i
^
xC^J
^^•S
^^^
nnicn
:R
^
GLASS
CHAMBER
DILUENT
NITROGEN
Figure 16-4. Apparatus for field calibration.
Ill-Appendix A-89
-------
k
Q*
H-
I
O
VENT'
VENT
1
ea O
o
PROBE
SAMPLE
LINE
SAMPLE
PUMP
DILUTION
SYSTEM
VENT
GAS
CHROMATOGRAPH
Figure 16-5. Determination of sample line loss.
-------
METHOD 17. DETERMINATION OT PARTICULATE
EMISSIONS FROM STATIONARY SOURCES (IN-
STACK FILTRATION METHOD) 82
Introduction
Particulale matter is not an absolute
quantity; rather, it is a function of tempera-
ture and pressure. Therefore, to prevent
variability in paniculate matter emission
regulations and/or associated test methods.
the temperature and pressure at which par-
ticulate matter is to be measured must be
carefully defined. Of the two variables (I.e.,
temperature and pressure), temperature has
the greater effect upon the amount of par-
ticulate matter in an effluent gas stream; in
most stationary source categories, the effect
of pressure appears to be negligible.
In method 5. 250* F is established as a
nominal reference temperature. Thus,
where Method 5 is specified in an applicable
subpart of the standards, paniculate matter
is defined with respect to temperature. In
order to maintain a collection temperature
of 250* F. Method 5 employs a heated glass
sample probe and a heated filter holder.
This equipment Is somewhat cumbersome
and requires care in its operation. There-
fore, where paniculate matter concentra-
tions (over the normal range of temperature
associated with a specified source category)
are known to be independent of tempera-
ture, it is desirable to eliminate the glass
probe and heating systems, and sample at
•tack temperature.
This method describes an in-stack sam-
pling system and sampling procedures for
use in such cases. It Is intended to be used
only when specified by an applicable sub-
part of the standards, and only within the
applicable temperature limits (if specified),
or when otherwise approved by the Admin-
istrator.
1. Principle and Applicability.
1.1 Principle. Particulate matter is with-
drawn isokinetically from the source and
collected on a glass fiber filter maintained
at stack temperature. The particulate mass
is determined grav.metrically after removal
of uncombined water.
1.2 Applicability. This method applies to
the' determination of particulate emissions
from stationary sources for determining
compliance with new source performance
standards, only when specifically provided
for in an applicable subpart of the stan-
dards. This method is not applicable to
stacks that contain liquid droplets or are
saturated with water vapor. In addition, this
method shall not be used as written if the
projected cross-sectional area of the probe
extension-filter holder assembly covers
more than 5 percent of the stack cross-sec-
tional area (see Section 4.1.2).
2. Apparatus.
2.1 Sampling Train. A schematic of the
sampling train used in this method is shown
in Figure 17-1. Construction details for
many, but not all. of the train components
are given in APTD-0581 (Citation 2 in Sec-
tion 7); for changes from the APTD-0581
document and for allowable modifications
to Figure 17-1, consult with the Administra-
tor.
Ill-Appendix A-91
-------
TEMPERATURE
SENSOR
IN STACK
FILTER HOLDER
x.y > 1.9em (0.75in.)*
IMPINGER TRAIN OPTIONAL. MAY Bf REPLACED
BY AN EQUIVALENT CONDENSER
z>7.6 cm (3 in.)'
H
H
(0
3
0-
H-
vo
to
TYPES
PITOT TUBE
TEMPERATURE
SENSOR
SAMPLING
NOZZLE
IN STACK
FILTER
HOLDER
REVERSE TYPE
PITOT TUBE
THERMOMETER
CHECK
VALVE
ORIFICE MANOMETER
• SUGGESTED (INTERFERENCE FREE) SPACINGS
THERMOMETERS ,Mp,NGERS
VACUUM
LINE
AIR-TIGHT
PUMP
DRY GAS METER
Figure 17-1. Particulate-Sampling Train. Equipped with tn-Stack Filter.
-------
The operating and maintenance proce-
dures for many of the sampling train com-
ponents are described in APTD-0576 (Cita-
tion 3 in Section 7). Since correct usage is
Important In obtaining valid results, all
users should read the APTD-0576 document
and adopt the operating and maintenance
procedures outlined in it, unless otherwise
specified herein. The sampling train con-
sists of the following components:
2.1.1 Probe Nozzle. Stainless steel (316)
or glass, with sharp, tapered leading edge.
The angle of taper shall be 030° and the
taper shall be on the outside to preserve a
constant internal diameter. The probe
nozzle shall be of the button-hook or elbow
design, unless otherwise specified by the Ad-
ministrator. If made of stainless steel, the
nozzle shall be constructed from seamless
tubing. Other materials of construction may
be used subject to the approval of the Ad-
ministrator.
A range of sizes suitable for Isoklnetic
sampling should be available, e.g., 0.32 to
1.27 cm (W> to Vt in)—or larger if higher
volume sampling trains are used—inside di-
ameter (ID) nozzles in increments of 0.16 cm
(Vio in). Each nozzle shall be calibrated ac-
cording to the procedures outlined in Sec-
tion 5.1.
2.1.2 Filter Holder. The in-stack filter
holder shall be constructed of borosilicate
or quartz glass, or stainless steel; if a gasket
is used, it shall be made of sllicone rubber,
Teflon, or stainless steel. Other holder and
gasket materials may be used subject to the
approval of the Administrator. The filter
bolder shall be designed to provide a posi-
tive seal against leakage from the outside or
around the filter.
2.1.3 Probe Extension. Any suitable rigid
probe extension may be used after the filter
holder.
2.1.4 Pilot Tube. Type S, as described In
Section 2.1 of Method 2, or other device ap-
proved by the Administrator: the pilot tube
shall be attached to the probe extension to
allow constant monitoring of the stack gas
velocity (see Figure 17-1). The impact (high
pressure) opening plane of the pitol tube
shall be even wilh or above the nozzle entry
plane during sampling (see Method 2,
Figure 2-6b). II is recommended: (1) that
the pitol tube have a known baseline coeffi-
cient, determined as outlined in Section 4 of
Method 2; and (2) that <3iis known coeffi-
cient be preserved by placing the pilot lube
In an interference-free arrangement with re-
spect lo Ihe sampling nozzle, filler holder,
and lemperature sensor (see Figure 17-1).
Note that the 1.9 cm (0.75 in) free-space be-
tween the nozzle and pilot tube shown in
Figure 17-1. is based on a 1.3 cm (0.5 in) ID
nozzle. If the sampling train is designed for
sampling at higher flow rates than that, de-
scribed in APTD-0581, thus necessitating
the use of larger sized nozzles, Ihe free-
space shall be 1.9 cm (0.75 in) wilh Ihe larg-
est sized nozzle in place.
Source-sampling assemblies lhat do nol
meel Ihe minimum spacing requirements of
Figure 17-1 (or the equivalent of Ihese re-
quirements, e.g.. Figure 2-7 of Melhod 2)
may be used; however, Ihe pilot tube coeffi-
cienls of such assemblies shall be deler-
mined by calibration, using methods subjecl
to the approval of Ihe Adminislrator.
2.1.5 Differential Pressure Gauge. In-
clined manometer or equivalent device
(Iwo), as described in Seclion 2.2 of Melhod
2. One manomeler shall be used for velocity
head (Ap) readings, and the other, for ori-
fice differential pressure readings.
2.1.6 Condenser. It is recommended that
the impinger system described in Melhod 5
be used lo delermine the moisture content
of the stack gas. Alternatively, any system
that allows measurement of both the water
condensed and the moisture leaving Ihe con-
denser, each to within 1 ml or 1 g, may be
used. The moisture leaving the condenser
can be measured either by: (1) monitoring
the temperature and pressure at the exit of
the condenser and using Dalton's law of
partial pressures; or (2) passing the sample
eras stream Ihrough a silica gel trap with
exit gases kept below 20' C (68* F) and de-
termining the weight gain.
Flexible tubing may be used between the
probe extension and condenser. If means
other lhan silica gel are used to delermine
the amount of moisture leaving the con-
denser, it is recommended thai silica gel still
be used between the condenser system and
pump to prevent moisture condensation in
Ihe pump and metering devices and lo avoid
the need to make corrections for moisture
In the metered volume.
2.1.7 Metering System. Vacuum trauge,
leak-free pump, thermometers capable of
measuring temperature to within 3' C (5.4€
F). dry gas meter capable of measuring
volume to within 2 percent, and related
equipment, as shown in Figure 17-1. Other
metering systems capable of maintaining
sampling rales wllhin 10 percenl of Isoklne-
tic and of determining sample volumes to
within 2 percent may be used, subject to the
approval of the Adminislralor. When the
melering syslem is used in conjunclion wilh
a pilot tube, the system shall enable checks
of isokinetic rales.
Sampling trains utilizing metering sys-
tems designed for higher flow rates than
thai described in APTD-0581 or APTD-0576
may be used provided that the specifica-
tions of this method are met.
2.1.8 Baromeler. Mercury, aneroid, or
olher barometer capable of measuring at-
mospheric pressure lo within 2.5 mm Hg
(0.1 in. Hg). In many cases, Ihe baromelric
reading may be obtained from a nearby na-
tional weather service station, In which case
the station value (which is the absolute
barometric pressure) shall be requested and
an adjustment, for elevation differences be-
tween the weather stalion and sampling
point shall be applied al a rale of minus 2.5
mm Hg (0.1 in. Hg) per 30 m (100 fl) eleva-
lion increase or vice versa for elevalion de-
crease.
2.1.9 Gas Densily Determination Equip-
ment. Temperalure sensor and pressure
gauge, as described in Sections 2.3 and 2.4 of
Method 2, and gas analyzer, if necessary, as
described in Method 3.
The lemperalure sensor shall be attached
to either the pitol lube or to the probe ex-
tension, in a fixed configuration. If the lem-
perature sensor is attached In the field; the
sensor shall be placed in an Interference-
free arrangement with respect to the Type
S pilol lube openings (as shown in Figure
17-1 or in Figure 2-7 of Melhod 2). Allerna-
tively. the temperalure sensor need nol be
attached to either the probe extension or
pilot tube during sampling, provided that a
difference of not more than 1 percenl in Ihe
average velocily measurement is inlroduced.
This alternative is subjecl to the approval
of the Administrator.
2.2 Sample Recovery.
2.2.1 Probe Nozzle Brush. Nylon bristle
brush with stainless steel wire handle. The
brush shall be properly sized and shaped lo
brush out the probe nozzle.
2.2.2 Wash Bottles—Two. Glass wash
bottles are recommended; polyethylene
wash bottles may be used at the option of
the tester. It is recommended that acetone
nol be stored in polyethylene bottles for
longer than a month.
2.2.3 Glass Sample Storage Containers.
Chemically resistant, borosilicate glass bot-
tles, for acetone washes, 500 ml or 1000 ml.
Screw cap liners shall either be rubber-
backed Teflon or shall be conslnicled so as
to be leak-free and resistant to chemical
atlack by acetone. (Narrow moulh glass bot-
tles have been found to be less prone to
leakage.) Alternatively, polyethylene bottles
may be used.
2.2.4 Petrl Dishes. For filler samples;
glass or polyelhylene, unless olherwise
specified by Ihe Adminislralor.
2.2.5 Graduated Cylinder and/or Bal-
ance. To measure condensed waler lo wilhin
1 ml or 1 g. Graduated cylinders shall have
subdivisions no greater than 2 ml. Mosl lab-
oratory balances are capable of weighing to
the nearest 0.5 g or less. Any of these bal-
ances Is suitable for use here and in Section
2.3.4.
2.2.6 Plastic Storage Containers. Air
tight containers to store silica gel.
2.2.7 Funnel and Rubber Policeman. To
aid in transfer of silica gel to container; not
necessary if'silica gel is weighed in the field.
2.2.8 Funnel. Glass or polyethylene, to
aid in sample recovery.
2.3 Analysis.
2.3.1 Glass Weighing Dishes.
2.3.2 Desiccator.
2.3.3 Analytical Balance. To measure to
within 0.1 mg.
2.3.4 Balance. To measure to within 0.5
mg.
2.3.5 Beakers. 250 ml.
2.3.6 Hygrometer. To measure the rela-
tive humidity of the laboratory environ-
ment.
2.3.7 Temperature Gauge. To measure
the temperalure of Ihe laboratory environ-
menl.
3. Reagents.
3.1 Sampling.
3.1.1 Filters. The in-slack filters shall be
glass mats or thimble fiber fillers, without
organic binders, and shall exhibit at least
99.95 percent efficiency (00.05 percent pene-
tration) on 0.3 micron dioctyl phlhalale
smoke particles. The filler efficiency lests
shall be conducted In accordance with
ASTM standard method D 2986-71. Tesl
dala from Ihe supplier's qualily conlrol pro-
gram are sufficienl for Ihis purpose.
3.1.2 Silica Gel. Indicaling lype, 6- to 16-
mesh. If previously used, dry al 175' C (350'
F) for 2 hours. New silica gel may be used as
received. Allemalively, olher lypes of deslc-
cants (equivalent or better) may be used.
subject to the approval of the Administra-
tor.
3.1.3 Crushed Ice.
3.1.4 Stopcock Grease. Acetone-insoluble.
heat-stable sllicone grease. This is not nec-
essary if screw-on connectors with Teflon
sleeves, or similar, are used. Alternatively.
other lypes'Of stopcock grease may be used.
subjecl to Ihe approval of the Administra-
tor.
3.2 Sample Recovery. Acetone, reagent
(Trade, 00.001 percent residue, in glass bot-
tles. Acetone from melal containers general-
ly has a high residue blank and should not
be used. Sometimes, suppliers transfer ac-
etone to glass bottles from melal containers.
Thus, acetone blanks shall be run prior to
field use and only acetone with low blank
Ill-Appendix A-93
-------
values (00.001 percent) shall be used. In no
case shall a blank value of greater than
0.001 percent of the weight of acetone used
be subtracted from the sample weight.
3.3 Analysis.
3.3.1 Acetone. Same as 3.2.
3.3.2 Desiccant. Anhydrous calcium sul-
fate, indicating type. Alternatively, other
types of desiccants may be used, subject to
the approval of the Administrator.
4. Procedure.
4.1 Sampling. The complexity of this
method is such that, In order to obtain reli-
able results, testers should be trained and
experienced with the test procedures.
4.1.1 Pretest Preparation. All compo-
nents shall be maintained and calibrated ac-
cording to the procedure described in
APTD-0576, unless otherwise specified
herein.
Weigh several 200 to 300 g portions of
silica gel in air-tight containers to the near-
est 0.5 g. Record the total weight of the
silica gel plus container, on each container.
As an alternative, the silica gel need not be
preweighed, but may be weighed directly in
its Impinger or sampling holder just prior to
train assembly.
Check filters visually against light for ir-
regularities and flaws or plnhole leaks.
Label filters of the proper size on the back
side near the edge using numbering ma-
chine ink. As an alternative, label the ship-
ping containers (glass or plastic petri dishes)
and keep the filters in these containers at
all times except during sampling and weigh-
ing.
Desiccate the filters at 20±5.6' C (68±10'
F) and ambient pressure for at least 24
hours and weigh at intervals of at least 6
hours to a constant weight, i.e., 00.5 mg
change from previous weighing; record re-
sults to the nearest 0.1 mg. During each
weighing the filter must not be exposed to
the laboratory atmosphere for a period
greater than 2 minutes and a relative hu-
midity above 50 percent. Alternatively
(unless otherwise specified by the Adminis-
trator), the filters may be oven dried at 105*
C (220* F) for 2 to 3 hours, desiccated for 2
hours, and weighed. Procedures other than
those described, which account for relative
humidity effects, may be used, subject to
the approval of the Administrator.
4.1.2 Preliminary Determinations. Select
the sampling site and the minimum number
of sampling points according to Method 1 or
as specified by the Administrator. Make a
projected-area model of the probe exten-
sion-filter holder assembly, with the pilot
tube face openings positioned along the cen-
terline of the stack, as shown in Figure 17-2.
Calculate the estimated cross-section block-
age, as shown in Figure 17-2. If the blockage
exceeds 5 percent of the duct cross sectional
area, the tester has the following options:
(Da suitable out-of-stack filtration method
may be used instead of in-stack filtration; or
(2) a special in-stack arrangement, in which
the sampling and velocity measurement
sites are separate, may be used; for details
concerning this approach, consult with the
Administrator (see also Citation 10 in Sec-
tion 7). Determine the stack pressure, tem-
perature, and the range of velocity heads
using Method 2; it is recommended that a
leak-check of the pilot lines (see Method 2,
Section 3.1) be performed. Determine the
moisture' content using Approximation
Method 4 or its alternatives for the purpose
of making isokinetic sampling rate settings.
Determine the stack gas dry molecular
weight, as described in Method 2, Section
8.6; if Integrated Method 3 sampling is used
for molecular weight determination, the in-
tegrated bag sample shall be taken simulta-
neously with, and for the same total length
of time'as, the particular sample run.
STACK
WALL
IN STACK FILTER
PROBE EXTENSION
ASSEMBLY
ESTIMATED
BLOCKAGE
fsHADED AREA]
|_ DUCT AREA J
X 100
Figure 172. Proiected-area model of cross-section blockage
(approximate average for 9 sample traverse) caused by an
in-stack filter holder-probe extension assembly.
Ill-Appendix A-94
-------
Select a nozzle size based on the range of
velocity heads, such- that it is not necessary
to change the nozzle size in order to main-
tain isokinetic sampling rates. During the
run, do not change the nozzle size. Ensure
that the proper differential pressure gauge
is chosen for the range of velocity heads en-
countered (see Section 2.2 of Method 2).
Select a probe extension length such that
all traverse points can be sampled. For large
stacks, consider sampling from opposite
sides of the stack to reduce the length of
probes.
Select a total sampling time greater than
or equal to the minimum total sampling
time specified in the test procedures for the
specific industry such that (1) the sampling
time per point is not less than 2 minutes (or
some greater time interval if specified by
the Administrator), and (2) the sample
volume taken (corrected to standard condi-
tions) will exceed the required minimum
total gas sample volume. The latter is based
on an approximate average sampling rate.
It is recommended that the number of
minutes sampled at each point be an integer
or an integer plus one-half minute, in order
to avoid timekeeping errors.
In some circumstances, e.g., batch cycles,
it may be necessary to sample for shorter
times at the traverse points and to obtain
smaller gas sample volumes. In these cases,
the Administrator's approval must first be
obtained.
4.1.3 Preparation of Collection Train.
During preparation and assembly of the
sampling train, keep all openings where con-
tamination can occur covered until just
prior to assembly or until sampling is about
to begin.
If impingers are used to condense stack
gas moisture, prepare them as follows: place
100 ml of water in each of the first two im-
pingers, leave the third impinger empty,
and transfer approximately 200 to 300 g of
preweighed silica gel from its container to
the fourth impinger. More silica gel may be
used, but care should be taken to ensure
that it is not entrained and carried out from
the impinger during sampling. Place the
container in a clean place for later use in
the sample recovery. Alternatively, the
weight of the silica gel plus impinger may
be determined to the nearest 0.5 g and re-
corded.
If some means other than impingers is
used to condense moisture, prepare the con-
denser (and, if appropriate, silica gel for
condenser outlet) for use.
Using a tweezer or clean disposable surgi-
cal gloves, place a labeled (identified) and
weighed filter in the filter holder. Be sure
that the filter is properly centered and the
gasket properly placed so as not to allow the
sample gas stream to circumvent the filter.
Check filter for tears after assembly is com-
pleted. Mark the probe extension with heat
resistant tape or by some other method to
denote the proper distance into the stack or
duct for each sampling point.
Assemble the train as in Figure 17-1, using
a very light coat of sllicone grease on all
ground glass joints and greasing only the
outer portion (see APTD-0576) to avoid pos-
sibility of contamination by the silicone
grease. Place crushed ice around the im-
pingers.
4.1.4 Leak Check Procedures.
4.1.4.1 Pretest Leak-Check. A pretest
leak-check is recommended, but not re-
quired. If the tester opts to conduct the pre-
test leak-check, the following procedure
shall be used.
After the sampling train has been assem-
bled, plug the inlet to the probe nozzle with
a material that will be able to withstand the
stack temperature. Insert the filter holder
into the stack and wait approximately 5
minutes (or longer, If necessary) to allow
the system to come to equilibrium with the
temperature of the stack gas stream. Turn
on the pump and draw a vacuum of at least
380 .mm Hg (15 in. Hg); note that a lower
vacuum may be used, provided that it is not
exceeded during the test. Determine the
leakage rate. A leakage rate in excess of 4
percent of the average sampling rate or
0.00057 m'/min. (0.02 cfm), whichever is
less, is unacceptable.
The following leak-check instructions for
the sampling train described in APTD-0576
and APTD-0581 may be helpful. Start the
pump with by-pass valve fully open and
coarse adjust valve completely closed. Par-
tially open the coarse adjust valve and
slowly ..close the by-pass valve until the de-
sired vacuum is reached. Do not reverse di-
rection of by-pass valve. If the desired
vacuum is exceeded, either leak-check at
this higher vacuum or end the leak-check as
shown below and start over.
When the leak-check is completed, first
slowly remove the plug from the inlet to the
probe nozzle and immediately turn off the
vacuum pump. This prevents water from
being forced backward and keeps silica gel
from being entrained backward.
4.1.4.2 Leak-Checks During Sample Run.
If. during the sampling run, a component
(e.g., filter assembly or impinger) change be-
comes necessary, a leak-check shall be con-
ducted immediately before the change is
made. The leak-check shall be done accord-
Ing to the procedure outlined in Section
4.1.4.1 above, except that it shall be done at
a vacuum equal to or greater than the maxi-
mum value recorded up to that point in the
test. If the leakage rate is found to be no
greater than 0.00057 m'/min (0.02 cfm) or 4
percent of the average sampling rate
(whichever is less), the results are accept-
able, and no correction will need to be ap-
plied to the total volume of dry gas metered;
if, however, a higher leakage rate is ob-
tained, the tester shall either record the
leakage rate and plan to -correct the sample
volume as shown in Section 6.3 of this
method, or shall void the sampling run.
Immediately after component changes,
teak-checks are optional; if such leak-checks
are done, the procedure outlined in Section
4.1.4.1 above shall be used.
4.1.4.3 Post-Test Leak-Check. A leak-
check is mandatory at the conclusion of
each sampling run. The leak-check shall be
done in accordance with the procedures out-
lined in Section 4.1.4.1, except that it shall
be conducted at a vacuum equal to or great-
er than the maximum value reached during
the sampling run. If the leakage rate is
found to be no greater than 0.00057 m'/min
(0.02 cfm) or 4 percent of the average sam-
pling rate (whichever is less), the results are
acceptable, and no correction need be ap-
plied to the total volume of dry gas metered.
If, however, a higher leakage rate is ob-
tained, the tester shall either record the
leakage rate and correct the sample volume
as shown in Section 6.3 of this method, or
ahall void the sampling run.
4.1.5 Particulate Train Operation.
During the sampling run, maintain a sam-
pling rate such that sampling is within 10
percent of true isokinetic, unless otherwise
specified by the Administrator.
For each run, record the data required on
the example data sheet shown in Figure 17-
3. Be sure to record the initial dry gas meter
reading. Record the dry gas meter readings
at the beginning and end of each sampling
time increment, when changes in flow rates
are made, before and after each leak check,
and when sampling is halted. Take other
readings required by Figure 17-3 at least
once at each sample point during each time
increment and additional readings when sig-
nificant changes (20 percent variation in ve-
locity head readings) necessitate additional
adjustments in flow rate. Level and zero the
manometer. Because the manometer level
and zero may drift due to vibrations and
temperature changes, make periodic checks
during the traverse.
Ill-Appendix A-95
-------
PLANT
LOCATION.
OPERATOR.
DATE
RUN NO
SAMPLE BOX NO..
METER BOX N0._
METERAH@
CFACTOR
PITOT TUBE COEFFICIENT, Cp.
BAROMETRIC PRESSURE
ASSUMED MOISTURE, %
PROBE EXTENSION LENGTH, m(ft.)
NOZZLE IDENTIFICATION NO
AVERAGE CALIBRATED NOZZLE DIAMETER cm (in.).
FILTER NO
LEAK RATE, m3/min,(cfm)
STATIC PRESSURE, mm Hg (in. Hg)
SCHEMATIC OF STACK CROSS SECTION
TRAVS.flSC POfiVf
NUMBER
TOTAL
SAMPLING
TIME
(9). min.
AVERAGE
VACUUM
mm Hg
(in. Hg)
STACK
TEMPERATURE
Jty
°C (*F)
VELOCITY
HEAD
(APS>,
mm H20
(in. H20)
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METER,
mm H20
(in. HjO)
GAS SAMPLE
VOLUME.
m3 (ft3)
GAS SAMPLE TEMPERATURE
AT DRY GAS METER
INLET,
°C (°F)
Avc]
OUTLET,
°C (°F)
Avc)
Avg
TEMPERATURE
OF GAS
LEAVING
CONDENSER OR
LASTIMPINGER
°C (°F)
H
M
I
13
(D
3
X
>
VD
Figure 17-3. Participate field data.
-------
Clean the portholes prior to the test run
to minimize the chance of sampling the de-
posited material. To begin sampling, remove
the nozzle cap and verify that the pilot tube
and probe extension are properly posi-
tioned. Position the nozzle at the first tra-
verse point with the tip pointing directly
into the gas stream. Immediately start the
pump and adjust the flow to isokinetic con-
ditions. Nomographs are available, which
aid in the rapid adjustment to the isokinetic
sampling rate without excessive computa-
tions. These nomographs are designed for
use when the Type S pilot tube coefficient
is 0.85 ±0.02, and the stack gas equivalent
density (dry molecular weight) is equal to
29±4. APTD-0576 details the procedure for
using the nomographs. If Cp and Ma are out-
side the above stated ranges, do not use the
nomographs unless appropriate steps (see
Citation 7 in Section 7) are taken to com-
pensate for the deviations.
When the stack Is under significant nega-
tive pressure (height of impinger stem),
take care to close the coarse adjust valve
before inserting the probe extension assem-
bly into the stack to prevent water from
being forced backward. If necessary, the
pump may be turned on with the coarse
adjust valve closed.
When the probe is in position, block off
the openings around the probe and porthole
to prevent unrepresentalive dilution of the
gas stream.
Traverse the stack cross section, as re-
quired by Method 1 or as specified by the
Administrator, being careful not to bump
the probe nozzle into the stack walls when
sampling near the walls or when removing
or inserting the probe extension through
the portholes, to minimize chance of ex-
tracting deposited material.
During the test run. take appropriate
steps (e.g., adding crushed ice to the im-
pinger ice bath) to maintain a temperature
of less than 20' C (.66' P) at the condenser
outlet; Ihis will prevenl excessive moisture
losses. Also, periodically check the level and
zero of the manometer.
If the pressure drop across the filter be-
comes too high, making isokinetic sampling
difficult to maintain, the filter may be re-
placed in the midst of a sample run. It is
recommended that another complete filter
holder assembly be used rather than at-
tempting to change the filter itself. Before a
new filter holder is installed, conduct a leak
check, as outlined in Section 4.1.4.2. The
total particulate weight sball include the
summation of all filter assembly catches.
A single train shall be used for the entire
sample run, except in cases where simulta-
neous sampling is required in two or more
separate ducts or at two or more different
locations within the same duct, or, in cases
where equipment failure necessitates a
change of trains. In all other situations, the
use of two or more trains will be subject to
the approval of the Administrator. Note
that when two or more trains are used, a
separate analysis of the collected particu-
late from each train shall be performed,
unless identical nozzle sizes were used on all
trains, in which case the particulate catches
from the individual trains may be combined
and a single analysis performed.
At the end of the sample run, turn off the
' pump, remove the probe extension assembly
from the stack, and record the final dry gas
meter reading. Perform a leak-check, as out-
lined in Section 4.1.4.3. Also, leak-check the
pilot lines as described in Section 3.1 of
Method 2; the lines must pass Ihis leak-
check, in order to validate the velocity head
data.
4.1.6 Calculation of Percent Isokinetic.
Calculate percent isokinetic (see Section
6.11) to determine whether another test run
should be made. If there is difficulty in
maintaining Isokinetic rates due to source
conditions, consult with the Administrator
for possible variance on the Isokinetic rates.
4.2 Sample Recovery. Proper cleanup
procedure begins as soon as the probe ex-
tension assembly is removed from the stack
at the end of the sampling period. Allow the
assembly to cool.
When the assembly can be safely handled.
wipe off all external paniculate matter near
the tip of the probe nozzle and place a cap
over it to prevent losing or gaining partlcu-
late matter. Do not cap off the probe tip
tightly while the sampling train is cooling
down es this would create a vacuum in the
filter holder, forcing condenser water back-
ward.
Beforo moving the cample train to the
cleanup site, disconnect the filter holder-
probe nozzle assembly from the probe ex-
tension: cap the open inlet of the probe ex-
tension. Be careful not to lose any conden-
sate, if present. Remove the umbilical cord
from the condenser outlet and cap the
outlet. If a flexible line is used between the
first impinger (or condenser) and the probe
extension, disconnect the line at the probe
extension and let any condensed water or
liquid drain into the impingers or condens-
er. Disconnect the probe extension from the
condenser; cap the probe extension outlet.
After wiping off the silicone grease, cap off
the condenser inlet. Ground glass stoppers,
plastic caps, or serum caps (whichever are
appropriate) may be used to close these
openings.
Transfer both the filter holder-probe
nozzle assembly and the condenser to the
cleanup area. This area should be clean and
protected from the wind so that the chances
of contaminating or losing the sample will
be minimized.
Save a portion of the acetone used for
cleanup as a blank. Take 200 ml of this ac-
etone directly from the wash bottle being
used and place it in a glass sample container
labeled "acetone blank."
• Inspect the train prior to and during dis-
assembly and note any abnormal conditions.
Treat the samples as follows:
Container No. 1. Carefully remove the
filter from the filter holder and place it in
its Identified petri dish container. Use a pair
of tweezers and/or clean disposable surgical
gloves to handle the filter. If it is necessary
to fold the filter, do so such that the partic-
ulate cake is inside the fold. Carefully trans-
fer to the petri dish any particulate matter
and/or filter fibers- which adhere to the
filter holder gasket, by using a dry Nylon
bristle brush and/or a sharp-edged blade.
Seal the container.
Container No, 2. Taking care to see that
dust on the outside of the probe nozzle or
other exterior surfaces does not get into the
sample, quantitatively, recover particulate
matter or any condensate from the probe
nozzle, fitting, and front half of the filter
holder by washing these components with
acetone and placing the wash in a glass con-
tainer. Distilled water may be used instead
of acetone when approved by the Adminis-
trator and shall be used when specified by
the Administrator: in these cases, save a
water blank and follow Administrator's di-
rections on analysis. Perform the acetone
rinses as follows:
Carefully remove the probe nozzle and
clean the inside surface by rinsing with ac-
etone from a wash bottle and brushing with
a Nylon bristle brush. Brush until acetone
rinse shows no visible particles, after which
make a final rinse of the inside surface with
acetone.
Brush and rinse with acetone the inside
parts of the fitting in a similar way until no
visible particles remain. A funnel (glass or
polyethylene) may be used to aid in trans-
ferring liquid washes to the container. Rinse
the brush with acetone and quantitatively
collect these washings in the sample con-
tainer. Between sampling runs, keep
brushes clean and protected from contami-
nation.
After ensuring that all joints are wiped
clean of silicone grease (If applicable), clean
the Inside of the front half of the filter
holder by rubbing the surfaces with a Nylon
bristle brush and rinsing with acetone.
Rinse each surface three tiroes or more If
needed to remove visible particulate. Make
final rinse of the brush and filter holder.
After all acetone washings and particulate
matter are collected in the sample contain-
er, tighten the lid on. the sample container
so that acetone will not leak out when it is
shipped to the laboratory. Mark the height
of the fluid level to determine whether or
not leakage occurred during transport.
Label the container to clearly identify its
contents.
Container No. 3. if silica gel is used in the
condenser system for mositure content de-
termination, note the color of the gel to de-
termine if it has been completely spent;
make a notation of its condition. Transfer
the silica gel back to its original container
and seal. A funnel may make it easier to
pour the silica gel without spilling, and a
rubber policeman may be used as an aid in
removing the silica gel. It is not necessary to
remove the small amount of dust particles
that may adhere to the walls and are diffi-
cult to remove. Since the gain in weight is to
be used for moisture calculations, do not use
any water or other liquids to transfer the
silica gel. If a balance Is available in the
field, follow the procedure for Container
Wo. 3 under "Analysis."
Condenser Water. Treat the condenser or
impinger water as follows: make a notation
of any color or film in the liquid catch Mea-
sure the liquid volume to within ±1 .A! by
using a graduated cylinder or, if a balance is
available, determine the liquid weight to
within ±0.5 g. Record the total volume or
weight of liquid present. This information is
required to calculate the moisture content
of the effluent gas. Discard the liquid after
measuring and recording the volume or
weight.
4.3 Analysis. Record the data required on
the example sheet shown in Figure 17-4.
Handle each sample container as follows:
Container No. 1. Leave the contents in the
shipping container or transfer the filter and
any loose particulate from the sample con-
tainer to a tared glass weighing dish. Desic-
cate for 24 hours in a desiccator containing
anhydrous •calcium sulfate. Weigh to a con-
stant weight and report the results to the
nearest 0.1 mg. For purposes of this Section,
4.3, the term "constant weight" means a dif-
ference of no more than 0.5 mg or 1 percent
of total weight less tare weight, whichever is
greater, between two consecutive weighings,
with no less than 6 hours of desiccation
time between weighings.
Alternatively, the sample may be oven
dried at the average stack temperature or
Ill-Appendix A-9 7
-------
05* C (220' P>. whichever is less, for 2 to 3
ours, cooled in the desiccator, and weighed
> a constant weight, unless otherwise speci-
ied by the Administrator. The tester may
Iso opt to oven dry the sample at the aver-
«e stack temperature or 105' C (220* F).
whichever is less, tor 2 to 3 hours, weigh the
ample, and use this weight as a final
reight.
Plant.
Date.
Run No..
Filter No.
Amount liquid lost during transport
Acetone blank volume, ml
Acetone wash volume, ml
Acetone black concentration, mg/mg (equation 174)
Acetone wash blank, mg (equation 17-5)
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED.
mg
FINAL WEIGHT
^>*~
-------
Container No. 2. Note the level of liquid in
the container and confirm on the analysis
sheet whether or .not leakage occurred
during transport. If a noticeable amount of
leakage has occurred, either void the sample
or use methods, subject to the approval of
the Administrator, to correct the final re-
sults. Measure the liquid in this container
either volumetrically to ±1 ml or gravime-
trically to ±0.5 g. Transfer the contents to a
tared 250-ml beaker and evaporate to dry-
ness at ambient temperature and pressure.
Desiccate for 24 hours and weigh to a con-
stant weight. Report the results to the near-
est 0.1 mg.
Container No. 3. This step may be con-
ducted in the field. Weigh the spent silica
gel (or silica gel plus impinger) to the near-
est 0.5 g using a balance.
"Acetone Blank" Container. Measure ac-
etone in this container either volumetrically
or gravimetrically. Transfer the acetone to a
tared 250-ml beaker and evaporate to dry-
ness at ambient temperature and pressure.
Desiccate for 24 hours and weigh to a con-
stant weight. Report the results to the near-
est 0.1 mg..
NOTE.—At the option of the tester, the
contents of Container No. 2 as well as the
acetone blank container may be evaporated
at temperatures higher than ambient. If
evaporation is done at an elevated tempera-
ture, the temperature must be below the
boiling point of the solvent; also, to prevent
"bumping," the evaporation process must be
closely supervised, and the contents of the
beaker must be swirled occasionally to
maintain an even temperature. Use extreme
care, as acetone is highly flammable and
has a low flash point.
5. Calibration. Maintain a laboratory log
of all calibrations.
5.1 Probe Nozzle. Probe nozzles shall be
calibrated before their initial use in the
field. Using a micrometer, measure the
inside diameter of the nozzle to the nearest
0.025 mm (0.001 in.). Make three separate
measurements using different diameters
each time, and obtain the average of the
measurements. The difference between the
high and low numbers shall not exceed 0.1
mm H0.004 in.). When nozzles become
nicked, dented, or corroded, they shall be
reshaped, sharpened, and recalibrated
before use. Each nozzle shall be permanent-
ly and uniquely identified.
5.2 Pitot Tube. If the pilot tube is placed
in an interference-free arrangement with re-
spect to the other probe assembly compo-
nents, its baseline (isolated tube) coefficient
shall be determined as outlined in Section 4
of Method 2. If the probe assembly is not in-
terference-free, the pilot tube assembly co-
efficient shall be determined by calibration,
using methods subject to the approval of
the Administrator.
5.3 Metering System. Before its Initial
use in the field, the metering system shall
be calibrated according to the procedure
outlined in APTD-0576. Instead of physical-
ly adjusting the dry gas meter dial readings
to correspond to the wet test meter read-
ings, calibration factors may be used to
mathematically correct the gas meter dial
readings to Ihe proper values.
Before calibrating the metering system, it
is suggested that a leak-check be conducted.
For metering systems having diaphragm
pumps, the normal leak-check procedure
will not detect leakages within the pump.
For these cases the following leak-check
procedure is suggested: make a 10-minute
calibration run at 0.00057 m'/min (0.02
cfm); at the end of the run, take the differ-
ence of the measured wet test meter and
dry gas meter volumes; divide the difference
by 10, to get the leak rate. The leak rate
should not exceed 0.00057 m'/min (0.02
cfm).
After each field use, the calibration of the
metering system shall be checked by per-
forming three calibration runs at a single,
intermediate orifice setting (based on the
previous field test), with the vacuum set at
the maximum value reached during the test
series. To adjust the vacuum, insert a valve
between the wet test meter and the inlet of
the metering syslem. Calculale the average
value of the calibration factor. If the cali-
bration has changed by more than 5 per-
cent, recalibrate the meter over the full
range of orifice settings, as outlined in
APTD-0576.
Allemative procedures, e.g., using Ihe ori-
fice meter coefficients, may be used, subject
to the approval of the Administrator.
NOTE.—If the dry gas meter coefficient
values obtained before and after a test
series differ by more than 5 percent, the
test series shall either be voided, or calcula-
tions for the test series shall be performed
using whichever meter coefficient value
(i.e., before or after) gives the lower value of
total sample volume.
5.4 Temperature Gauges. Use the proce-
dure in Section 4.3 of Method 2 to calibrate
in-stack temperature gauges. Dial thermom-
eters, such as are used for Ihe dry gas meter
and condenser outlet, shall be calibrated
against mercury-in-glass thermometers.
5.5 Leak Check of Metering System
Shown in Figure 17-1. That portion of the
sampling train from the pump to the orifice
meter should be leak checked prior to initial
use and after each shipment. Leakage after
the pump will result in less volume being re-
corded than is actually sampled. The follow-
ing procedure is suggested (see Figure 17-5).
Close the main valve on the meter box.
Insert a one-hole rubber stopper with
rubber tubing attached into the orifice ex-
haust pipe. Disconnect and vent the low side
of the orifice manometer. Close off Ihe low
side orifice tap. Pressurize the system to 13
to 18 cm (5 to 7 in.) water column by blow-
ing into Ihe rubber tubing. Pinch off the
tubing and observe the manometer for one
minute. A loss of pressure on the mano-
meter indicates a leak in the meter box;
leaks, if present, must be corrected.
Ill-Appendix A-99
-------
X
o
JD
O)
E
_
I
u
to
01
u
O)
5.6 Barometer. Calibrate against a mer-
cury barometer.
6. Calculations. Carry out calculations, re-
taining at least one extra decimal figure
beyond that of the acquired data. Round off
figures after the final calculation. Other
forms of the equations may be used as long
as they give equivalent results.
6.1 Nomenclature.
Ar=Cross-sectional area of nozzle, m' (ft1).
8,, = Water vapor In the gas stream, propor-
tion by volume.
C.=Acetone blank residue concentration,
mg/g.
c.=Concentration of particulate matter in
stack gas, dry basis, corrected to stan-
dard conditions, g/'dscm (g/dscf).
I=Percent of isokinetic sampling.
1%=Maximum acceptable leakage rate for
either a pretest leak check or for a leak
check following a component change;
equal to 0.00057 mVmin (0.02 cfm) or 4
percent of the average sampling rate.
whichever is less.
L,=Individual leakage rate observed during
the leak check conducted prior to the
"i"1" component change (1=1. 2. 3 ... n),
m'/min (cfm).
1^, = Leakage rate observed during the post-
test leak check, mVmin (cfm).
mn = Total amount of particulate matter col-
lected, mg.
M, = Molecular weight of water. 18.0 g/g-
mole (18.0 Ib/lb-mole).
m. = Mass of residue of acetone after evapo-
ration, mg.
Pb., = Barometric pressure at the sampling
site, mm Hg (in. Hg).
P, = Absolute stack gas pressure, mm Hg (in.
Hg).
P.u! = Standard absolute pressure, 760 mm
Hg (29.92 in. Hg).
R=Ideal gas constant. 0.06236 mm Hg-mV
•K-g-mole (21.85 in. Hg-ftVR-lb-mole).
Tm=Absolute average dry gas meter tem-
perature (see Figure 17-3), 'K (°R).
T,=Absolute average stack gas temperature
(see Figure 17-3), 'K CR>.
TM,, = Standard absolute temperature. 293°K
(528'R).
V. = Volume of acetone blank, ml.
V.» = Volume of acetone used in wash, ml.
V,t=Tota! volume of liquid collected in im-
pingers and silica gel (see Figure 17-4),
ml.
Vm = Volume of gas sample as measured by
dry gas meter, dcm (dcf).
Vm(.u)i=Volume of gas sample measured by
the dry gas meter, corrected to standard
conditions, dscm (dscf).
V«UUL>=Volume of water vapor in the gas
sample, corrected to standard condi-
tions, scm (scf).
v.=Stack gas velocity, calculated by Method
2, Equation 2-9. using data obtained
from Method 17. m/sec (ft/sec).
W.=Weight of residue in acetone wash. mg.
Y = Dry gas meter calibration coefficient.
AH = Average pressure differential across
the orifice meter (see Figure 17-3), mm
H,O (in. H,O).
p. = Density of acetone, mg/ml (see label on
bottle).
=„ = Density of water, 0.9982 g/ml (0.002201
Ib/ml).
e = Total sampling time, min.
e,=Sampling time interval, from the begin-
ning of a run.until the first component
change, min.
6, = Sampling time interval, between two
successive component changes, begin-
ning with the interval between the first
and second char.ges, min.
Ill-Appendix A-100
-------
0,=Sampling time Interval, from the final
(n"1) component change, until the end of
the sampling run, min.
13.6 = Spec\fic gravity of mercury.
60=Sec/min.
100 = Conversion to percent.
6.2 Average dry gas meter temperature
and average orifice pressure drop. See data
sheet (Figure 17-3).
6.3 Dry Gas Volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (20° C, 760 mm Hg or
68* F. 29.92 in. Hg) by using Equation 17-1.
6.6 Acetone Blank Concentration.
P. + (AH/13.6)
s K w V Dar
W r
Equation 17-1
where:
K, = 0.3858' K/mm Hg for metric units;
17.64' R/in. Hg for English units.
NOTE.—Equation 17-1 can be used as writ-
ten unless the leakage rate observed during
any of the mandatory leak checks (i.e., the
post-test leak check or leak checks conduct-
ed prior to component changes) exceeds L..
If Lp or L, exceeds L., Equation 17-1 must be
modified as follows:
(a) Case I. No component changes made
during sampling run. In this case, replace
V, in Equation 17-1 with the expression:
[Vm-(L,-L.)e]
(b) Case II. One or more component
changes made during the sampling run. In
this case, replace Vm in Equation 17-1 by the
expression:
«l - J (L,- - LJ
i=2
Equation 17-4
6.7 Acetone Wash Blank.
W.=C.V.,p.
Equation 17-5
6.8 Total Particulate Weight. Determine
the total particulate catch from the sum of
the weights obtained from containers 1 and
2 less the acetone blank (see Figure 17-4).
NOTE.—Refer to Section 4.1.5 to assist in
calculation of results involving two or more
filter assemblies or two or more sampling
trains.
6.9 Particulate Concentration.
c.=(0.001 g/mg) (mn/VnUM))
Equation 17-6
6.10 Conversion Factors:
Prom
To
Multiply by
scf
B/ff
g/ft'
g/ff
m'
gr/ff
lb/ff
g/m'.
0.02832
15.43
2.205x10-'
35.31
6.11 Isokinetic Variation.
6.11.1 Calculation from Raw Data.
100 Ts [K3V1c + (VJT/T ) (Pbar * AH/13.6H
60
PS An
Equation 17-7
where:
K,=0. 003454 mm Hg-mVml-'K for metric
units: 0.002669 in. Hg-ft'/ml-'R for Eng-
lish units.
V
6.11.2 Calculation
Values.
from Intermediate
1. Addendum to Specifications for Inciner-
ator Testing at Federal Facilities. PHS,
NCAPC. December 6. 1967.
2. Martin, Robert M., Construction Details
of Isokinetic Source-Sampling Equipment.
Environmental Protection Agency. Re-
search Triangle Park, N.C. APTD-0581.
April, 1971.
3. Rom, Jerome J., Maintenance, Calibra-
tion, and Operation of Isokinetic Source-
Sampling Equipment. Environmental Pro-
tection Agency. Research Triangle Park.
N.C. APTD-0576. March, 1972.
4. Smith, W. S.. R. T. Shigehara. and W.
F. Todd. A Method of Interpreting Stack
Sampling Data. Paper Presented at the 63rd
Annual Meeting of the Air Pollution Con-
trol Association, St. Louis, Mo. June 14-19,
1970.
5. Smith, W. S., et al.. Stack Gas Sampling
Improved and Simplified with New Equip-
ment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at
Federal Facilities. PHS. NCAPC. 1967.
7. Shigehara, R. T., Adjustments in the
EPA Nomograph for Different Pitot Tube
Coefficients and Dry Molecular Weights.
Stack Sampling News 2:4-11. October. 1974.
8. Vollaro, R. F., A Survey of Commercial-
ly Available Instrumentation for the Mea-
surement of Low-Range Gas Velocities. U.S.
Environmental Protection Agency, Emission
Measurement Branch. Research Triangle
Park. N.C. November. 1976 (unpublished
paper).
9. Annual Book of ASTM Standards. Part
26. Gaseous Fuels; Coal and Coke; Atmo-
spheric Analysis. American Society for Test-
Ing and Materials. Philadelphia, Pa. 1974.
pp. 617-622.
10. Vollaro. R. P., Recommended Proce-
dure for Sample Traverses In Ducts Smaller
than 12 Inches In Diameter v.s. environ-
mental Protection Ap^ncy, Emission Mea-
surement Branch. .Research Triangle Park,
N.C. November, )*76.
(Sec. 114. Clean Air Act if amended (42
U.S.C. 7414)).6883
and substitute only for those leakage rate'
(L, "r IT,> which exceed L,.
6.4 Volume of water vapor.
'.<.«• •.«(»)••»•.«
Equation 17-2
where:
K,=0.001333 m'/ml for metric units: 0.04707
ft Vml for English units.
6.5 Moisture Content.
B
Vw(std)
ws " Vm(std) + Vw(std)
Equation 17-3
I
. Ts
'std
- K
^4 jr
Vm(std)Pstd 10°
vs e An Ps 60 {1"Bws;
Ts Vm(std)
vs An 6 ^-BWS'
Equation 17-8
where:
K. = 4.320 for metric units; 0.09450 for Eng-
lish units.
G.i2 . tcceplabie Results. If 90 percent
010110 percent, the results are acceptable. If
the re:-alts are low in comparison to the
stivnda •:.' and I is beyond the acceptable
range, c-:. if I is less than 90 percent, the Ad-
ministrator may opt to accept the results.
Use Citation 4 in Section 7 to make judg-
ments. Otherwise, reject the results and
repeat the test.
7. Bibliography.
Ill-Appendix A-101
-------
Method19. Determination of Sulfur
Dioxide Removal Efficiency and
Particulate, Sulfur Dioxide and Nitrogen
Oxides Emission Rates From Electric
Utility Steam Generators 98
1. Principle and Applicability
4..1 Principle.
1.1.1 Fuel samples from before and
after fuel pretreatment systems are
collected and analyzed for sulfur and
heat content, and the percent sulfur
dioxide (ng/Joule, Ib/million Btu)
reduction is calculated on a dry basis.
(Optional Procedure.)
1.1.2 Sulfur dioxide and oxygen or
carbon dioxide concentration data
obtained from sampling emissions
upstream and downstream of sulfur
dioxide control devices are used to
calculate sulfur dioxide removal
efficiencies. (Minimum Requirement.) As
an alternative to sulfur dioxide
monitoring upstream of sulfur dioxide
control devices, fuel samples may be
collected in an as-fired condition and
analyzed for sulfur and heat content.
(Optional Procedure.)
1.1.3 An overall sulfur dioxide
emission reduction efficiency is
calculated from the efficiency of fuel
pretreatment systems and the efficiency
of sulfur dioxide control devices.
1.1.4 Particulate, sulfur dioxide,
nitrogen oxides, and oxygen or carbon
dioxide concentration data obtained
from sampling emissions downstream
from sulfur dioxide control devices are
used along with F factors to calculate
particulate, sulfur dioxide, and nitrogen
oxides emission rates. F factors are
values relating combustion gas volume
to the heat content of fuels.
1.2 Applicability. This method is
applicable for determining sulfur
removal efficiencies of fuel pretreatment
and sulfur dioxide control devices and
the overall reduction of potential sulfur
dioxide emissions from electric utility
steam generators. This method is also
applicable for the determination of
particulate, sulfur dioxide, and nitrogen
oxides emission rates.
2. Determination of Sulfur Dioxide
Removal Efficiency of Fuel
Pretreatment Systems
2.1 Solid Fossil Fuel.
2.1.1 Sample Increment Collection.
Use ASTM D 2234', Type I, conditions
A, B, or C, and systematic spacing.
Determine the number and weight of
increments required per gross sample
representing each coal lot according to
Table 2 or Paragraph 7.1.5.2 of ASTM D
2234'. Collect one gross sample for each
raw coal lot and one gross sample for
each product coal lot.
2.1.2 ASTM Lot Size. For the purpose
of Section 2.1.1, the product coal lot size
is defined as the weight of product coal
produced from one type of raw coal. The
raw coal lot size is the weight of raw
coal used to produce one product coal
lot. Typically, the lot size is the weight
of coal processsed in a 1-day (24 hours)
period. If more than one type of coal is
treated and produced in 1 day. then
gross samples must be collected and
analyzed for each type of coal. A coal
lot size equaling the 90-day quarterly
fuel quantity for a specific power plant
may be used if representative sampling
can be conducted for the raw coal and
product coal.
Note.—Alternate definitions of fuel lot
sizes may be specified subject to prior
approval of the Administrator.
2.1.3 Cross Sample Analysis.
Determine the percent sulfur content
(%S) and gross calorific value (GCV) of
the solid fuel on a dry basis for each
gross sample. Use ASTM 2013 ' for
sample preparation, ASTM D 3177 ' for
sulfur analysis, and ASTM D 3173 ' for
moisture analysis. Use ASTM D 3176 •
for gross calorific value determination.
2.2 Liquid Fossil Fuel.
2.2.1 Sample Collection. Use ASTM
D 270 ' following the practices outlined
• for continuous sampling for each gross
sample representing each fuel lot.
2^2 Lot Size. For the purposes of
Section 2.2.1, the weight of product fuel
from one pretreatment facility and
intended as one shipment (ship load,
barge load, etc.] is defined as one
product fuel lot. The weight of each
crude liquid fuel type used to produce
one product fuel lot is defined as one
inlet fuel lot.
Note.— Alternate definitions of fuel lot
sizes may be specified subject to prior
approval of the Administrator.
Note.— For the purposes of this method,
raw or inlet fuel (coal or oil) is defined as the
fuel delivered to the desulhirization
pretreatment facility or to the steam
generating plant. For pretreated oil the input
oil to the oil desulfurization process (e.g.
hydrotreatment emitted) is sampled.
2.2.3 Sample Analysis. Determine
the percent sulfur content (%S) and
gross calorific value (GCV). Use ASTMD
240 ' for the sample analysis. This value
can be assumed to be on a dry basis.
2.3 Calculation of Sulfur Dioxide
Removal Efficiency Due to Fuel
Pretreatment. Calculate the percent
sulfur dioxide reduction due to fuel
pretreatment using the following
equation:
*VGCVo
100
Where:
%Ri=Sulfur dioxide removal efficiency due
pretreatment; percent.
%S0=Sulfur content of the product fuel lot on
a dry basis; weight percent.
%S,=Sulfur content of the inlet fuel lot on a
dry basis; weight percent.
GCV0=Gross calorific value for the outlet
fuel lot on a dry basis; kj/kg (Btu/lb).
GCV|=Gross calorific value for the inlet fuel
lot on a dry basis; kj/kg (Btu/lb).
Note.—If more than one fuel type is used to
produce the product fuel, use the following
equation to calculate the sulfur contents per
unit of heat content of the total fuel lot, %S/
GCV:
IS/GCV
n
.1
k-1
t(*Sk/GCVk)
Where:
Yk=The fraction of total mass input derived
from each type, k, of fuel.
%Sfc=Sulfur content of each fuel type, k,'on a
dry basis; weight percent
GCVk=Gross calorific value for each fuel
type, k, on a dry basis; kj/kg (Btu/lb).
n=The number of different types of fuels.
1 Use the moil recent revision or designation of
the ASTM procedure f pecified
1 Use the most recent revision or designation of
the ASTM procedure specified.
Ill-Appendix A-102
-------
3. Determination of Sulfur Removal
Efficiency of the Sulfur Dioxide Control
Device
3.1 Sampling. Determine SO2
emission rates at the inlet and outlet of
the sulfur dioxide control system
according to methods specified in the
applicable subpart of the regulations
and the procedures specified in Section
5. The inlet sulfur dioxide emission rate
may be determined through fuel analysis
(Optional, see Section 3.3.)
3.2. Calculation. Calculate the
percent removal efficiency using the
following equation:
.
9(m)
100
Where:
KRc = Sulfur dioxide removal efficiency of
the sulfur dioxide control system using
inlet and outlet monitoring data; percent.
E.O „=Sulfur dioxide emission rate from the
outlet of the sulfur dioxide control
system; ng/J (Ib/million Btu).
" Eu i=Sulfur dioxide emission rate to the
outlet of the sulfur dioxide control
system; ng/J (Ib/million Btu).
3.3 As-fired Fuel Analysis (Optional
Procedure). If the owner or operator of
an electric utility steam generator
chooses to determine the sulfur dioxide
irnput rate at the inlet to the sulfur .
dioxide control device through an as-
fired fuel analysis in lieu of data from a
sulfur dioxide control system inlet gas
monitor, fuel samples must be collected
in accordance with applicable
paragraph in Section 2. The sampling
can be conducted upstream of any fuel
processing, e.g., plant coal pulverization.
For the purposes of this section, a fuel
lot size is defined as the weight of fuel
consumed in 1 day (24 hours) and is
directly related to the exhaust gas
monitoring data at the outlet of the
sulfur dioxide control system.
3.3.1 Fuel Analysis. Fuel samples
must be analyzed for sulfur content and
gross calorific value. The ASTM
procedures for determining sulfur
content are defined in the applicable
paragraphs of Section 2.
3.3.2 Calculation of Sulfur Dioxide
Input Rate. The sulfur dioxide imput rate
determined from fuel analysis is
calculated by:
2.0(XSf) ,
Is • s(iv T x 10' for S. I. units.
2.0(tSf) .
scv T x 10 for English units.
Where:
I * Sulfur dioxide Input rate from as-fired fuel analysis,
ng/J (Ib/m11l1on Btu).
IS. • Sulfur content of as-fired fuel, on a dry basis; weight
percent.
GCV • Gross calorific value for as-fired fuel, on a dry basis;
kJ/kg (Btu/lb).
3.3.3 Calculation of Sulfur Dioxide 3.3.2 and the sulfur dioxide emission
Emission Reduction Using As-fired Fuel rate, ESO», determined in the applicable
Analysis. The sulfur dioxide emission paragraph of Section 5.3. The equation
reduction efficiency is calculated using f°r. sulfur dioxide emission reduction
the sulfur imput rate from paragraph ' efficiency is:
«g(f) -100 x (1.0 -
Where:
XR >.< • Sulfur dioxide removal efficiency of the sulfur
dioxide control system using as-f1red fuel analysis
data; percent.
Eso •,Sulfur dioxide emission'rate from sulfur dioxide control
-»U2
system; ng/J (Ib/million Btu).
I$ • Sulfur dioxide Input rate from as-fired fuel analysis;
ng/J (Ib/m1l11on Btu).
Ill-Appendix A-103
-------
4. Calculation of Overall Reduction in
Potential Sulfur Dioxide Emission
4.1 The overall percent sulfur
dioxide reduction calculation uses the
sulfur dioxide concentration at the inlet
to the sulfur dioxide control device as
Where:
the base value. Any sulfur redaction
realized through fuel cleaning is
.introduced into the equation as an
average percent reduction, XRf.
4.2 Calculate the overall percent
sulfur reduction as:
O.o-
%RQ • Overall sulfur dioxide reduction; percent.
XR- • Sulfur dioxide removal efficiency of fuel pretreatment
from Section 2; percent. Refer to applicable subpart
for definition of applicable averaging period.
SR • Sulfur dioxide removal efficiency of sulfur dioxide control
device either 0. or CO. - based calculation or calculated
frost fuel analysts and emission data, from Section 3;
percent. Refer to applicable subpart for definition of
applicable averaging period.
5. Calculation of Particulate, Sulfur
Dioxide, and Nitrogen Oxides Emission
Rates
and oxygen concentrations have been
determined in Section 5.1, wet or dry F
factors are used. (Fw) factors and
associated emission calculation
procedures are not applicable and may
not be used after wet scrubbers; (FJ or
(Fd) factors and associated emission
calculation procedures are used after
wet scrubbers.] When pollutant and
carbon dioxide concentrations have
been determined in Section 5.1. Fc
factors are used.
5.2.1 Average F Factors. Table 1
shows average Fd, F,, and Fc factors
(scm/J, scf/miUion Btu) determined for
commonly used fuels. For fuels not
listed in Table 1, the F factors are
calculated according to the procedures
outlined in Section 5.2.2 of this section.
S.2.2 Calculating an F Factor. If the
fuel burned is not listed in Table 1 or if
the owner or operator chooses to
determine an F factor rather than use
the tabulated data, F factors are
calculated using the equations below.
.The sampling and analysis procedures
followed in obtaining data for these
calculations are subject to the approval
of the Administrator and the
Administrator should be consulted prior
to data collection.
5.1 Sampling. Use the outlet SO* or
Ot or COi concentrations data obtained
in Section 3.1. Determine the particulate,
NO,, and O» or CO. concentrations
according to methods specified in an
applicable subpart of the regulations.
5.2 Determination of an F Factor.
Select an average F factor (Section 5.2.1)
or calculate an applicable F factor
(Section 5.2.2.). If combined fuels are
fired, the selected or calculated F factors
are prorated using the procedures in
Section 5.2.3. F factors are ratios of the
gas volume released during combustion
of a fuel divided by the heat content of
the fuel A dry F factor (FJ is the ratio of
the volume of dry flue gases generated
to the calorific value of the fuel
combusted: a wet F factor (Fw) is the
ratio of the volume of wet flue gases
generated to the calorific value of the
fuel combusted; and the carbon F factor
(FJ is the ratio of the volume of carbon
dioxide generated to the calorific value
of the fuel combusted. When pollutant
For SI Units:
227.0(W) + 9S.7«C) * 35.4(«) + 8.6(«N) - 28.5QO)
GCV
347.4(XH)+95.7(SC)+35.4(IS)+8.6{*N)-28.5(JO)-H3.0(SH20)**
For English Units:
106C5.57(tH) * 1.53(«C) * 0.57(»S) » O.U(M) - 0.46(10)1
- - - -
106[5.57(XHH .53(SC)*0.57(tS)+O.U(SN)-0.46(M)+0.
io6[o.32i(«:n
The »zO tern nay be omitted 1f tH and U Include the unavailable
hydrogen and oxygen In the fore of HO.
Ill-Appendix A-104
-------
Where:
Fa. F0, and Fc have the units of scm/J. or scf/
million Btu: %H, %C. %S, %N, %O, and
%H,O are the concentrations by weight
(expressed in percent) of hydrogen.
carbon, sulfur, nitrogen, oxygen, and
water from en ultimate analysis of the
fuel; and GCV is the gross calorific value
of the fuel in kj/kg or Btu/lb and
consistent with the ultimate analysis.
Follow ASTM D 2015° for solid fuels, D
240* for liquid fuels, and D 1826° for
gaseous fuels as applicable in '
determining GCV.
5.2.3 Combined Fuel Firing F Factor.
For affected facilities firing
combinations of fossil fuels or fossil
fuels and wood residue, the F,j, F0, or F«
factors determined by Sections 5.2.1 or
5.2.2 of this section shall be prorated in
accordance with applicable formula as
follows:
20.9
20.9
rd
fi
I
n
Z sfc
OP
OF
F.
.Where:
»„=The fraction of total heat input derived
from each type of fuel, 1C.
n=The number of fuels being burned in.
combination.
5.3 Calculation of Emission Rate.
Select from the following paragraphs the
applicable calculation procedure and
calculate the participate, SO0, and NOn
emission rate. The values in the
equations are defined as:
E=Pollutant emission rate, ng/) (Ib/million
Btu).
C=Pollutant concentration, ng/scm (H>/scf).
Note.—It io necessary in oome cases to
convert measured concentration uaito to
other units for these calculations.
Use the following table for such,
conversions:
©cmroroten Foctoro te? e®RC3f!ta3H®n
From— To— KuJttpty by—
9/scm
rng/ccm
ppm(SOJ
ppm/(SOo)...<. ___
ppm/(KOJ -------
.... rtg/con..
~ ng/cctn..
ng/ccm..
„. rtg/ccrn-
... rtg/ccm..
_. B>/ccf
_ G)/ccf
10°
10°
2.630x10°
1.812x10°
-1.880x10-'
1.164x10-'
5.3.1 Oxygen-Based F Factor
Procedure.
5.3.1.1 Dry Basis. When both percent
oxygen (%O^ and the pollutant
concentration (C
-------
59 V
Where:
EM=Pollutant emission rate from steam
generator effluent, ng/J (Ib/million Btu).
EC=Pollutant emission rate in combined
cycle effluent: ng/J (Ib/million Btu).
Egt=Pollutant emission rate from gas turbine
effluent; ng/J (Ib/million Btu).
Xw=Fraction of total heat input from
supplemental fuel fired to the steam
generator.
X^=Fraction of total heat input from gas
turbine exhaust gases.
Note.—The total heat input to the steam
generator is the sum of the heat input from
supplemental fuel fired to the steam
generator and the heat input to the steam
generator from the exhaust gases from the
gas turbine.
5.5 Effect of Wet Scrubber Exhaust.
Direct-Fired Reheat Fuel Burning. Some
wet scrubber systems require that the
temperature of the exhaust gas be raised
above the moisture dew-point prior to
the gas entering the stack. One method
used to accomplish this is directfiring of
an auxiliary burner into the exhaust gas.
The heat required for such burners is
from 1 to 2 percent of total heat input of
the steam generating plant. The effect of
this fuel burning on the exhaust gas
components will be less than ±1.0
percent and will have a similar effect on
emission rate'calculations. Because of
this small effect, a determination of
effluent gas constituents from direct-
fired reheat burners for correction of
•tack gas concentrations is not
necessary.
Where:
•.^Standard deviation of the average outlet
hourly average emission rates for the
reporting period; ng/J (Ib/million Btu).
81= Standard deviation of the average inlet
hourly average emission rates for the
reporting period; ng/J (Ib/million Btu).
6.3 Confidence Limits. Calculate the
lower confidence limit for the mean
outlet emission rates for SOi and NO,
and, if applicable, the upper confidence
limit for the mean inlet emission rate for
SOt using the following equations:
T«bte 1»-1.—F Factors for Viriow fuels'
E,*=E,+t».»8,
Where:
EO* s The lower confidence limit for the mean
outlet emission rates; ng/J (Ib/million
Btu).
E,* =The upper confidence limit for the mean
inlet emission rate; ng/J (Ib/million Btu).
U-»= Values shown below for the indicated
number of available data points (n):
F.
F.
F.
Fuel type
dscm
J
dad
10* Btu
10* Btu
tcf
10* Btu
Coal:
Lignite
€••
Gas;
Natural..™ - ........
Propane ...........
Butane
Wood Bark ;
2.71x10-'
2.63x10"'
2.65x10-'
2.47x10-'
2.43x10-'
2.34x10"'
2.34x10-'
__ 2.48x10-'
2.58x10-'
(10100)
(9780)
(9860)
(9190)
(8710)
(8710)
(8710)
(9240) .
(9600) .
2.83X10-'
2.66x10-'
3.21X10-'
2.77x10-'
2.85x10-'
2.74x10-'
2.79x10-'
(10540)
(10640)
(11950)
(10320)
(10810)
(10200)
(10390)
0.530x10-'
0.484X10-'
0.513X10-'
0.383X10-'
0.287X10-*
0.321x10-'
.0.337x10-'
0.492x10-'
0.497X10-'
(1970)
(1600)
(1910)
(1420)
(1040)
(1190)
(1250)
(1830)
(1850)
Values tor V.
•Aadasarfedaccorolng to ASTM 0386-66.
• Crude, residual, or dWfflate.
• Determined at standard conditions: 20' C (68* F) and 760 mm Hg (28.92 tn. Kg).
10
11
12-16
17-21
22-26
27-31
32-51
52-91
92-151
152 or more
6.31
2.42
2.35
213
2.02
1.94
1.89
1.86
1.63
131
1.77
1.73
1.71
1.70
1.68
1.67
1.66
1.65
8. Calculation of Confidence Limits for
Inlet and Outlet Monitoring Data
6.1 Mean Emission Rates. Calculate
the mean emission rates using hourly
averages in ng/J (Ib/million Btu) for SO»
and NO, outlet data and, if applicable,
SO. inlet data using the following
equations:
I X-
6.2 Standard Deviation of Hourly
Emission Rates. Calculate the standard
deviation of the available outlet hourly
average emission rates for SO* and NO,
and, if applicable, the available inlet
hourly average emission rates for SOi
using the following equations:
o
£ X
1
Where:
Eo=Mean outlet emission rate; ng/J (lb/
million Btu).
E,=Mean inlet emission rate; ng/J (Ib/million
Btu).
Xo=Hourly average outlet emission rate; ng/J
Ob/million Btu).
x,=Hourly average in let emission rate; ng/j
(Ib/million Btu).
n,=Number of outlet hourly averages
available for the reporting period.
n,=Number of inlet hourly averages
available for reporting period.
PCC
PCC
Where:
The values of this table are corrected for
n-1 degrees of freedom. Use n equal to
the number of hourly average data
points.
7. Calculation to Demonstrate
Compliance When Available
Monitoring Data Are Less Than the
Required Minimum
7.1 Determine Potential Combustion
Concentration (PCC) for SOt.
7.1.1 When the removal efficiency
due to fuel pretreatment (% R() is
included in the overall reduction in
potential sulfur dioxide emissions (% RJ
and the "as-fired" fuel analysis is not
used, the potential combustion
concentration (PCC) is determined as
follows:
ng/J
1b/m1ll1on Btu.
Potential emissions removed by the pretreatment
process, using the fuel parameters defined In
section 2.3; ng/J (Ib/m11l1on Btu).
Ill-Appendix A-106
-------
7.1.2 When the "as-fired" fuel
analysis is used and the removal
efficiency due to fuel pretreatment (% Rf)
is not included in the overall reduction
in potential sulfur dioxide emissions (%
R0), the potential combustion
concentration (PCC) is determined as
follows:
PCC = I.
PCC
PCC
7.1.4 When inlet monitoring data are
used and the removal efficiency due to
fuel pretreatment (% Rr) is not included
in the overall reduction in potential
sulfur dioxide emissions {% R0), the
potential combustion concentration
(PCC) is determined as follows:
PCC = E,*
Where:
EI* = The upper confidence limit of the mean
inlet emission rate, as determined in
section 6.3.
7.2 Determine Allowable Emission
Rates (£,„).
7.2.1 NO,. Use the allowable
emission rates for NO, as directly
defined by the applicable standard in
terms of ng/J (Ib/million Btn).
7.2.2 SO,. Use the potential
combustion concentration (PCC) for SO»
as determined in section 7.1. to
determine the applicable emission
standard. If the applicable standard is
an allowable emission rate in ng/J (lb/
million Btu), the allowable emission rate
Where:
I, = The sulfur dioxide input rate as defined
in section 3.3
7.1.3 When the "as-fired" fuel
analysis is used and the removal
efficiency due to fuel pretreatment (% Rf)
is included in the overall reduction (%
R0), the potential combustion
concentration (PCC) is determined as
follows:
Ib/mUMon Btu.
is used as E,td. If the applicable standard
is an allowable percent emission,
calculate the allowable emission rate
(lit,,) using the following equation:
E.U = % PCC/100
Where:
% PCC = Allowable percent emission as
defined by the applicable standard;
percent.
7.3 Calculate Eo"lE,ta. To determine
compliance for the reporting period
calculate the ratio:
Where:
E,,* = The lower confidence limit for the
mean outlet emission rates, as defined in
section 6.3; ng/J (Ib/million Btu).
E.U = Allowable emission rate as defined in
section 7.2; ng/J (Ib/million Btu).
If Eo*/E,w is equal to or less than 1.0, the
facility is in compliance; if Eg'/Biu is greater
than 1.0, the facility is not in compliance for
the reporting period.
Ill-Appendix A-107
-------
Method 20—Determination of Nitrogen
Oxides, Sulfur Dioxide, and Oxygen
Emissions from Stationary Gas Turbines
1. Applicability and Principle
1.1 Applicability. This method is
applicable for the determination of nitrogen
oxides (NO,), sulfur dioxide (SOj), and
oxygen (Oa) emissions from stationary gas
turbines. For the NO, and Oa determinations.
this method includes: (1) measurement
system design criteria, (2) analyzer
performance specifications and performance
test procedures; and (3) procedures for
emission testing.
1.2 Principle. A gas sample is
continuously extracted from the exhaust
stream of a stationary gas turbine; a portion
of the sample stream is conveyed to
instrumental analyzers for determination of
NO, end O, content. During each NO, and
OOj determination, a separate measurement
of SOi emissions is made,- using Method 6, or
it equivalent. The O» determination is used to
adjust the NO, and SO> concentrations to a
reference condition.
2. Definitions
2.1 Measurement System. The total
equipment required for the determination of a
gas concentration or a gas emission rate. The
system consists of the following major
subsystems:
2.1.1 Sample Interface. That portion of a
system that is used for one or more of the
following: sample acquisition, sample
transportation, sample conditioning, or
protection of the analyzers from the effects of
the stack effluent.
2.1.2 NO, Analyzer. That portion of the
system that senses NO, and generates an
output proportional to the gas concentration.
2.1.3 O» Analyzer. That portion of the
system that senses O» and generates an
output proportional to the gas concentration.
2.2 Span Value. The upper limit of a gas
concentration measurement range that is
specified for affected source categories in the
applicable part of the regulations.
23 Calibration Gas. A known
concentration of a gas in an appropriate
diluent gas.
2/4 Calibration Error. The difference
between the gas concentration indicated by
the measurement system and the known
concentration of the calibration gas.
2.5 Zero Drift The difference in the
measurement system output readings before
and after a stated period of operation during
which no unscheduled maintenance, repair.
or adjustment took place and the input
concentration at the time of the
measurements was zero.
2.8 Calibration Drift. The difference in the
measurement system output readings before
and after a stated period of operation during
which no unscheduled maintenance, repair,
or adjustment took place and the input at the
time of the measurements was a high-level
value.
2.7 Residence Time. The elapsed time
from the moment the gas sample enters the
probe tip to the moment the same gas sample
reaches the analyzer inlet.
2.8 Response Time. The amount of time
required for the continuous monitoring
system to display on the data output 95
percent of a step change in pollutant
concentration.
2.9 Interference Response. The output
response of the measurement system to a
component in the sample gas, other than the
gas component being measured.
3. Measurement System Performance
Specifications
3.1 NO, to NO Converter. Greater than 90
percent conversion efficiency of NO* to NO.
. 3.2 Interference Response. Less than ± 2
percent of the span value.
3.3 Residence Time. No greater than 30
seconds.
3.4 Response Time. No greater than 3
minutes.
3.5 Zero Drift. Less than ± 2 percent of
the span value.
3.6 Calibration Drift. Less than ± 2
percent of the span value.
4. Apparatus and Reagents
4.1 Measurement System. Use any
measurement system for NO. and O» that is
expected to meet the specifications in this
method. A schematic of an acceptable
measurement system is shown in Figure 20-1.
The essential components of the
measurement system are described below:
Figure 20 1. Measurement system design for stationary gas turbines.
EXCESS
SAMPLE TO VENT
4.1.1 Sample Probe. Heated stainless
steel, or equivalent, open-ended, straight tube
of strfficient length to traverse the sample
points.
4.1.2 Sample Line. Heated (> 95°C)
stainless steel or Teflon*.bing to transport
the sample gas to the sample conditioners
and analyzers.
4.1.3 Calibration Valve Assembly. A
three-way valve assembly to direct the zero
and calibration gases to the sample
conditioners and to the analyzers. The
calibration valve assembly shall be capable
of blocking the sample gas flow and of
introducing calibration gases to the
measurement system when in the calibration
mode.
4.1.4 NOa to NO Converter. That portion
of the system that converts the nitrogen
dioxide (NOa) in the sample gas to nitrogen
oxide (NO). Some analyzers are designed to
measure NO, as NO> on a wet basis and can
be used without an NO, to NO converter or a
moisture removal trap provided the sample
line to the analyzer is heated (>95°C) to the
inlet of the analyzer. In addition, an NO, to
NO converter is not necessary if the NO,
portion of the exhaust gas is less than 5
percent of the total NO, concentration. As *
guideline, an NOa to NO converter is not
necessary if the gas turbine is operated at 90
percent or more of peak load capacity. A
converter is necessary under lower load
conditions.
4.1.5 Moisture Removal Trap. A
refrigerator-type condenser designed to
continuously remove condensate from the
sample gas. The moisture removal trap is not
necessary for analyzers that can measure
NO, concentrations on a wet basis: for these
analyzers, (a) heat the sample line up to the
inlet of the analyzers, (b) determine the
moisture content using methods subject to thi
approval of the Administrator, and (c) correc
the NO, and Oi concentrations to a dry basis
4.1.6 Particulate Filter. An in-stack or an
out-of-stack glass fiber filter, of the type
specified in EPA Reference Method 5:
however, an out-of-stack filter is
recommended when the stack gas
temperature exceeds 250 to 300°C.
4.1.7 Sample Pump. A nonreactive leak-
free sample pump to pull the sample gas
through the system at a flow rate sufficient it
minimize transport delay. The pump shall be
made from stainless steel or coated with
Teflon or equivalent.
4.1.8 Sample Gas Manifold. A sample gas
manifold to divert portions of the sample gas
stream to the analyzers. The manifold may be
constructed of glass, Teflon, type 316
stainless steel, or equivalent.
4.1.9 Oxygen and Analyzer. An analyzer
to determine the percent Oi concentration of
the sample gas stream.
4.1.10 Nitrogen Oxides Analyzer. An
analyzer to determine the ppm NO,
concentration in the sample gas stream.
4.1.11 Data Output. A strip-chart recorder..
analog computer, or digital recorder for
recording measurement data.
4.2 Sulfur Dioxide Analysis. EPA
Reference Method 8 apparatus and reagents.
4.3 NO, Caliberation Gases. The
calibration gases for the NO, analyzer may
be NO in N,. NO, in air or N,, or NO and NO,
Ill-Appendix A-108
-------
ill NI. For NO, measurement analyzers that
require oxidation of NO to NO* the
calibration gases must be in (he form of NO
in NI. Use four calibration gas mixtures as
specified below:
4.3.1 High-level Gas. A gas concentration
that is equivalent to 60 to 90 percent of the
spun value.
4.3.2 Mid-level Gas. A gas concentration
that is equivalent to 45 to 55 percent of the
spun value.
4.3.3 Low-level Gas. A gas concentration
that is equivalent to 20 to 30 percent of the
span value.
4.3.4 Zero Gas. A gas concentration of
less than 0.25 percent of the span value.
Ambient air may be used for the NO, zero
pas.
4.4 Ot Calibration Gases. Use ambient air
•il 20.9 percent as the high-level O, gas. Use a
gas concentration that is equivalent to 71-14
percent O» for the mid-level gas. Use purified
nitrogen for the zero gas.
4.5 NO,/NO Gas Mixture. For
determining the conversion efficiency of the
NO, to NO converter, use a calibration gas
mixture of NO, and NO in N,. The mixture
will be known concentrations of 40 to 60 ppm
NO, and 90 to 110 ppm NO and certified by
the gas manufacturer. This certification of gas
concentration must include a brief
description of the procedure followed in
determining the concentrations.
5. Measurement System Performance Test
Procedures
Perform the following procedures prior lu
measurement of emissions (Section 6) and
only once for each test program, i.e.,-the
scries of all test runs for a given gas turbine
engine.
5.1 Calibration Gas Checks. There are
two alternatives for checking the
concentrations of the calibration gases, (a)
The first is to use calibration gases that arg
documented traceable to National Bureau of
Standards Reference Materials. Use
Traceability Protocol for Establishing True
Concentrations of Gases Used for
Calibrations and Audits of Continuous
Source Emission Monitors (Protocol Number
1) that is available from the Environmental
Monitoring and Support Laboratory. Quality
Assurance Branch, Mail Drop 77,
Environmental Protection Agency, Research
Triangle Park. North Carolina 27711. Obtain a
certification from the gas manufacturer that
the protocol was followed. These calibration
gases are not to be analyzed with the .
Reference Methods, (b) The second
alternative is to use calibration gases not
prepared according to the protocol. If this
alternative is chosen, within 1 month prior to
the emission test, analyze each of the
calibration gas mixtures in triplicate using
Reference Method 7 or the procedure outlined
in Citation 8.1 for NO, and use Reference
Method 3 for O». Record the results on a data
sheet (example is shown in Figure 20-2). For
the low-level, mid-level, or high-level gas
mixtures, each of the individual NO,
analytical results must be within 10 percent
(or 10 ppm, whichever is greater) of the
triplicate set average (Ot test results must be
within 0.5 percent O,); otherwise, discard the
entire set and repeat the triplicate analyses.
If the average of the triplicate reference
method test results is within 5 percent for
NO. gas or 0.5 percent O, for the Ot gas of
the calibration gas manufacturer's tag value.
use the tag value; otherwise, conduct at least
three additional reference method test
analyses until the results of six individual
NO, runs (the three original plus three
additional) agree within 10 percent (or 10
ppm. whichever is greater) of the average (O,
test results must be within 0.5 percent O2).
Then use this average for the cylinder value.
5.2 Measurement System Preparation.
Prior to the emission test, assemble the
measurement system following the
manufacturer's written instructions in
preparing and operating the NO, to NO
converter, the NO, analyzer, the Ot analyzer,
and other components.
Date.
.(Must bt within 1 month prior to the test period)
Reference method used.
Sample run
1
2
3
Average
Maximum % deviation*'
Gas concentration, ppm
Low level8
Mid leveJb
High level0
8 Average must ba.20 to 30% of span value.
b Average must be 45 to 55% of span value.
c Average must be 80 to 90% of span value.
° Must be £ ± 10% of applicable average or 10 ppm.
whichever is greater,
Figure 20-2. Analysis of calibration gases.
Ill-Appendix A-109
-------
calibration valve until all readings are stable:
then, switch to monitor the stack effluent
until a stable reading can be obtained.
Record the upscale response time. Next.
introduce high-level calibration gas into the
system. Once the system has stabilized at the
high-level concentration, switch to monitor
the stack effluent and wait until a stable
value is reached. Record the downscale
response time. Repeat the procedure three
times: A stable value is equivalent to a
change of less than 1 percent of span value
for 30 seconds or less than 5 percent of the
measured average concentration for 2
minutes. Record the response time data on a
form similar to Figure 20-5. the readings of
the upscale or downscale reponse time, and
report the greater time as the "response time"
for the analyzer. Conduct a response time
test prior to the initial field use of the
measurement system, and repeat if changes
are made in the measurement system.
Date of test.
Analyzer type.
Span gas concentration.
Analyzer span setting
Upscale
1.
2.
3.
. S/N.
.ppm
ppm
.seconds
.seconds
.seconds
Average upscale response.
1
Downscale 2
3
.seconds
. seconds
.seconds
. seconds
Average downscale response.
.seconds
System response time = slower average time =.
.seconds.
Figure 20-5. Response time
5.6 NO. NO Conversion Efficiency.
Introduce to the system, at the calibration
valve assembly, the NOi/NQ gas mixture
(Section 4.5). Record the response of the NO,
analyzer. If the instrument response indicates
less than 90 percent NOi to NO conversion.
make corrections to the measurement system
and repeat the check. Alternatively, the NO»
to NO converter check described in Title 40
Part 86: Certification and Test Procedures for
Heavy-Duty Engines for 1979 and Later
Model Years may be used. Other alternate
procedures may be used with approval of the
Administrator.
6'. Emission Measurement Test Procedure
6.1 Preliminaries.
6.1.1 Selection of a Sampling Site. Select a
sampling site as close as practical to the
exhaust of the turbine. Turbine geometry',
stack configuration, internal baffling, and
point of introduction of dilution air will vary
for different turbine designs. Thus, each of
these factors must be given special
consideration in order to obtain a
representative sample. Whenever possible,
the sampling site shall be located upstream of
the point of introduction of dilution air into
the duct. Sample ports may be located before
or after the upturn elbow, in order to
accommodate the configuration of the turning
vanes and baffles and to permit a complete.
unobstructed traverse of the stack. The
sample ports shall not be located within 5
feet or 2 diameters (whichever is less) of the
gas discharge to atmosphere. For
supplementary-fired, combined-cycle plants.
the sampling site shall be located between
the gas turbine and the boiler. The diameter
of the sample ports shall be sufficient to
allow entry of the sample probe.
6.1.2 A preliminary Oi traverse is made
for the purpose of selecting low O, values.
Conduct this test at the turbine condition that
is the lowest percentage of peak load
operation included in the program. Follow the
procedure below or alternative procedures
subject to the approval of the Administrator
may be used:
6.1.2.1 Minimum Number of Points. Select
a minimum number of points as follows: (1)
eight, for stacks having cross-sectional areas
less than 1.5 m* (16.1 ft1); (2) one sample point
for each 0.2 m* (2.2 ft* of areas, for stacks of
1.5 m2 to 10.0 m1 (16.1-107.6 ft3) in cross-
sectional area: and (3) one sample point for
each 0.4 m-(4.4 ft1) of area, for stacks greater
than 10.0 m : (107.6 ft *) in cross-sectional
area. Note that for circular ducts, the number
of sample points must be a multiple of 4. and
for rectangular ducts, the number of points
must be one of those listed in Table 20-2:
therefore, round off the number of points
(upward), when appropriate.
6.1.2.2 Cross-sectional Layout and
Location of Traverse Points. After the number
of traverse points for the preliminary O-
sampling has been determined, use Method 1
to located the traverse points.
6.1.2.3 Preliminary O! Measurement.
While the gas turbine is operating at the
lowest percent of peak load, conduct a
preliminary O2 measurement as follows:
Position the probe at the first traverse point
and begin sampling. The minimum sampling
time at each point shall be 1 minute plus the
average system response time. Determine the
average steady-state concentration of Ozat
each point and record the data on Figure 20-
6.
6.1.2.4 Selection of Emission Test
Sampling Points. Select the eight sampling
points at which the lowest Oa concentration
were obtained. Use these same points for all
the test runs at the different turbine load
conditions. More than eight points may be
used, if desired.
Table 20-2.—Cross-sectional Layout for
Rectangular Stacks
No of traverse ponls;
12.
18
20
25
30
36
42
49
Matrix
layout
3x3
4x3
4x4
5x4
5x5
6x5
6x6
7x6
7x7
Ill-Appendix A-110
-------
5.3 Calibration Check. Conduct the
calibration checks for both the NO, and the
O, analyzers as follows:
54.1 After the measurement system has
been prepared for use (Section 5.2), introduce
zero gases and the mid-level calibration
gases; set the analyzer output responses to
the appropriate levels. Then introduce each
of the remainder of the calibration gases
described in Sections 4.3 or 4.4, one at a time.
to the measurement system. Record the
responses on a form similar to Figure 20-3.
5.3.2 If the linear curve determined from
the zero and mid-level calibration gas
responses does not predict the actual
response of the low-level (not applicable for
the Ot analyzer) and high-level gases within
±2 percent of the span value, the calibration
shall be considered invalid. Take corrective
measures on the measurement system before
proceeding with the test
5.4 Interference Response. Introduce the
gaseous components listed in Table 20-1 into
the measurement system separately, or as gas
mixtures. Determine the total interference
output response of the system to these
components in concentration units; record the
values on a form similar to Figure 20-4. If the
sum of the interference responses of the test
gases for either the NO, or O, analyzers is
greater than 2 percent of the applicable span
value, take corrective measure on the
measurement system.
Tatri* 20-1.—Interference Test Gas Concentration
500±50ppm.
200±20ppm.
10±1 percent
- a>.8±i
percent
CO..
SO.....
CO.
O.
T««i 9* Analy/m nuiin
type CuHccnirtlMin. ppn» ntpomu > .it man
Anatyie, output f
bnlrumcnt .pan
Fipjr* 304. Iflbtttrvnce
Turbine type:,
Date:
Identification number.
Test number
Analyzer type:,
Identification number.
Cylinder Initial analyzer Final analyzer Difference:
value, response, responses, . initial-final.
ppm or % ppm or % ppm or % ppm or %
Zero gas
Low • level gas
Mid - level gas
High - level gas
Percent drift:
Absolute difference
X100.
Span value
Figure 20-3. Zero and calibration data.
Conduct an interference response test of
each analyzer prior to its initial use in the
field. Thereafter, recheck the measurement
system if changes are made in the
instrumentation that could alter the
interference response, e.g., changes in the
type of gas detector.
In lieu of conducting the interference
response test, instrument vendor data, which
demonstrate that for the test gases of Table
20-1 the interference performance
specification is not exceeded, are acceptable.
5.5 Residence and Response Time.
5.5.1 Calculate the residence time of the
sample interface portion of the measurement
system using volume and pump flow rate
information. Alternatively, if the response
time determined as defined in Section 5.5.2 is
less than 30 seconds, the calculations are not
necessary.
5.5.2 To determine response time, first
introduce zero gas into the system at the
Ill-Appendix A-lll
-------
Location:
Plant,
Date.
City. State.
Turbine identification:
Manufacturer __
Model, serial number.
Sample point
Oxygen concentration, ppm
Figure 20-6. Preliminary oxygen traverse.
6.2 NO, and O, Measurement. This test is
to be conducted at each of the specified load
conditions. Three test runs at each load
condition constitute a complete test.
6.2.1 At the beginning of each NO, test
run and, as applicable, during the run, record
turbine data as indicated in Figure 20-7. Also.
record the location and number of the
traverse points on a diagram.
0.2.2 Position the probe at the first point
determined in the preceding section and
begin sampling. The minimum sampling time
at each point shall be at least 1 minute plus
the average system response time. Determine
the average steady-state concentration of O>
and NO, at each point and record the data on
Figure 2O-8.
Ill-Appendix A-112
-------
TURBINE OPERATION RECORD
Test operator Date
Turbine identification:
Type
Serial No
Location:
Plant
City
Ultimate fuel
Analysis C
H
N
Ambient temperature.
Ambient humidity
Test time start
Ash
H20
Trace Metals
Na
Test time finish.
Fuel flow ratea_
Va
etcc
Water or steam
Flow rate3
Ambient Pressure.
Operating load.
aDescribe measurement method, i.e., continuous flow meter,
start finish volumes, etc.
bi.e., additional elements added for smoke suppression.
Figure 20-7. Stationary gas turbine data.
Turbine identification:
Manufacturer
Test operator name.
O2 instrument type.
Serial No
MnHel, serial Nn , ... .. M~»^ instrument tv/ne
Serial N
Location:
Sample
Pl.nt P°int
rity State
Amhipnt temperature .
Amhipnt pressure
Rate
Test time - start
Time,
min.
oS.
%
NOX,
ppm
Test time - finish.
aAverage steady-state value from recorder or
instrument readout.
Figure 20-8. Stationary gas turbine sample point record.
Ill-Appendix A-113
-------
6.2.3 After sampling the last point,
conclude the test run by recording the final
turbine operating parameters and by
determining the zero and calibration drift, as
follows:
Immediately following the test run at each
load condition, or if adjustments are
necessary for the measurement system during
the tests, reintroduce the zero and mid-level
calibration gases as described in Sections 4.3,
and 4.4, one at a time, to the measurement
system at the calibration valve assembly.
(Make no adjustments to the measurement
system until after the drift checks are made).
Record the analyzers' responses on a form
similar to Figure 20-3. if the drift values
exceed the specified limits, the test run
preceding the check is considered invalid and
will be repeated following corrections to the
measurement system. Alternatively, the test
results may be accepted provided the
measurement system is recalibrated and the
calibration data that result in the highest
corrected emission rate are used.
6.3 SOi Measurement. This test is
conducted only at the 100 percent peak load
condition. Determine SO, using Method 6, or
equivalent, during the test. Select a minimum
of six total points from those required for the
NO, measurements; use two points for each
•ample run. The sample time at each point
shall be at least 10 minutes. Average the Oi
readings taken during the NO, test runs at
sample points corresponding to the SO,
traverse points (see Section 6.2.2) and use
this average Ot concentration to correct the
integrated SO, concentration obtained by
Method 6 to 15 percent O, (see Equation 20-
1).
If the applicable regulation allows fuel
sampling and analysis for fuel sulfur content
to demonstrate compliance with sulfur
emission unit, emission sampling with
Reference Method 6 is not required, provided
the fuel sulfur content meets the limits of the
regulation.
7. Emission Calculations
7.1 Correction to 15 Percent Oxygen.
Using Equation 20-1, calculate the NO, and
SOi concentrations (adjusted to 15 percent
Ot). The correction to 15 percent O, is
sensitive to the accuracy of the O,
measurement. At the level of analyzer drift
specified in the method (±2 percent of full
scale), the change in the Oi concentration
correction can exceed 10 percent when the O,
content of the exhaust is above 16 percent O,.
Therefore Oi analyzer stability and careful
calibration are necessary.
'•adj
5.!.
~-
(Equation 20-1)
Where:
CMJ=Pollutant concentration adjusted to
15 percent O, (ppm)
Cmeu = Pollutant concentration measured,
dry basis (ppm)
5.9=20.9 percent O.-15 percent Otl the
defined O> correction basis
Percent O>=Percent O, measured, dry
basis (%)
7.2 Calculate the average adjusted NO,
concentration by summing the point values
and dividing by the number of sample points.
8. Citations
8.1 Curtis, F. A Method for Analyzing NO,
Cylinder Gases-Specific Ion Electrode
Procedure, Monograph available from
Emission Measurement Laboratory, ESED,
Research Triangle Park, N.C 27711, October
1978.
Ill-Appendix A-114
-------
Method 24—Determination of Volatile Matter
Content, Water Content Density, Volume n?
Solids, and Weight Solids of Surface Coating*
1. Applicability and Principle
1.1 Applicability. This method applies to
the determination of volatile matter content,
water content density, volume solids, and
weight solids of paint, varnish, lacquer, or
related surface coatings.
1.2 Principle. Standard methods are used
to determine the volatile matter content,
water content density, volume solids, and
weight solids of the paint varnish, lacquer, or
related surface coatings.
2. Applicable Standard Methods
Use the apparatus, reagents, and
procedures specified in the standard methods
below:
2.1 ASTM D1475-60. Standard Method of
Test for Density of Paint, Lacquer, and
Related Products.
2.2 ASTM D 2369-61. Provisional Method
of Test for Volatile Content of Paints.
2.3 ASTM D 3792-79. Standard Method of
Test for Water in Water Reducible Paint by
Direct Injection into a Gas Chromatograph.
2.4 ASTM Provisional Method of Test for
Water in Paint or Related Coatings by the
Karl Fischer Titration Method.
3. Procedure
3.1 Volatile Matter Content. Use the
procedure in ASTM D 2369-81 to determine
the volatile matter content (may include
water) of the coating. Record the following
information:
W(=Weight of dish and sample before
heating, g.
W»=Weight of dish and sample after heating,
g.
W3=Sample weight g.
Run analyses in pairs (duplicate sets) for
each coating until the criterion in section 4.3
is met. Calculate the weight fraction of the
volatile matter (W,) for each analysis as
follows:
Eq. 24-1
Record the arithmetic average (W.).
3.2 Water Content For waterborne (water
reducible) coatings only, determine the
weight fraction of water (W.) using either
"Standard Method of Test for Water in Water
Reducible Paint by Direct Infection into a Gas
Chromatograph" or "Provisional Method of
Test for Water in Paint or Related Costings
by the Karl Fischer Titration Method" A
waterbome coating is any coating which
contains more than 5 percent water by weight
in its volatile fraction. Run duplicate sets of
delerminations-until the criterion in. section
4.3 is met. Record the arithmetic average
(W.).
3.3 Coating Density. Determine the
density (D^, kg/liter) of the surface coating
using the procedure in ASTM D1475-60.
Run duplicate sets of determinations for
each coaling until the criterion in section 4.3
is met. Record the arithmetic average (Dc).
3.4 Solids Content. Determine the volume
fraction (V.) solids of the coating by
calculation using the manufacturer's
formulation.
4. Data Validation Procedure
4.1 Summary. The variety of coatings that
may be subject to analysis makes it
necessary to verify the ability of the analyst
and the analytical procedures to obtain
reproducible results for the coatings tested.
This is done by running duplicate analyses on
each sample tested and comparing results
with the within-laboratory precision
statements for each parameter. Because of
the inherent increased imprecision in the
determination of the VOC content of
waterbome coatings as the weight percent
water increases, measured parameters for
waterborne coatings are modified by the
appropriate confidence limits based on
between-laboratory precision statements.
4.2 Anelytioal Precision Statements. The
wtthiB-taboretory and between-laboratory
precision statements are given below:
Within.
laboratory
Between-
laboratory
Volatile matter content, w.. 1.S pet W 4.7 pel W,
Water content, w. 2* pet W. 7.5 pet W..
Density. D, 0.001 kg/liter... 0.002 kg/liter.
4.3 Sample Analysis Criteria. For W, and
W., run duplicate analyses until the
difference between the two values in a set is
less than or equal to the within-laboratory
precision statement for that parameter. For D,
run duplicate analyses until each value in a
set deviates from the mean of the set by no
more than the within-laboratory precision
statement. If after several attempts it is
concluded that the ASTM procedures cannot
be used for the specific coating with the
established within-laboratory precision, the
Administrator will assume responsibility for
providing the necessary procedures for
revising the method or precision statements
upon written request to: Director, Emission
Standards and Engineering Division. (MD-13)
Office of Air Quality Planning and Standards,
U.S. Environmental Protection Agency.
Research Triangle Park. Nortti Carolina
27711.
4.4 Confidence Limit Calculations for
Waterbome Coatings. Based on'the between-
laboratory precision statement*, calculate the
confidence limits for waterborne coatings as
follows:
To calculate the lower confidence limit
subtract the appropriate between-laboratory
precision value from the measured mean
value for that parameter. To calculate the
upper confidence limit add the appropirate
between-laboratory precision value to the
measured mean value for that parameter. For
W, and DC, use the lower confidence limits,
and for W,, use the upper confidence limit.
Because V. is calculated, there is no
adjustment for the parameter.
5. Calculations
S.1 Nonaqueous Volatile Matter.
5.1.1 Solvent-borne Coatings.
W.=W, Eq. 24-3
Where:
W0=Weight fraction nonaqueous volatile
matter, g/g.
5.1.2 Waterborne Coatings.
W0=W.-W, Eq. 24-3
5.2 Weight fraction solids.
W.=1-W, Eq. 24-4
Where: W.=Weight solids, g/g.
ft Bibliography
6.1 Provisional Method Test for Volatile
Content of Paints. Available from: Chairman,
Committee D-l on Paint and Related
Coatings and Materials, American Society for
Testing and Materials, 1916 Race Street
Philadelphia, Pennsylvania 19103. ASTM
Designation D 2369-81,
6.2 Standard Method of Test for Density
of Paint Varnish, Laaqoer. and Related
Products, fa: 1880 Book of ASTM Standards,
Part 27. Philadelphia. Pennsylvania. ASTM
Designation D1475-60.1960.
6.3 Standard Method of Test for Water in
Water Reducible Paint by Direct Injection
into a Gas Chromatograph. Available from:
Chairman, Committee D-l on Paint and
Related Coatings and Materials, American
Society for Testing and Materials, 1916 Race
Street Philadelphia, Pennsylvania 19103.
ASTM Designation D 3792-79.
6.4 Provisional Method of Teat Water in
Paint or Related Coatings by the Karl Fischer
Titration Method. Available from: Chairman,
Committee D-l on Paint and Related
Coatings and Materials, American Society for
Testing and Materials, 1916 Race Street
Philadelphia. Pennsylvania 19103.
Ill-Appendix A-115
-------
Method 25—Determination of Total Gaseous
Nonmethane Organic Emission* as Carbon'I7
1. Applicability and Principle
1.1 Applicability. This method applies to
the measurement of volatile organic
compounds (VOC] as total gaseous
nonmethane organics (TGNMO) as carbon in
source emissions. Organic paniculate matter
will interfere with the analysis and therefore,
in some cases, an in-stack particulate filter U
required. This method is not the only method
that applies to the measurement of TGNMO.
Costs, logistics, and other practicalities of
sowce testing may make other test methods
more desirable for measuring VOC of certain
effluent streams. Proper Judgment is required
in determining the most applicable VOC test
method. For example, depending upon the
molecular weight of the organics in the
effluent stream, a totally automated semi-
continuous nonmethane organic (NMO)
analyzer interfaced directly to the source
may yield accurate results. This approach has
the advantage of providing emission data
•emi-continuously over an extended time
period.
Direct measurement of an effluent with a
flame ionization detector (FID) analyzer may
be appropriate with prior characterization of
the gas stream and knowledge that the
detector responds predictably to the organic
compounds in the stream. If present, methane
will, of course, also be measured. In practice.
the FID can be applied to the determination
of the mass concentration of the total
molecular structure of the organic emissions
under the following limited conditions: (1)
Where only one compound is known to exist;
(2) when the organic compounds consist of
only hydrogen and carbon; (3) where the
relative percentage of the compounds is
known or can be determined, and the FID
response to the compounds is known; (4)
where a consistent mixture of compounds
exists before and after emission control and
only the relative concentrations are to be
assessed; or (5) where the FID can be
calibrated against mass standards of the
compounds emitted (solvent emissions, for
example).
Another example of the use of a direct FID
is as a screening method. If there is enough
information available to provide a rough
estimate of the analyzer accuracy, the FID
analyzer can be used to determine the VOC
content of an uncharacterized gas stream.
With a sufficient buffer to account for
possible inaccuracies, the direct FID can be a
useful tool to obtain the desired results
without costly exact determination.
k> situations where a qualitative/
quantitative analysis of an effluent stream is
desired or required, a gas chromatographic
FID system may apply. However, for sources
emitting numerous organics, the time and
expense of this approach will be formidable.
\2 Principle. An emission sample is
withdrawn from the stack at a constant rate
through a chilled condensate trap by means
of an evacuated sample tank. TGNMO are
determined by combining the analytical
results obtained from independent analyses
of the condensate trap and sample tank
fractions. After sampling is completed, the
organic contents of the condensate trap are
oxidized to carbon dioxide (CO,) which is
quantitatively collected in an evacuated
vessel; then a portion of the CO, is reduced to
methane (CH,) and measured by a FID. The
organic content of the sample fraction
collected in the sampling tank is measured by
injecting a portion into a gas
chromatographic (GC) column to achieve
separation of the nonmethane organics from
carbon monoxide (CO), COa and CH.; the
nonmethane organics (NMO) are oxidized to
COi, reduced to CH,, and measured by a FID.
In this manner, the variable response of the
FID associated with different types of
organics is eliminated.
2. Apparatus
The sampling system consists of a
condensate trap, flow control system, and
sample tank (Figure 1). The analytical system
consists of two major sub-systems: an
oxidation system for the recovery and
conditioning of the condensate trap contents
and a NMO analyzer. The NMO analyzer is a
CC with backflush capability for NMO
analysis and is equipped with an oxidation
catalyst, reduction catalyst, and FID. (Figures
2 and 3 are schematics of a typical NMO
analyzer.) The system for the recovery and
conditioning of die organics captured in the
condensate trap consists of a heat source,
oxidation catalyst, nondlspersive infrared
(NDIR) analyzer and an intermediate
collection vessel (Figure 4 is a schematic of a
typical system.) TGNMO sampling equipment
can be constructed from commercially
available components and components
fabricated in a machine shop. NMO
analyzers are available commercially or can
be constructed from available components by
a qualified instrument laboratory.
2.1 Sampling. The following equipment is
required:
2.1.1 Probe. 3.2-mm OD (Vfe-in.) stainless
steel tubing.
2.1.2 Condensate Trap. Constructed of 318
stainless steel; construction details of a
suitable trap are shown in Figure S.
2.1.3 Flow Shut-off Valve. Stainless steel
control valve for starting and stopping
sample flow.
2.1.4 Flow Control System. Any system
capable of maintaining the sampling rate to
within ±10 percent of the selected flow rate
(50 to 100 cc/min range).
2.1.5 Vacuum Gauge. Gauge for
monitoring the vacuum of the sample tank
during leak checks and sampling.
2.1.6 Sample Tank. Stainless steel or
aluminum tank with a volume of 4 to 8 liters,
equipped with a stainless steel female quick
connect for assembly to the sample train and
analytical system.
2.1.7 Mercury Manometer. U-tube
mercury manometer capable of measuring
pressure to within 1 mm Hg in the 0-900 mm
range.
2.1.8 Vacuum Pump. Capable of
evacuating to an absolute pressure of 10 mm
Hg.
2.2 Analysis. The following equipment is
required:
2.2.1 Condensate Recovery and
Conditioning Apparatus. An apparatus for
recovering and catalytically oxidizing the
condensate trap contents is required. Figure 4
is a schematic of such a system. The analyst
must demonstrate prior to initial use that the
analytical system is capable of proper
oxidation and recovery, as specified in
section S.I. The condensate recovery and
conditioning apparatus consists of the
following major components.
2.2.1.1 Heat Source. A heat source
sufficient to heat the condensate trap
(including probe) to a temperature where the
trap turns a "dull red" color. A system using
both a propane torch and an electric muffle-
type furnace is recommended.
2.2.1.2 Oxidation Catalyst A catalyst
system capable of meeting the catalyst
efficiency criteria of this method (section
5.1.2). Addendum I of this method lists a
catalyst system found to be acceptable.
2.2.1.3 Water Trap. Any leak-proof
moisture trap capable of removing moisture
from the gas stream.
2.2.1.4 NDIR Detector. A detector capable
of indicating COi concentration in the zero to
1 percent range. This detector is required for
monitoring the progress of combustion of the
organic compounds from the condensate trap.
2.2.1.5 Pressure Regulator. Stainless steel
needle valve required to maintain the trap
conditioning system at a near constant
pressure.
2.2.1.6 Intermediate Collection Vessel.
Stainless steel or aluminum collection vessel
equipped with a female quick connect. Tanks
with nominal volumes in the 1 to 4 liter range
are recommended.
2.2.1.7 Mercury Manometer. U-tube
mercury manometer capable of measuring
pressure to within 1 mm Hg in the 0-900 mm
range.
2.2.1.8 Gas Purifiers. Gas purification
systems sufficient to maintain CO, and
organic impurities in the carrier gas and
auxiliary oxygen at a level of less than 10
ppm (may not be required depending on
quality of cylinder gases used).
2.2.2 NMO Analyzer. Semi-continuous
GC/FID analyzer capable of; (1) separating
CO. COi, and CH, from nonmethane organic
compounds, (2) reducing the CO, to CH, and
quantifying as CH. and (3) oxidizing the
nonmethane organic compounds to CO*
reducing the CO, to CH. and quantifying as
CH.. The analyst must demonstrate prior to
initial use that the analyzer is capable of
proper separation, oxidation, reduction, and
measurement (section 5.2). The analyzer
consists of the following major components:
2.2.2.1 Oxidation Catalyst. A catalyst
system capable of meeting the catalyst
efficiency criteria of this method (section
5.2.1). Addendum I of this method lists a
catalyst system found to be acceptable.
2.2.2.2 Reduction Catalyst. A catalyst
system capable of meeting the catalyst
efficiency criteria of this method (section
5.2.3). Addendum I of this method lists a
catalyst system found to be acceptable.
2.2.2.3 Separation Column(s). Gas
chromatographic column(s) capable of
separating CO, CO* and CH. from NMO
compounds as demonstrated according to the
procedures established in this method
(section 5.2.5). Addendum I of this method
lists a column found to be acceptable.
2.2.2.4 Sample Injection System. A GC
sample injection valve fitted with a sample
Ill-Appendix A-116
-------
loop properly sized to interface with the
NMO analyzer (1 cc loop recommended).
2.2.2.5 FID. A FID meeting the following
specifications is required.
2.2.2.S.1 Linearity. A linear response (±
5%) over the operating range as demonstrated
by the procedures established in section 5.2.2.
2.2.2.5.2 Range. Signal attenuators shall
be available to produce a minimum signal
response of 10 percent of full scale for a full
scale range of 10 to 50000 ppm CH*.
2.2.2.6 Data Recording System. Analog
strip chart recorder or digital intergratlon
system compatible with the FID for
permanently recording the analytical results.
2.2.3 Barometer. Mercury, aneroid, or
other barometer capable of measuring
atmospheric pressure to within 1 mm Hg.
2.2.4 Thermometer. Capable of measuring
the laboratory temperature within 1°C.
2.2.5 Vacuum Pump. Capable of
evacuating to an absolute pressure of 10 mm
Hg.
2.2.6 Syringe (2). 10 /il and 100 jxl liquid
injection syringes.
2.2.7 Liquid Sample Injection Unit 316 SS
U-tube fitted with a Teflon injection septum,
see Figure 6.
3. Reagents
3.1 Sampling. Crushed dry ice is required
during sampling.
3.2 Analysis.
3.2.1 NMO Analyzer. The following gases
are needed:
3.2.1.1 Carrier Gas. Zero grade gas
containing less than 1 ppm C. Addendum I of
this method lists a carrier gas found to be
acceptable.
3.2.1.2 Fuel Gas. Pure hydrogen,
containing less than 1 ppm C.
3.2.1.3 Combustion Gas. Zero grade air or
oxygen as required by the detector.
3.2.2 Condensate Recovery and
Conditioning Apparatus.
3.2.2.1 Carrier Gas. Five percent Oi in N,,
containing less than 1 ppm C.
3.2.2.2 Auxiliary Oxygen. Zero grade
oxygen containing less than 1 ppm C.
3.2.2.3 Hexane. ACS grade, for liquid
injection.
3.2.2.4 Toluene. ACS grade, for liquid
injection.
3.3 Calibration. For all calibration gases.
the manufacturer must recommend a
maximum shelf life for each cylinder (i.e., the
length of time the gas concentration is not
expected to change more than ± 5 percent
from its certified value). The date of gas
cylinder preparation, certified organic
concentration and recommended maximum
shelf life must be affixed to each cylinder
before shipment from the gas manufacturer to
the buyer. The following calibration gases are
required.
3.3.1 Oxidation Catalyst Efficiency Check
Calibration Gas. Gas mixture standard with
nominal concentration of 1 percent methane
in air.
3.3.2 Flame lonization Detector Linearity
and Nonmethane Organic Calibration Gases
(3). Gas mixture standards with nominal
propane concentrations of 20 ppm, 200 ppm,
and 3000 ppm, in air.
3.3.3 Carbon Dioxide Calibration Gases
(3). Gas mixture standards with nominal CO,
concentrations of 50 ppm, 500 ppm. and 1
percent, in air. Note: total NMO less than 1
ppm required for 1 percent mixture.
3.3.4 NMO Analyzer System Check
Calibration Gases (4).
3.3.4.1 Propane Mixture. Gas mixture
standard containing (nominal) 50 ppm CO, 50
ppm Cm, 2 percent CO,, and 20 ppm C>H«.
prepared in air.
3.3.4.2 Hexane. Gas mixture standard
containing (nominal} 50 ppm hexane in air.
3.3.4.3 Toluene. Gas mixture standard
containing (nominal) 20 ppm toluene in air.
3.3.4.4 Methanol. Gas mixture standard
containing (nominal) 100 ppm methanol m air.
4. Procedure
4.1 Sampling.
4.1.1 'Sample Tank Evacuation and Leak
Check. Either in the laboratory or in the Reid.
evacuate the sample tank to 10 mm Hg
absolute pressure or less (measured by a
mercury U-tube manometer) then leak check
the sample tank by isolating the tank from
the vacuum pomp and allowing the tank to sit
for 10 minutes. The tank is acceptable if no
change in tank vacuum is noted.
4.1.2 Sample Train Assembly, fust prior to
assembly, measure the tank vaccuum using a
mercury U-tube manometer. Record this
vaccum (PJ, the ambient temperature (Tu),
and the barometric pressure (IV) at this time.
Assuring that the flow shut-off valve is in the
closed position, assemble the sampling
system as shown in Figure 1. Immerse the
condensate trap body in dry ice to within 2.5
or 5 cm of the point where the inlet tube joins
the trap body.
4.1.3. Pretest Leak Check. A pretest leak
check is required. After the sampling train is
assembled, record the tank vacuum as
indicated by the vaccum gauge. Wait a
minimum period of 10 minutes and recheck
the indicated vacuum. If the vacuum has not
changed, the portion of the sampling train
behind the shut-off valve does not leak and is
considered acceptable. To check the front
portion of the sampling train, assure that the
probe tip is tightly plugged and then open the
sample train flow shut-off valve. Allow the
sample train to sit for a minimum period of 10
minutes. The leak check is acceptable if no
visible change in the tank vacuum gauge
occurs. Record the pretest leak rate (cm/Hg
per 10 minutes). At the completion of the leak
check period, close the sample flow shut-off
valve.
4.1.4. Sample Train Operation. Place the
probe into the stack such that the probe is
perpendicular to the direction of stack gas
flow; locate the probe tip at a single
preselected point If a probe extension which
will not be analyzed as part of the
condensate trap is being used, assure that at
least a 15 cm section of the probe which will
be analyzed with the trap is in the stack
effluent For stacks having a negative static
pressure, assure that the sample port is
sufficiently sealed to prevent air in-leakage
around the probe. Check the dry ice level and
add ice if necessary. Record the clock time
and sample tank gauge vacuum. To begin
sampling, open the flow shut-off valve and
adjust (if applicable) the control valve of the
How control system used in the sample train;
maintain a constant flow rate (±10 percent)
throughout the duration of the sampling
period. Record the gauge vacuum and
flowmeter setting (if applicable) at 5-minute
intervals. Select a total sample time greater
than or equal to the minimum sampling time
specified in the applicable subpart of the
regulation; end the sampling when this time
period is reached or when a constant flow
rate can no longer be maintained due to
reduced •ample tank vacuum. When the
sampling is completed, close the flow shut-off
verve and record the final sample time and
guagt vaeuum readings. Note: If the sampling
had to be stopped before obtaining the
minimum sampling time (specified in the
applicable subpart] because a constant flow
rate could not be maintained, proceed aa
follows: After removing the probe from the
•tack, remove the used sample tank from the
sampling train (without disconnecting other
portions of the sampling train) and connect
another sample tank to the sampling train.
Prior to attaching the new tank to the
sampling train, assure that the tank vacuum
(measured on-site by the U-tube manometer)
has been recorded on the data form and that
the tank has been leak-checked (on-site).
After the new tank is attached to the sample
train, proceed with the sampling until the
required minimum sampling time has been •
exceeded.
4.1.5 Post Test Leak Check. A leak check
is mandatory at the conclusion of each test
run. After sampling is completed, remove the
probe from the stack and plug the probe tip.
Open the sample train flow shut-off valve
and monitor the sample tank vacuum gauge
for a period of 10 minutes. The leak check is
acceptable if no visible change in the tank
vacuum gauge occurs. Record the post test
leak rate (cm Hg per 10 minutes). If the
sampling train does not pass the post leak
check, invalidate the run or use a procedure
acceptable to the Administrator to adjust the
data.
4.2 Sample Recovery. After the post test
leak check is completed, disconnect the
condensate trap at the flow metering system
and tightly seal both ends of the condensate
trap. Keep the trap packed in dry ice until the
samples are returned to the laboratory for
analysis. Remove the flow metering system
from the sample tank. Attach 'the U-tube
manometer to the tank (keep length of
connecting tine to a minimum) and record the
final tank vacuum (Pt); record the tank
temperature (Tj and barometric pressure at
this time. Disconnect the manometer from the
tank. Assure that the test run number is'
properly identified on the condensate trap
and the sample tank(s).
4.3 Condensate Recovery and
Conditioning. Prepare the condensate
recovery and conditioning apparatus by
setting the carrier gas flow rate and heating
the catalyst to its operating temperature.
Prior to initial use of the condensate recovery
and conditioning apparatus, a system
performance test must be conducted
according to the procedures established in
section 5.1 of this method. After successful
completion of the initial performance test the
system is routinely used for sample
conditioning according to the following
procedures:
4.3.1 System Blank and Catalyst
Efficiency Check. Prior to and immediately
Ill-Appendix A-117
-------
following the conditioning of each set of
•ample traps, or on a daily basia (whichever
occurs first) conduct the carrier gas blank test
end catalyst efficiency test as specified in
sections 5.1.1 and 6.1.2 of this method. Record
the carrier gas initial and final blank values,
BU and OK, respectively. If the criteria of the
tests cannot be met, make the necessary
repairs to the system before proceeding.
4.3.2 Condensate Trap Carbon Dioxide
Purge and Sample Tank Pressurization. The
first step to analysis is to purge the
aondwiMte trap of any COi which H may
contain and to simultaneously pressurize the
•ample tank. This is accomplished as follows:
Obtain both the sample tank and condensate
trap from the teat run to be analyzed. Set up
the condensate recovery and conditioning
apparatus so that the carrier flow bypasses
the condensate trap hook-up terminals,
bypasses the oxidation catalyst, and is
vented to the atmosphere. Next attach the
condensate trap to the apparatus and pack
the trap in dry ice. Assure that the valves
isolating the collection vessel connection
from the atmospheric vent and the vacuum
pump are closed and then attach the sample
tank to the system as if it were the
intermediate collection vessel. Record the
tank vacuum on the laboratory data form.
Assure that the NDIR analyzer indicates a
zero output level and then switch the carrier
flow through the condensate trap;
immediately switch the carrier flow from vent
to collect The condensate trap recovery and
conditioning apparatus should now be set up
as indicated in Figure 8. Monitor the NDIR;
.when COi is no longer being passed through
the system, switch die carrier flow so thai it
once again bypasses the condensate trap.
Continue in this manner until the gas sample
tank is pressurized to a nominal gauge
pressure of 800 mm Hg. At this time, isolate
the tank, vent the carrier flow, and record the
•ample tank pressure (Ptt), barometric
pressure (IV), and ambient temperature (Tu).
Remove the sample tank from the system.
4.3.3 Recovery of Condensate Trap
Sample. Oxidation and collection of the
sample in the condensate trap is now ready
to begin. From the step just completed in
section 4.3.1.2 above, the system should be
set up so that the carrier flow bypasses the
condensate trap, bypasses the oxidation
catalyst and is vented to the atmosphere.
Attach an evacuated intermediate collection
vessel to the system and then switch the
carrier so that it flows through the oxidation
catalyst Switch the carrier from vent to
collect and open the valve to the collection.
vessel; remove the dry ice from the trap and
then switch the carrier flow through the trap.
The system should now be set up to operate
as indicated in Figure 9. During oxidation of
the condensate trap sample, monitor the
NDIR to determine when all the sample has
been removed and oxidized (indicated by
return to baseline of NDIR analyzer output).
Begin heating the condensate trap and probe
with a propane torch. The trap should be
heated to a temperature at which the trap
glows a "dull red" (approximately SOO'C).
During the early part of the trap "burn out,"
adjust the carrier and auxiliary oxygen flow
rates so that an excess of oxygen is being fed
to the catalyst system. Gradually increase the
flow of carrier gas through the trap. After the
NDIR indicates that most of the organic
matter has been purged, place the trap in a
muffle furnance (SOO'C). Continue to heat the
probe with a torch or some other procedure
(e.g., electrical resistance heater). Continue
this procedure for at least 5 minutes after the
NDIR has returned to baseline. Remove the
heat from the trap but continue the carrier
flow until the intermediate collection vessel
is pressurized to a gauge pressure of 800 mm
Hg (nominal). When the vessel is pressurized.
vent the carrier measure and record the final
intermediate collection vessel pressure (PJ as
well as the barometric pressure (PbJ, ambient
temperature (T,), and collection vesael
volume (V,).
4.4 Analysis. Prior to putting the NMO
analyzer into routine operation, an initial
performance test must be conducted. Start
the analyzer and perform all the necessary
functions in order to put the analyzer in
proper working order, then conduct the
performance test according to the procedures
established in section 52. Once the
performance test has been successfully
completed and the CO* and NMO calibration
response factors determined, proceed with
sample analysis as follows:
4.4.1 Daily operations and calibration
checks. Prior to and immediately following
the analysis of each set of samples or on a
daily basis (whichever occurs first) conduct a
calibration test according to the procedures
established in section 5.3. If the criteria of the
daily calibration test cannot be met repeat
tile NMO analyzer performance test (section
5.2) before proceeding.
4.4.2 Analysis of Recovered Condensate
Sample. Purge the sample loop with sample
and then inject a preliminary sample in order
to determine the appropriate FID attenuation.
Inject triplicate samples from the
intermediate collection vessel and record the
values obtained for the condensible ocganics
as CO, (C«J.
4.4.3 Analysis of Sample Tank. Purge the
sample loop with sample and inject a
preliminary sample in order to determine the
appropriate FID attenuation for monitoring
the backflushed non-methane organic*. Inject
triplicate samples from the sample tank and
record the values obtained for the
nonmethane organics (
B. Calibration and Operational Checks
Maintain a record of performance of each
item.
5.1 Initial Performance Check of
Condensate Recovery and Conditioning
Apparatus.
5.1.1 Carrier Gas and Auxiliary Oxygen
Blank. Set equal flow rates for both the
carrier gas and auxiliary oxygen. With the
trap switching valves in the bypass position
and the catalyst in-line, fill an evacuated
intermediate collection vessel with carrier
gas. Analyze the collection vessel for CO*
the carrier blank is acceptable if the CO,
concentration is less than 10 ppm.
5.1.2 Catalyst Efficiency Check. Set up the
condensate trap recovery system so that the
carrier flow bypasses the trap inlet and is
vented to the atmosphere at the system
outlet Assure that the valves isolating the
collection system from the atmospheric vent
and vacuum pump
an evacuated intermediate collection vessel
to the system. Connect the methane standard
gas cyclinder (section 3.3.1) to the system's
condensate trap connector (probe end. Figure
4). Adjust the system valving so that the
standard gas cylinder acts as the carrier gas
and adjust the flow rate to the rate normally
used during trap sample recovery. Switch off
the auxiliary oxygen flow and then switch
from vent to collect in order to begin
collecting a sample. Continue collecting a
sample in a normal manner until the
Intermediate vessel is filled to a nominal
gauge pressure of 300 mm Hg. Remove tha.
Intermediate vessel from the system and vent
the carrier flow to the atmosphere. Switch the
valving to return the system to its normal
carrier gas and normal operating conditions.
Analyse the collection vessel for CO>; the
catalyst efficiency is acceptable if the CO,
concentration is within ±5 percent of the
expected value.
5.1.3 System Performance Check.
Construct a liquid sample injection unit
similar in design to the unit shown in Figure
6. Insert this unit into the condensate
recovery and conditioning system in place of
a condensate trap and set the carrier gas and
auxiliary oxygen flow rates to normal
operating levels. Attach an evacuated
intermediate collection vessel to the system
and switch from system vent to collect With
the carrier gas routed through the injection
unit, and the oxidation catalyst inject a liquid
sample (see. 5.L3.1 to 5,1.3.4) via the injection
septum. Heat the injection unit with a torch
while monitoring the oxidation reaction on
the NDIR. Continue the purge until the
reaction is complete. Measure the final
collection vessel pressure and then analyze
the Vessel to determine the CO,
concentration. For each injection, calculate
the percent recovery using the equation in
section 6.6.
The performance test is acceptable if the
average percent recovery is 100 ± 10 percent
with a relative standard deviation (section
6.7) of less than 5 percent for each set of
triplicate Injections as follows:
5.1.3.1 100 ;il hexane.
S.I.3.2 10 fil hexane.
5.1.3.3 100 fil toluene.
5.1.3.4 10 fil toluene.
5.2 Initial NMO Analyzer Performance
Test
5.2.1 Oxidation Catalyst Efficiency Check.
Turn off or bypass the NMO analyzer
reduction catalyst Make triplicate injections
of the high level methane standard (section
3.3.1). The oxidation catalyst operation is
acceptable if no FID response is noted.
5.2.2 Analyzer Linearity Check and NMO
Calibration. Operating both the oxidation and
reduction catalysts, conduct a linearity check
of the analyzer using the propane standards
specified in section 3.3. make triplicate
injections of each calibration gas and then
calculate the average response factor (area/
ppm C) for each gas, as well as the overall
mean of the response factor values. The
instrument linearity is acceptable if the
average response factor of each calibration
gas is within ± 5 percent of the overall mean
value and if the relative standard deviation
(section 6.7) for each set of triplicate
Ill-Appendix A-118
-------
injections 1» IBM than ± 5 percent Record the
overall mean of the propane response factor
values as the NMO calibration response
factor (RFuo).
6.2.3 Reduction Catalyst Efficiency Check
and COi Calibration. An exact determination
of the-reduction catalyst efficiency is not
required. Instead, proper catalyst operation is
indirectly checked and continuously
monitored by establishing a COi response
factor and comparing it to the NMO response
factor. Operating both the oxidation and
reduction catalysts make triplicate injections
of each of the CO, calibration gases (section
3.3.3). Calculate the average response factor
(area/ppm) for each calibration gas, as well
as the overall mean of the response factor
values. The reduction catalyst operation is
acceptable if the average response factor of
each calibration gas is within ± 5 percent of
the overall mean value and if the relative
standard deviation (section 6.7) for each set
of triplicate injections is less than ± 5
percent Additionally, the CO, overall mean
response factor must be within ± 10 percent
of the NMO calibration response factor
(RFnn,) calculated in section 5.2,2. Record the
overall mean of the response factor values as
the CO, calibration response factor (RFCO,).
6.2.4 NMO System Blank. For the high
level CO, calibration gas (section 3.3,3)
record the NMO value measured during the
CO, calibration conducted in section 5.2.3.
This value is the NMO blank value for the
analyzer (BJ and should be less than 10 ppm.
&2.S System Performance Check. Check
the column separation and overall
performance of the analyzer by making
triplicate injections of the calibration gases
listed in section 3.3.4. The analyzer
performance is acceptable if the measured
NMO value for each gas (average of triplicate
injections) is within ± 12 percent of the
expected value.
6.3 NMO Analyzer Daily Calibration.
6.3.1 NMO Blank and CCv Inject
triplicate samples of the high level CO,
calibration gas (section 3.3.3) and calculate
the average response factor. The system
operation is adequate if the calculated
response factor is within ± 10 percent of the
RFooi calculated during the initial
performance test (section 5^.2). Use the daily
response factor (DRF^) for analyzer
calibration and the calculation of measured
CO, concentrations in the collection vessel
samples. In addition, record the NMO blank
value (BJ; this value should be less than 10
ppm.
6.3.2 NMO Calibration. Inject triplicate
samples of the mixed propane calibration
cylinder (section 3.3.4.1) and calculate the
average NMO response factor. The system
operation is adequate if the calculated
response factor is within ± 10 percent of the
RFmo calculated during the initial
performance test (section 5.2.1). Use the daily
response factor (DRFmo) for analyzer
calibration and calculation of NMO
concentrations in the «ample tanks.
6.4 Sample Tank. The volume of the gas
sampling tanks used must be determined.
Prior to putting each tank in service,
determine the tank volume by weighing the
tanks empty and then filled with deionized
distilled water; weigh to the nearest 5 gm and
record the results. Alternatively, measure the
volume of water used to fill the tanks to the
nearest 6 ml
5.5 -Intermediate Collection Vessel The
volume of the intermediate collection vessels
used to collect CO, during the analysis of the
condensate traps must be determined. Prior
to patting each vessel into service, determine
the volume by weighing the vessel empty and
then filled with deionized distilled water:
weigh to the nearest 5 gm and record the
results. Alternatively, measure the volume of
water used to fill the tanks to the nearest 6
ml
Ill-Appendix A-119
-------
H
H
H
>
t)
"O
n>
3
H-
X
NJ
O
6. Calculations
Note: All equations are written using absolute pressure;
i
absolute pressures are determined by adding the measured barometric
pressure to the measured gauge pressure.
6.1 Sample Volume, For each test run, calculate the gas
volume sampled:
V, « 0.386 V (-£ - JtL)
s \Tt Tt1/
6.2 Noncondenslble Organlcs. For each sample tank, determine
the concentration of nonmethane organics (ppm C):
r1
pt pti
* £ C
. B
tnij a
6.3 Condenslble Organlcs, For each condensate trap determine
the concentration of organics (ppm C):
C. - 0.386
VvPf
s f
cnv
6.4 Total Gaseous Nonmethane Organlcs (TGNMO). To determine
the TGNMO concentration for each test run, use the following
equation:
6.5 Total Gaseous Nonmethane Organlcs (TGNMO) Mass
Concentration. To determine the TGNMO mass concentration as
carbon for each test run, use the following equation:
Mr • 0.498 C
6.6 Percent Recovery. To calculate the percent recovery for
the liquid Injections to the condensate recovery and conditioning
system use the following equation:
percent recovery « 1.6 r
W
6.7 Relative Standard Deviation.
Pf Ccm
T7 IT
RSD
I (X1 r X)'
n - 1
-------
Where:
B. = Measured NMO blank value for NMO
analyzer, ppm C.
B, = Measured CO, "^ «*» *" ox***™ •»«"">
•nd cnndlUoiUna mum cantor KM, ppm CO
C=total gaseous nonmethane organic
(TCNMO) concentration of the effluent.
ppm C equivalent.
0,: = Calculated condensible organic
(condensate trap) concentration of the .
effluent, ppm C equivalent.
COT = Measured concentration (NMO
analyzer) for the condensate trap
(intermediate collection vessel), ppm
CO,
C, = Calculated noncondensible organic
concentration (sample tank) of the
effluent, ppm C equivalent.
dm=Measured concentration (NMO
analyzer) for the sample tank, ppm NMO.
L=Volume of liquid injected, microliters.
M = Molecular weight of the liquid injected,
g/g-mole.
MC = total gaseous non-methane organic
(TGNMO) mass concentration of the
effluent, mg C/dscm.
N = Carbon number of the liquid compound
injected (N = 7 for toluene, N=6 for
hexane).
P,=Final pressure of the intermediate
collection vessel, mm Hg absolute.
Pu = Gas sample tank pressure prior to
sampling, mm Hg absolute.
P, = Gas sample tank pressure after sampling.
but prior to pressurizing, mm Hg
absolute.
Pu= Final gas sample tank pressure after
pressurizing, mm Hg absolute.
T,=Fmal temperature of intermediate
collection vessel, °K.
Tu = Sample tank temperature prior to
sampling. °K.
T, = Sample tank temperature at completion
of sampling. °K.
Tu=Sample tank temperature after
pressurizing °K.
V = Sample tank volume, cm.
V. = Intermediate collection vessel volume,
cm
V, = Gas volume sampled, dscm.
n = Number of data points.
q=Total number of analyzer injections of
intermediate collection vessel during
analysis (where k = injection number, 1
. . . q).
r = Total number of analyzer injections of
sample tank during analysis (where
j = injection number, 1. . . r).
x, = Individual measurements.
X —Mean value.
p = Density of liquid injected, g/cc.
7. Bibliography
7.1 Salo, Albert E.. Samuel Witz, and
Robert D. MacPhee. Determination of Solvent
Vapor Concentrations by Total Combustion
Analysis: A Comparison of Infrared with
Flame lonization Detectors. Paper No. 75-33.2
(Presented at the 68th Annual Meeting of the
Air Pollution Control Association. Boston,
MA. June 15-20,1975.) 14 p.
7.2 Salo, Albert E.. William L. Oaks, and
Robert D. MacPhee. Measuring the Organic
Carbon Content of Source Emissions for Air
Pollution Control. Paper No. 74-190.
(Presented at the 67th Annual Meeting of the
Air Pollution Control Association. Denver,
CO. June 9-13,1974.) 25 p.
Method 25
Addendum I. System Components
In test Method 25 several important system
components are not specified; instead
minimum performance specifications are
provided. The method 1» written in this
manner to permit individual preference in
choosing components, as well as to
encourage development and use of improved
components. This addendum is added to the
method in order to provide users with some
specific information regarding components
which have been found satisfactory for use
with the method. This listing is given only for
the purpose of providing information and
does not constitute an endorsement of any
product by the Environmental Protection
Agency. This list is not meant to imply that
other components not listed are not
acceptable.
1. Condensate Recovery and Conditioning
System Oxidation Catalyst. %" ODX14"
inconel tubing packed with 8 inches of
hopcalite* oxidizing catalyst and operated at
BOO'C in a tube furnace. Note: At this
temperature, this catalyst must be purged
with carrier gas at all times to prevent
catalyst damage.
2. NMO Analyzer Oxidation Catalyst. Vt"
ODX14" inconel tubing packed with 6 inches
of hopcalite oxidizing catalyst and operated
at 800°C in a tube furnace. (See note above.).
3. NMO Analyzer Reduction Catalyst.
Reduction Catalyst Module; Byron
Instruments, Raleigh, N.C.
4. Gas Chromatographic Separation
Column. Vs inch OD stainless steel packed
with 3 feet of 10 percent methyl silicone. Sp
2100 (or equivalent) on Supelcoport (or
equivalent), 80/100 mesh, followed by 1.5 feet
Porapak Q (or equivalent) 60/80 mesh. The
inlet side is to the silicone. Condition the
column for 24 hours at 200°C with 20 cc/min
N, purge.
During analysis for the nonmethane
organics the separation column is operated as
follows: First, operate the column at — 78°C
(dry ice bath) to elute CO and CH4. After the
CM. peak operate the column at 0°C to elute
CO,. When the CO, is completely eluted,
switch the carrier flow to backflush the
column and simultaneously raise the column
temperature to 100°C in order to elute all
nonmethane organics (exact timings for
column operation are determined from the
calibration standard).
Note.—The dry ice operating condition
may be deleted if separation of CO and CH,
is unimportant.
Note.—Ethane and ethylene may or may
not be measured using this column; whether
or not ethane and ethylene are quantified will
depend on the CO, concentration in the gas
sample. When high levels of CO, are present,
ethane and ethylene will elute under the tail
of the CO, peak.
5. Carrier Gas. Zero grade nitrogen or
helium or zero air.
'MSA registered trademark.
Ill-Appendix A-121
-------
PROBE
EXTENSION
(IF REQUIRED)
•o-
VACUUM
GAUGE
FLOW
RATE
CONTROLLER
PROBE
STACK
WALL
il
_L ON/OFF
nk FLOW
^ \ VALVE
CONNECTOR
CONDENSATE
TRAP
EVACUATED
SAMPLE
TANK
Figure 1. Sampling apparatus.
III-Appendix A-122
-------
CARRIER GAS
.CALIBRATION STANDARDS
SAMPLE TANK
INTERMEDIATE
COLLECTION
VESSEL
(CONDITIONED TRAP SAMPLE)
NON-METHANE
ORGANICS
HYDROGEN
COMBUSTION
AIR
Figure 2. Simplified schematic of non-methane organic (NMO) analyzer.
Ill-Appendix A-123
-------
CATALYST
BYPASS VALVE
T
SEPARATION
COLUMN
NONMETHANE
ORGANIC
(BACKFLUSH)
CO
C02
CH4
COLUMN\V
BACKFLUSH^
VALVE
SAMPLE
INJECT
VALVE
SAMPLE /CALIBRATION
TANK / CYLINDERS
OXIDATION
CATALYST
HEATED
CHAMBER
GAS
PURIFICATION
FURNACE
HEATED CHAMBER
FLOW
METER
Figure 3. Nonmethane organic (NMO) analyzer.
-------
\
FLOW __._
1 X" MCTCOC ~--^ TRAP
a u-jK ^cn
y ~^ FLOW
Kt .CONTROL
,..., /fj VALVES"^
f i iS^l- f^^1 ""
^
SWITCHING
i— —\ VALVES i— —i
1 r/>x •• -, n iSL "^
1 CONNECTORS^ ^
S i vl «
' PURIFIER j-L^ "^| c
' — \2*Q PURIFIER |
i
VftLVEV-j)
dj
VACUUM" >
PUMP ME
MAN
f\ <
CA
02 *P
0
7_f\ REGULATING V
^V VALVE />
QUICK r^-
CONNECT IP
/^
<^y
T y c
X PROBE c
/^-ENO C
X A ^
1^1 L/*
i-L //\ HEAT
RRIER SAMPLE
ercent CONOENSATE
2/N2 TRAP
U
&
VENT HEAT
/J^. NDIR
( f-)— ANALYZER*
L-h * FOR MONITORING PROG
^ k OF COMBUSTION ONL
1
••FOR EVACUATING
*=^ iMTFRMFniATF VtSStlS ANU SAM
RCURY 'rnMcr?,^ (OPTION*
OMETER C°J)LEESsI[
HEAT
TRACE
• <
cV
pf-»
r^ ^— -
CATALYST
BYPASS
VENT |^
WAY ^^
ALVES^I
1 OXIDATION
I CATALYST
j HEATED
CHAMBER
RESS
Y
COLLECTIOf
PLE TANKS
L)
1 I
1 i
1 1
V
H20
TRAP
1
1
1
„ 1
1
|
Figure 4. Condensate recovery and conditioning apparatus.
Ill-Appendix A-125
-------
PROBE. 3mm (1/8 w) O.D.
CONNECTOR
EXIT TUBE. 6mm ('/. in) 0.0
INLET TUBE. 6mm (!i in) O.D.
qp
^CONNECTOR
NO. 40 HOLE
(THRU BOTH WALLS)
CONNECTOR/REDUCER
CRIMPED AND WELDED GAS TIGHT SEAL
^BARREL 19mm W in) 0.0. X 140mm (5 % in) LONG.
1.5mm (1/16 in) WALL
WELDED JOINTS
BARREL PACKING. 316 SS WOOL PACKED TIGHTLY
AT BOTTOM. LOOSELY AT TOP
HEAT SINK (NUT.PRESS-FIT TO BARREL)
WELDED PLUG
MATERIAL: TYPE 316 STAINLESS STEEL
Figure 5 Condensat?
Ill-Appendix A-126
-------
INJECTION
SEPTUM
CONNECTING T
FROM
CARRIER
APPRO X.
IS cm (6 in)
CONNECTING
FLBOW
TO
CATALYST
6 mm (1/4 in)
316 SS TUBING
Figure 6. Liquid sample injection unit.
Ill-Appendix A-127
-------
VOLATILE ORGANIC CARBON
FACIIIT¥_
LOCATION.
DATE
SAMPLE LOCATION.
OPERATOR
RUN NUMBER
TANK NUMBER.
.TRAP NUMBER.
.SAMPLE 10 NUMBER.
TANK VACUUM,
mm Hg cm Hg
PRETEST (MANOMETER)
POST TEST (MANOMITERl.
ir.Alir.M
(RAIIRF)
BAROMETRIC
PRESSURE.
mm Hg
AMBIENT
TEMPERATURE.
°C
LEAK RATE
cm Hg / 10 min
PRETEST.
POST TEST.
TIME
CLOCK/SAMPU
GAUGE VACUUM.
em Hg
FLOWMETERSETTWC
COMMENTS
Figure 7. Example Field Data Form.
Ill-Appendix A-128
-------
I
I
HEATED |
1 CHAMBER |
VENT
(CLOSED)\£-{)
A
(OPEN) y
Z_f\ REGULATING ^
\*/ VALVE /
(OPEN)
QUICK r-
CONNECTlr
\u
NOIR
ANALYZER*
/-{) FOR MONITORING PROGRESS
^ k OF COMBUSTION ONLY
3
l
I I
VACUUM**
PUMP
H20
TRAP
MERCURY
MANOMETER
INTERMEDIATE
COLLECTION
VESSEL
"FOR EVACUATING COLLECTION
VESSELS AND SAMPLE TANKS
(OPTIONAL)
Figure 8. Condensate recovery and conditioning apparatus, carbon dioxide purge.
Ill-Appendix A-129
-------
(CLOSED)
FLOW
METERS
FLOW
CONTROL
{ VALVES N
SWITCHING
VALVES
CONNECTORS
CATAtVSI
BYPASS
SAMPLE
CONOENSATE
TRAP
CARRIER
percent
02/N2
OXIDATION
CATALYST
NOIR
ANALYZER
FOR MONITORING PROGRESS
OF COMBUSTION ONLY
REGULATING
VALVE
(OPEN)
QUICK
CONNECT
V
H20
TRAP
VACUUM
PUMP
MERCURY
MANOMETER
INTERMEDIATE
COLLECTION
VESSEL
••FOR EVACUATING COLLECTION
VESSELS AND SAMPLE TANKS
(OPTIONAL)
Figure 9. Condensate recovery and conditioning apparatus, collection of trap orgamct
Ill-Appendix A-130
-------
18
APPENDIX B—PERFORMANCE SPECIFICATIONS
Performance Specification 1—Performance
specifications and specification test proce-
dures for transmlssometer systems for con-
tinuous measurement of the opacity of
'stack einlasiong ;" 2i
1. Principle and Applicability.
1.1 Principle. The opacity of partlculate
matter In stack emissions Is measured by a
continuously operating emission measure-
ment system. These systems are based upon
the principle of transmlssometry which Is a
direct measurement of the attenuation of
visible radiation (opacity) by participate
matter in a stack effluent. Light having spe-
cfic spectral characteristics is projected from
a lamp across the stack of a pollutant source
to a light sensor. The light Is attenuated due
to absorption and scatter by the partlculate
matter in the effluent. The percentage of
visible light attenuated is defined as the
opacity of the emission. Transparent stack
emissions that do not attenuate light will
have a transmlttance of 100 or an opacity of
0. Opaque stack emissions that attenuate all
of the visible light will have a transmittance
of 0 or an opacity of 100 percent. The trans-
mlssometer is evaluated by use of neutral
density filters to determine the precision of
the continuous monitoring system. Tests of
the system are performed to determine zero
drift, .calibration drift, and response time
characteristics of the system.
1.2 Applicability. This performance spe-
cification is applicable to the continuous
monitoring systems specified in the subparts
for measuring opacity of emissions. Specifi-
cations tor continuous measurement of vis-
ible emissions are elven in terms of. design,
performance, and installation parameters.
These specifications contain test procedures,
installation requirements, and data compu-
tation procedures for evaluating the accept-
ability of the continuous monitoring systems
subject to approval by the Administrator.
2. Apparatus.
2.1 Calibrated Filters. Optical filters with
neutral spectral characteristics and known
optical densities to visible light or screens
known to produce specified optical densities.
Calibrated filters with accuracies certified by
the manufacturer to' within ±3 percent
opacity shall be used. Filters required are
low. mid, and high-range filters with nom-
inal optical densities as follows-when the
transmlssometer is spanned at opacity levels
specified by applicable subparts:
Calibrated filter optical densities
with equivalent opacity in
Span val
(percent op
50 .
60
70
80
90
100
ue parenthesis
Low-
range
0.1 (20)
.1 (20)
... .1 (20)
... .1 (20)
1 (20)
1 (20)
Mid-
range
0.2 (37)
2 (37)
3 (50)
3 (50)
4 (60)
4 (60)
Hiph-
ranpe
0.3 (50)
.3 (50)
.4 (60)
.6 (75)
.7 (SCrt
It Is recommended that filter calibrations
be checked with a well-colllmated photopic
transmlssometer of known linearity prior to
use. The filters shall be of sufficlint size
to attenuate the entire light beam of the
transmissometer.
23 Data Recorder. Analog chart recorder
or other suitable device with Input voltage
range compatible with the analyzer sys;em
output. The resolution of the recorder's
data output shall be sufficient to allow com-
pletion of the test procedures within this.
specification. 23
2.3 Opacity measurement System. An In-
stack transmissometer (folded or single
path) with the optical design specifications
designated below, associated control units
and apparatus to keep optical surfaces clean.
3. Definitions.
3.1 Continuous Monitoring System. The
total equipment required for the determina-
tion of pollutant opacity in a source effluent.
Continuous monitoring systems consist of
major subsystems as follows:
3.1.1 Sampling Interface. The portion of a
continuous monitoring system for opacity
that protects the analyzer from the effluent.
3.12 Analyzer. That portion of the con-
tinuous monitoring system which senses the
pollutant and generates -a signal output that
is a function of the pollutant opacity.
3.1.3 Data Recorder. That portion of the
continuous monitoring system that processes
the analyzer output and provides a perma-
nent record of the output signal in terms of
pollutant opacity.
32 Transmissometer. The portions of a
continuous monitoring system for opacity
that include the sampling Interface end the
analyzer.
33 Span. The -value of opacity at which
the continuous monitoring system is set to
produce the maximum date display output.
The span shall be set at an opacity specified
in each applicable subpart.
3.4 Calibration Error. The difference be-
tween the opacity reading indicated by the
continuous monitoring system and the
known values of a series of test standards.
For this method the test standards are a
series of calibrated optical filters or screens.
3.5 Zero Drift; The change in continuous
monitoring system output over a stated pe-
riod of time of normal continuous operation
when the pollutant concentration at the
time of the measurements Is zero.
3.6 Calibration Drift. The change in the
continuous monitoring system output over
a stated period of time-of normal continuous
operation -when the pollutant concentration
at the time of the measurements is the same
known upscale value.
3.7 System Response. The time interval
from a step change In opacity in the stack
at the Input to the continuous monitoring
system to the time at which 95 percent of
the corresponding final value is reached as
displayed on the continuous monitoring sys-
tem data recorder.
3.8 Operational Test Period. A minimum
pertod of time over which a continuous
monitoring system is expected to operate
within certain performance specifications
without unscheduled maintenance, repair,
or adjustment.
3.9 Transmittance. The fraction o-f incident
light that Js transmitted through an optical
medium of interest.
3.10 Opacity. The fraction of Incident light
that 13 attenuated by an optical medium of
interest. Opacity (O) and transmittance (T)
are related as" follows:
O=l—T
3.11 Optical Density. A logarithmic meas-
ure of the amount of light that It attenuated
by an optical medium of interest. Optical
density (D) is related to the transmittance
and opacity as follows:
D=-logIOT
D=-log,0 (1-0)
3.12 Peak . Optical Response. The wave-
length of maximum sensitivity.of the Instru-
ment.
3.13 Mean Spectral Response. The wave-
length which bisects the total area under
the curve obtained pursuant to paragraph
9.2.1.
3.14 Angle of View. The maximum (total)
angle of radiation detection by the photo-
detector assembly of the analyzer.
3.15 Angle of Projection. The maximum
(total) angle that contains 95_ percent of
the radiation projected from the lamp assem-
bly of the analyzer. ' '
3.16 Pathlength. The depth of effluent in
the light beam between the receiver and the
transmitter of the single-pass transmissom-
eter, or the depth of effluent between the
transceiver and reflector of a double-pass
transmissometer. Two pathlengths are refer-
enced by this specification:
3.16.1 Monitor Pathlength. The depth of
effluent at the Installed location of the con-
tinuous monitoring system.
3.16.2 Emission Outlet Pathlength. THe
depth of effluent at the location emissions are
released to the atmosphere.
4. Installation Specification.
4.1 Location. The transmlssometer must
be located across a section of duct or stack
that will provide a particulate matter flow
through the optical volume of the trans-
mlssometer that is representative of the par-
ticulate matter flow through the duct or
stack. It is recommended that the monitor
pathlength or depth of effluent for the trans-
missometer include the entire diameter of
the duct or stack. In Installations using a
shorter pathlength, extra caution must be
used in determining the measurement loca-
tion representative of the particulate matter
flow through the duct or stack.
4.1.1 The transmlssometer location shall
be downstream from all partlculate control
equipment.
4.1.2 The transmissometer shall be located
as far from bends and obstructions as prac-
tical. . .
4.1.3 A transmissometer that is located
In the duct or stack following a bend shall
be Installed In the plane defined by the
bend where possible.
4.1.4 ,The transmissometer should be In-
stalled In an accessible location.
4.1.5 When required by the Administrator,
the owner or operator of a source must
demonstrate that the transmlssometer is lo-
cated in a section of duct or stack where
a representative particulate matter distribu-
tion exists. The determination shall be ac-
complished by examining the opacity profile
of the effluent at a series of positions across
the duct or stack while the plant is in oper-
ation at maximum or reduced operating rates
or by other tests, acceptable to the Adminis-
trator. ,
4.2 Slotted Tube. Installations that require
the use of a slotted tube shall use a slotted
tube of sufficient size and blackness so as
not to Interfere with the free flow of effluent
through the entire optical volume of the
transmlssometer or reflect light into the
transmissometer photodetector. Light re-
flections may be prevented by using black-
ened baffles within the slotted tube to pre-
vent the lamp radiation from Impinging upon
the tube walls, by restricting the angle of
projection of the light and the angle of view
of the photodetector assembly to less than
the cross-sectional area of the slotted tube,
or by other methods. The owner or operator
must show that the manufacturer of the
monitoring system has used appropriate
methods to minimize light reflections for
systems using slotted tubes.
4.3 Data Recorder Output. The continuous
monitoring system output shall permit ex-
panded display of the span opacity on a
standard 0 to 100 percent scale. Since all
opacity standards are based on the opacity
of the effluent exhausted to the atmosphere,
the system output shall be based upon the
emission outlet pathlength and permanently
recorded. For affected facilities whose moni-
tor pathlength is different from the facility's
emission outlet pathlength, a graph shall be
provided with the Installation.to show the
relationships between the continuous moni-
toring system recorded opacity based upon
the emission outlet pathlength and the opac-
ity of the effluent at the analyzer location
(monitor pathlength). Tests for measure-
ment of opacity that are required by this
performance specification are based upon the
I!I-Appendix B-l
-------
monitor pathlength. The graph necessary to
convert the data • recorder output to the
monitor pathlength-basis shall be established
as follows:
log (1-0.) =(!,/!,) log (1-00
where:
0, = the opacity of the effluent based upon
*i-
,0s = the opacity of the effluent based upon
12.
l, = the emission outlet pathlength.
13=the monitor pathlength.
5. Optical Design Specifications.
The optical design specifications set forth
In Section 6.1 shall be met in order for a
measurement system to comply with the
requirements of this method.
6. Determination of Conformance with De-
sign Specifications.
6.1 The continuous monitoring system for
measurement of opacity shall be demon-
strated to conform to the design specifica-
tions set forth as follows:
6.1.1 Peak Spectral Response. The peak
spectral response of the continuous moni-
toring systems shall occur between 500 nm
and 600 nm. Response at any wavelength be-
low 400 nm or above 700 nm shall be less
than 10 percent of the peak response of the
continuous monitoring system.
6.1.2 Mean Spectral Response. The mean
spectral response of the continuous monitor-
ing system shall occur between 500 nm and
600 nm.
6.1.3 Angle of View. The total angle of view
shall be no greater than 5 degrees.
6.1.4 Angle of Projection. The total angle
of projection shall be no greater than 5 de-
gress.
6.2 Conformance with the requirements
of section 6.1 may be demonstrated by the
owner or operator of the affected facility by
testing each analyzer or by obtaining a cer-
tificate of Conformance from the instrument
manufacturer. The certificate must certify
that at least one analyzer from each month's
production was tested and satisfactorily met
all applicable requirements. The certificate
must state that the first analyzer randomly
campled met all requirements of paragraph
6 of this specification. If any of the require-
ments were not met, the certificate must
show that the entire month's analyzer pro-
duction was resampled according to the mili-
tary standard 105D sampling procedure
(MIL-STD-105D) Inspection level II; was re-
tested for each of the applicable require-
ments under paragraph 6 of this specifica-
tion; and was determined to be acceptable
under MIL-STD-105D procedures. The certifi-
cate of Conformance must show the results
of each test performed 'for the analyzers
sampled during the month the analyzer be-
ing installed was produced. "
6.3 The general test procedures to be fqj-
lowed to demonstrate Conformance with Sec-
tion 6 requirements are given as follows:
(These procedures will not be applicable to
all designs and will require modification In
some cases. Where analyzer and optical de-
sign Is certified by the manufacturer to con-
form with the angle of view or angle of pro-
jection specifications, the respective pro-
csdures may be omitted.)
. 6.3.1 Spectral Response. Obtain spectral
data for detector, lamp, and filter components
used In the measurement system from their
respective manufacturers.
6.3.2 Angle of View. Set the received up
as specified by the manufacturer. Draw an
arc with radius of 3 meters. Measure the re-
ceiver response to a small (less than 3
centimeters) non-directional light source at
5-centimeter intervals on the arc for 26 centi-
meters on either side of the detector center-
line. Repeat the test in the vertical direction.
6.3.3 Angle of Projection. Set the projector
up as specified by the manufacturer. Draw
an arc with radius of 3 meters. Using a small
photoelectric light detector (less than 3
centimeters), measure the light intensity at
5-centimeter intervals on the arc for 26
centimeters on either side of the light source
centerline of projection. Repeat the test in
the vertical direction.
7. Continuous Monitoring System Pei-
formance Specifications. .
. The continuous monitoring system shall
meet the performance specifications In Table
1-1 to be considered acceptable under 'this
method.
TABLE 1-1.—Performance specifications
Parameter
Specificaliont
a. .Calibration error <3 pet opacity."
b Zero drift (24 h)....: <2 pet opacity.'
c.Calibration drift (24 h) <2 pet opacity.'
d. Response time 10 s (maximum).
e. Operational test period 168 h.
' Expressed as sum of absolute mean value and -the
95 pet confidence Interval of a series of tests.
8. Performance Specification Test Proce-
dures. The following test procedures shall be
used to determine Conformance with the re-
quirements of paragraph 7:
8.1 Calibration Error and Response Time
Test. These tests are to be performed prior to
installation of the system on the stack and
may be performed at the affected facility or
at other locations provided that proper notifi-
cation Is given. Set up and calibrate the
measurement system as specified by the
manufacturer's written instructions for the
monitor pathlength to be used In the In-
stallation. Span the analyzer as specified In
applicable subparts.
8.1.1 Calibration Error Test. Insert a series
of calibration filters in the transmissometer
path at the midpoint. A minimum of three
calibration filters (low, mid, and high-
range) selected In accordance with the table
under paragraph 2.1 and calibrated -within
3 percent must be used. Make a total of five
nonconsecutlve readings for each filter.
Record the measurement system output
readings In percent opacity. (See Figure 1-1.)
8.1.2 "System Response Test. Insert the
high-range filter In the transmlssometer
path five times and record the-time required
for the system to respond to 95 percent of
final zero and high-range filter values. (See
Figure 1-2.)
8.2 Field" Test for Zero Drift and Calibra-
tion Drift. Install the continuous monitoring
system on the affected facility and perform
the following alignments:
8.2.1 Preliminary Alignments. As soon as
possible after Installation and once a year
thereafter when the facility Is not In opera-
tion, perform the following optical and zero
alignments:
85.1.1 Optical Alignment. Align the light
beam from the transmlssometer upon the op-
tical surfaces located across the effluent (I.e.,
the retroflector or photodetector as applica-
ble) In accordance with the manufacturer's
Instructions.
8.2.1.2 Zero Alignment. After the transmls-
someter has been optically aligned and the
transmlssometer mounting Is mechanically
stable (I.e., no movement of the mounting
due to thermal contraction of the stack,
duct, etc.) and a clean stack condition has
been determined by a steady zero opacity
condition, perform the zero alignment. This
alignment Is performed by balancing the con-
tinuous monitor system response so that any
simulated zero check coincides with an ac-
tual zero check performed across the moni-
tor pathlength of the clean stack.
8.2.1.3 Span. Span the continuous monitor-
Ing system at the opacity specified in sub-
parts and offset the zero setting at least 10
percent of span so that negative drift can be
quantised.
8.2.2. Final Alignments. After the prelimi-
nary alignments have been completed and the
affected facility has been-started up and
reaches normal- operating temperature, re-
check the optical alignment In accordance
with 8.2.1.1 of this specification"* If the align-
ment has shifted, realign the optics, record
any detectable shift in the opacity measured
by the system that can be attributed to the
optical realignment, and notify the Admin-
istrator. This condition may not be objec-
tionable If the affected facility operates with-
in a fairly constant and adequately narrow
range of operating temperatures that does
not produce significant shifts in optical
alignment during normal operation of the
facility. Under circumstances where the facil-
ity operations produce fluctuations In the.
effluent gas temperature that result In sig-
nificant misalignments, the Administrator
may require Improved mounting structures or
another location for Installation of the -trans-
mlssometer.
8.2.3 Conditioning Period. After, complet-
ing the post-startup alignments, operate the
system for an Initial 168-hour conditioning
period In a normal operational manner.
8.2.4 Operational Test Period. After com-
pleting the conditioning period, operate the
system for an additional 168-hour period re-
taining the zero offset. The system shall mon-
itor the source effluent at all times except
when being zeroed or calibrated. At 24-hour
Intervals the zero and span shall be checked
according to the manufacturer's Instructions.
Minimum procedures used shall provide a
system check of the analyzer Internal mirrors
and all electronic circuitry Including the
lamp and photodetector assembly and shall
Include a procedure for producing a simu-
lated zero opacity condition and a simulated
upscale (span) opacity condition as viewed
by the receiver. The manufacturer's written
Instructions may be used providing that they
equal or exceed these minimum procedures.
Zero and span the transmlssometer, clean all
optical surfaces exposed to the effluent, rea-
lign optics, and make any necessary adjust-
ments to the calibration of the system dally.
These zero and calibration adjustments and
optical realignments are allowed only at 24-
hour Intervals or at such shorter Intervals as
the manufacturer's written Instructions spec-
ify. Automatic .corrections made by the
measurement system without operator Inter-
vention are allowable at any time. The mag-
nitude of any zero or span drift adjustments
shall be recorded. During this 168-hour op-
erational test period, record the following at
24-hour Intervals: (a) the zero reading and
span readings after the system Is calibrated
(these readings should be set at the same
value at the beginning of each 24-hour pe-
riod);. (b) the zero reading after each 24
hours of operation, but before cleaning and
adjustment; and (c) the span reading after
cleaning and zero adjustment, but before
span adjustment. (See Figure 1-3.)
9. Calculation, Data Analysis, and Report-
Ing.
8.1 Procedure for Determination of Mean
Values and Confidence Intervals.
9.1.1 The mean value of the data set Is cal-
culated according to equation 1-1.
n 1=1 Equation 1-1
where x,= absolute value of the individual
measurements,
S = sum of the individual values.
x=mearj value, and .,
n = number of data points.
9.1.2 The B5 percent confidence' Interval
(two-sided) is calculated according to equa-
tion 1-2:
C.I.rs = -
/n-1
Equation 1-2
where
£xi=sum of all data points,
t.t;s=ti — a/2, and
C.I.«5=95 percent confidence interval
estimate of the average mean
value.
The values in this table ere already cor-
rected for n-1 degrees of freedom. Use n equal
to the number of samples as data points.
Ill-Appendix B-2
-------
Values for t.s?5
n
2 ;........
3
4
5
6 i.
7
8.;.;
9 ... '
«.975
12.706
4 303
3. 18°
2.776
• 2. 571
2.447
2.865
2,300
n
10
11
12
13
14
15 . .
16
«.97o
2.262
2 228
2 201
2. 179
2 160
2. 145
2.131
92 Data Analysis and Reporting.
9.2.1 Spectral Response. -Combine the
spectral data obtained In accordance with
paragraph 6.3.1 to develop the effective spec-
tral response curve of the transmlssometer.
Report the wavelength at which the peak
response occurs, the wavelength at which the
mean response occurs, and the maximum
response at any wavelength below 400 nm
and above 700 nm expressed as a percentage
of the peak response as required under para-
graph 6.2.
9.2.2 Angle of View. Using the data obtained
In accordance with paragraph 6.3.2, calculate
•the response of the receiver as a function of
viewing angle In the horizontal and vertical
directions (26 centimeters of arc with a1
radius of 3 meters equal 5 degrees). Report
relative angle of view curves as required un-
der paragraph 6.2. '.
9.2.3 Angle of Projection. Using the data,
obtained In accordance with paragraph 6.3.3,
calculate the response of the photoelectric
detector as a function of projection angle In
the horizontal and vertical directions. Report
relative angle of projection curves as required
under .paragraph 6.2.
9.2.4 Calibration Error. Using the data from
paragraph 8.1 (Figure 1-1), subtract the
known filter opacity value from the value
shown by the measurement system for each
of the IS readings. Calculate the mean and
95 percent confidence Interval of the five dif-
ferent values at each test filter value accord-
Low .
Range 5
Span Value
opacity
t opacity
Hid High
Range I opacity Range _% opacity
Date of Test
Location of Test
Calibrated Filter
Analyzer Reading
% Opacity
Differences'
% Opacity
n
12
14.
15
Mean difference
Confidence Interval
Calibration error = Mean Difference + C.I.
Low Hid . High
Low, mid or high range
'Calibration fitter opacity - analyzer reading
Absolute value
Figure 1-1. Calibrator. Error Test
to equations 1—1 and 1-2. Report the sum
c.. the absolute mean difference and the 95
percent confidence Interval for each of the
'three test filters.
Dau of TMt
' S
-------
Zero Setting
Span Setting
. (Sbe paragraph 8.2.1) Dote of Test
Date Zero Rending
and (Before cleaning
Tims ond odjustosnt)
Span Reading Calibration
Zero Drift -(Aftrr cleaning and zero, adjustment Drift
(iZero) liut before span adjustment) (ASpan)
Zero Drift ° Mean Zero Drift"
•f CI (Zero)
Calibration Drift » Mean Span Drift" ,
+ CI (Span)
Absolute value
PERFOBMANCE SPECIFICATION 2—PERFORMANCE
SPECIFICATIONS AND SPECIFICATION TEST PRO-
CEDURES FOE MONITORS OF SOa AND NOx
,FROM STATIONARY SOURCES
1. Principle and Applicability.
1.1 Principle. The concentration of sulfur
dioxide or oxides of nitrogen pollutants in
stack emissions Is measured by a continu-
ously operating emission measurement sys-
tem. Concurrent with operation of the con-
tinuous monitoring system, the pollutant
concentrations are also measured with refer-
ence methods (Appendix A). An average of
the continuous monitoring system data .is
computed for each reference method testing
period and compared to determine the rela-
tive accuracy of the continuous monitoring
system. Other tests of the continuous mon-
itoring system are also performed to deter-
mine calibration error, drift, and response
characteristics of the system.
1.2 Applicability. This performance spec-
ification Is applicable to evaluation of con-
tinuous monitoring systems for measurement
ol nitrogen oxides or sulfur dioxide pollu-
tants. These specifications contain test pro-
cedures, Installation requirements, and data
computation procedures for evaluating the
acceptability of the continuous monitoring
systems. .
2. Apparatus.
2J. Calibration Gas Mixtures. Mixtures of
known concentrations of pollutant gas In a
diluent gas shall be prepared. The pollutant
gas shall be sulfur dioxide or the appropriate
oxlde(s) of nitrogen specified by paragraph
8 and within subparts. For sulfur dioxide gas
mixtures, the diluent gas may be air or nitro-
gen. For nitric oxide (NO) gas mixtures, the
diluent gas shall be oxygen-free (<10 ppm)
nitrogen, and for nitrogen dioxide (NO.) gas
mixtures the diluent gas shall be air. Concen-
trations of approximately 50 percent and 90
percent of span are required. The 90 percent
gas mixture Is used to set and to check the
opass and Is caferred to as the spaa gas.
2.2 Zero Goo. A gefl certified by the mcjna-
tocturer to contain Iocs than 1 ppm of the
polHttant SEO or ambient air may to ucstJ.
2.3 Equipment for measurement of the pol-
lutant gas concentration using the reference
method specified in the applicable standard.
2.4 Data Recorder. Analog chart recorder
or other suitable dsvice with Input voltage
range compatible with analyzer system out-
put. The'resolution of the recorder's data
output shall be sufficient to allow completion
of the test procedures within this specifi-
cation.
2.5 Continuous monitoring system for SO,
or NOr pollutants as applicable.
3. Definitions.
3.1 Continuous Monitoring System. The
total equipment required for the detennlnp-
-tton of a pollutant gas concentration In a
source effluent. Continuous monitoring sys-
tems consist of major subsystems as follows:
3.1.1 Sampling Interface—That portion of
an extractive continuous monitoring system
that performs one or more of the following
operations: acquisition, transportation, and
conditioning of a sample of the source efflu-
ent or that portion of an In-situ continuous
monitoring system that protects the analyzer
from the effluent.
3.1-.2 Analyzer—That portion of the con-
tinuous monitoring system which senses the
pollutant gas and generates a signal output
that is a function, of the pollutant concen-
tration.
3.1.3 Data Recorder—That portion of the
continuous monitoring system that provides
a permanent record of the output signal In
terms of concentration units.
3.2 Span. The value of pollutant concen-
tration at which the continuous monitor-
Ing system is set to produce the maximum
data display output. -The span shall be set
at the concentration specified in each appli-
cable subpart.
3.3 Accuracy (Relative). The degree of
correctness with which the continuous
monitoring system yields the value of gas
concentration of a sample relative to the
value, given by a denned reference mptfcoa.
TJils accuracy Is expressed in terms of error,
which Is the difference between the paired-
concentration macsurenranta enprecssd ca Q.
psccantege of tbo moan reference value. -
8.4 Calibration Error. The difference be-
tween the pollutant concentration Indi-
cated by the continuous monitoring system
and the known concentration of the test
gas mixture.
3.5 Zero Drift. The change to the continu-
ous monitoring system output over a stated
period of time of normal continuous opera-
tion when the pollutant concentration art
the tune for the measurements Is zero.
3.6 Calibration Drift. The change In the
continuous monitoring system output over
a stated time period of normal continuous
operations when the pollutant concentra-
tion at the time of the measurements Is the
same known upscale value.
3.7 Response Time. The time Interval
from a step change In pollutant concentra-
tion at the Input to the continuous moni-
toring system to the time at which 95 per-
cent of the corresponding' final value is
reached as displayed on the continuous
monitoring system data recorder.
3.8 Operational Period. A minimum period
of time over which a measurement system
is expected to operate within certain per-
formance specifications without unsched-
uled maintenance, repair, or adjustment.
3.9 Stratification. A condition Identified
by a difference In excess of 10 percent be-
tween the average concentration In the duct
or stack and the concentration at any point
more'than 1.0 meter from the duct or stack
wall.
4. Installation Specifications. Pollutant
continuous monitoring systems (SO, and
NO,) shall be Installed-at a sampling loca-
tion where measurements can be made which
are directly representative (4!l), or which
can be corrected so as to be representative
(45) of the total emissions from the affected
facility. Conformance with this requirement
shall be accomplished as follows:
4.1 Effluent gases may be assumed to be
nonstratifled if a sampling location eight or
more stack diameters (equivalent diameters)
downstream of any air In-leakage is se-
lected. This assumption and data correction
procedures under paragraph 4.2.1 may not
be applied to sampling locations upstream
of an air preheater In a stsara generating
facility under" Subpart D of this part. For
sampling locations where effluent gases are
either demonstrated (4.3) or may be as-
sumed to be nonstratifled (eight diameters),
a point (extractive systems) or path (in-situ
systems) of average concentration may be
monitored. 23
45 For sampling locations where effluent
gases cannot be assumed to be nonstrati-
fied (less than eight diameters) or have been
shown under paragraph 4.3 to be stratified,
results obtained must be consistently repre- '
sentatlve (e.g. a point of average concentra-
tion may shift with load changes) or the
data generated by sampling at a point (ex-
tractive systems) or across a path (in-situ
systems) must be corrected (4.2.1 arid 4.2.2)
so as to be representative of the total emis-
sions from the affected faculty. Conform-
ance with this requirement may be accom-
plished In either of the following ways:
4.2.1 Installation of a diluent continuous
monitoring system (O_ or CO, as applicable)
in accordance with the procedures under
paragraph 4.2 of Performance Specification
3 of this appendix. If the pollutant and
diluent monitoring systems are not of the
same type (both extractive or both In-sltu),
the extractive system must use a multipoint
probe.
45.2 Installation - of extractive pollutant
monitoring systems using multipoint sam-
pling probes or ln-sltu pollutant monitoring
systems that sample or view emissions which
are consistently representative of the total
emissions for the entire cross section. The
Administrator may require (fate, to bo oub-
III-Appendix B-4
-------
mltted to. demonstrate that the emissions
sampled or viewed are consistently repre-
sentative for several typical facility process.
operating conditions. ' ••••- - ' ••
4.3 The owner or operator may perform a
traverse to characterize any stratification of
effluent gases that might exist In a stack or
duct. If no stratification is present, sampling
procedures under paragraph 4.1 may be ap-
plied even though the eight diameter criteria
is not met.
4.4 When single point sampling probes for
extractive systems are Installed within the
stack or duct-under paragraphs 4.1 and 4.2.1.
.the sample may not be extracted at any point
less than 1.0 meter from the stack or duct
wall. Multipoint sampling probes Installed
under paragraph 4.2.2 may be located at any
points necessary to .obtain consistently, rep-
resentative samples.
5. Continuous Monitoring System Perform-
ance Specifications. :
The continuous monitoring system shall
meet-the performance specifications in Table
2-1 to be considered acceptable under 'this
method.
TABLE 2-1.—Performance speciflcationa
Parameter
Specification
1. Accuracy' <20 pet of the mean value of the reference method test
data. . . .
2. Calibration error i —^ — <, 5 pet of each (50 pet, 90 pet) calibration gas mixture
value.
3. Zero drift (2 h)' 2 pet of span
4. Zero drift (24 h)« ...;.. ;i...;.. Do.
5. Calibration drift (2 h)'. -.....-.. • Do.
6. Calibration drift (24 h)l ;- ;...» 2.5 pet. of span
7. Response Ume.... .......;.. : IS minmaximum.
8. Operational period.... ; ...i...... .:..- 168 h minimum.
1 Expressed as yr" of absolute mean value plus 95 pet confidence Interval of a series ottests.
tional 168-hour period retaining the zero
offset. The system shall monitor the source
effluent at all times except when being
zeroed, calibrated, or backpurged.
6.2.2.1 Field Test for Accuracy (Relative).
For continuous monitoring systems employ-
Ing extractive sampling, the probe tip for the
continuous monitoring system and the probe
tip for the Reference Method sampling train
should be placed at adjacent locations in the
duct. For NOX continuous monitoring sys-
tems, make 27 NOX concentration measure-
ments, divided into nine sets, using the ap-
plicable reference method. No more than one
set of tests, consisting of three Individual
measurements, shall be performed in any '
one hour. All individual measurements of
each set shall be performed concurrently,
or within a three-minute interval and the
results averaged. For SO, continuous moni-
toring systems, make nine SO. concentration
measurements using the applicable reference
method. No more than one measurement
shall be performed in any one hour. Record
the reference method test data and the con-
tinuous monitoring system concentrations
on the example data sheet shown In Figure
2-3.
6.2.22 Field Test for Zero Drift and Cali-
bration Drift. For extractive systems, deter-
mine the values given by zero and span gas
pollutant concentrations at two-hour inter-
vals until 15 sets of data are obtained. For
nonextractive measurement systems, the zero
value may be determined by mechanically
producing a zero condition that provides a
system check of the analyzer internal mirrors
and all electronic circuitry including the
radiation source and detector assembly or
by inserting three or more calibration gas
cells and computing the zero point from the
upscale measurements. If this latter tech-
nique is used, a graph (s) must be retained
by the owner or operator for each measure-
ment system that shows the relationship be-
tween the upscale measurements and the
zero point. The span of the system shall be
checked by using a calibration gas cell cer-
tified by the manufacturer to be function-
ally equivalent to SO percent of span concen-
tration. Record the zero and span measure-
ments (or the computed zero drift) on the
example data sheet shown In Figure 2-4.
The two-hour periods over which measure-
ments are conducted need not be consecutive
but may not overlap. All measurements re-
quired under this paragraph may be- con-
ducted concurrent with testa under para-
graph 622.1.
6. Performance Specification Test Proce-
dures. The following -test procedures shall be
used to determine conformance with the
requirements of paragraph 5. For NO, an-
requlrements of paragraph 5. For NOi an-
alyzers that oxidize nitric oxide (NO) to
nitrogen dioxide (NO,), the response time
test under paragraph 6~.3 of this method shall
be performed using nitric oxide (NO) span
gas. Other tests for NO, continuous monitor-
ing systems under paragraphs 6.1 and 62 and
all tests for sulfur dioxide systems shall be
performed using the pollutant span gas spe-
cified by each subpart.
6.1 Calibration Error Test Procedure. Set
up and calibrate the complete continuous
monitoring system according to the manu-
facturer's wrlten instructions. This may be
accomplished either in the laboratory or In
the field.
6.1.1 Calibration Gas Analyses. Triplicate
analyses of the gas mixtures shall be per-
formed within two weeks prior to use using
Reference Methods 6 for SO, and 7 for NO*.
Analyze each calibration gas mixture (50%,
G0%) and record the results on the example
sheet shown In Figure 2-1. Each sample test
result must be within 20 percent of the aver-
aged result or the tests shall be repeated.
This step may be omitted for non-extractive
monitors where dynamic calibration gas mix-
tures are not used (8.12).
6.12 Calibration Error Test Procedure.
Make a total of 15 nonconsecutive measure-
ments by alternately using zero gas and each
:allberatlon gas mixture concentration (e.g.,
3%. 50%, 0%, 90%. 50%. 90%. 50%, 0%.
etc.). For nonextractive continuous monitor-/
Ing systems, this test procedure may be per-
formed by using two or more calibration gas
cells whose concentrations are certified by
the manufacturer to be functionally equiva-
lent to these gas concentrations. Convert the
continuous monitoring system output read-
Ings to ppm and record the results on the •
example sheet shown In Figure 2-2.
62 Field Test for Accuracy (Relative),
Zero Drift, and Calibration Drift. Install and
operate the continuous monitoring system In
accordance with the manufacturer's written
Instructions and drawings-as follows:
62.1 Conditioning Period. Offset the zero
setting at least 10 percent of the span so
that negative zero drift can be quantified.
Operate the system for an Initial 168-hour
conditioning period In normal operating '
manner*
62.2.3 Adjustments. Zero and calibration
corrections and adjustments are allowed only
at 24-hour Intervals or at such shorter In-
tervals as the manufacturer's written In-
structions - specify. Automatic corrections
made by the measurement system without
operator intervention or initiation are allow-
able at any time. During the entire 168-hour
operational test period, record on the- ex-
ample sheet shown In Figure 2-5 the values
given by zero and span gas pollutant con-
centrations before' and after adjustment at
24-hour Intervals.
63 Field Test for Response Time.
63.1 Scope of Test. Use the entire continu-
ous monitoring system as Installed, including
sample transport lines If used. Flow rates,
line' diameters, pumping rates, pressures (do
not allow the pressurized calibration gas to
change the normal operating pressure In the
sample, line), etc.. shall be at the nominal
values for normal operation as specified In
the manufacturer's written Instructions. If
the analyzer is used to sample more than one
pollutant source (stack), repeat this test for
each sampling point.
6.32 Response Time 'Test Procedure. In-
troduce zero gas into the continuous moni-
toring system sampling Interface or as close
to the sampling Interface as possible. When
the system output reading has stabilized,
switch quickly to a known concentration of
pollutant gas. Record the time from concen-
tration switching to 95 percent of final stable
response. For non-extractive monitors,- the
highest available calibration gas concentra-
tion shall be switched Into and out of the
sample path and response times recorded.
Perform this test sequence three (3) times.
Record the results of each test on the
example sheet shown in Figure 2-6.
7. Calculations, Data Analysis and Report-
Ing. •
7.1 Procedure for determination of mean
values and confidence intervals.
7.1.1 The mean 'value of a data set is
calculated according to equation 2-1. '
. |-1 Equation 2--J
where:
xt=absolute value of the measurements,
Z=sum of the individual values,
x.=mean value, and 23
n = number of data points.
7.12 The 95 percent confidence Interval
(two-sided) is calculated according to equa-
tion 2-2: •
CT t.«TS
.1.94 = —r- —
Equation 2-2
where:
£xi=sum of all data points,
t.9ij=ti—a/2, and
C.I.jj=95 percent confidence interval
estimate of the average mean
value.
Values for'.975
I Operational Test Period. Operate the
continuous monitoring system for an addl-
The values in this table are already cor-
rected for n-1 degrees of freedom. Use n
ill-Appendix B-5
-------
equal to the number of sample* as data
point*.
7.8 Data Analysts and Reporting.
72.1 Accuracy (Relative). For each of the
nine reference method test points, determine
the average pollutant concentration reported
by the continuous monitoring system. These
average concentrations shall be determined
from the continuous monitoring system data
recorded under 7.2.2 by integrating or aver-
aging the pollutant concentrations over each
at the time Intervals concurrent with each
reference method testing period. Before pro--
ceedlng to the next step, determine the basis
(wet or dry) of the continuous monitoring
system data and reference method test data
concentrations. If the bases are not con-
sistent, apply a moisture correction to either
reference method concentrations or the con-
tinuous monitoring system concentrations
as appropriate. Determine the correction
factor by moisture tests concurrent with the
reference method testing periods. Report the
moisture test method and the correction pro-
cedure employed. For each of the nine test
runs determine the difference for each test
run by subtracting the respective reference
method test concentrations (use average of
each set of three measurements for NO.)
from the continuous monitoring system Inte-
grated or averaged concentrations. Using
these data, compute the mean difference and
the 95 percent confidence Interval of the dif-
ferences (equations 2-1 land 2-2). Accuracy
is reported au the sum of the absolute value
of the mean difference and the 95 percent
confidence Interval of the differences ex-
pressed as a percentage of the mean refer-
ence method value. Use the example sheet
shown In Figure 3-3.
7.2.2 Calibration Error. Using the data
from paragraph 6.1, subtract the measured
pollutant concentration determined under
paragraph 6.1.1 (Figure 2-1) from the value
shown by the continuous monitoring system
for each of the five readings at each con-
centration measured under 8.1.2 (Figure 2-2).
Calculate the mean of these difference values
and the 95 percent confidence intervals ac-
cording to equations 2-1 and 2-2. Report the
calibration error (the sum of the absolute
value of the mean difference and the 95 per- •
cent confidence Interval) as a percentage of
each respective calibration gas concentra-
tion. Use example sheet shown In Figure 2-2.
733 Zero Drift (2-hour). Using the zero
concentration- values measured each two
hours during the field test, calculate the dif-
ferences between consecutive two-hour read-
Ings expressed in ppm. Calculate the mean
difference and the confidence interval using
equations 2-1 and 2—2. Report the zero drift
as the sum of the absolute mean value and
the confidence Interval as a percentage of
. span. Use example sheet shown. In Figure
2-4. . -.-
7.2.4 Zero Drift (24-hour). Using the zero
concentration values measured every 24
hours during the field test, calculate the dif-
ferences between the zero point after .zero
adjustment and the zero value 24 hours later
just prior to zero adjustment.-Calculate the
mean value of these points and the 'confi-
dence interval.using equations 2-1 and 2-2.
Report the zero drift (the sum of the abso-
lute mean and confidence Interval) as a per-
centage of span. Use example sheet shown In
Figure 3-5.
- 7.2.5 Calibration Drift (2-hour). Using
the calibration values obtained at two-hour
Intervals during the field test, calculate the
differences between consecutive two-hour
readings expressed as ppm. These values
should be corrected for the corresponding
zero drift during that two-hour period. Cal-
culate the mean and confidence Interval of
these corrected difference values using equa-
tions 2-1 and 2—2. Do not use the differences
between non-consecutive readings. Report
the calibration drift as the sum of the abso-
lute mean and confidence Interval as a per-
centage of span. Use the example sheet shown
in Figure 2-4.
7.2.8 CJlbratlon Drift (24-hour). JJslng
tha calibration values measured every 24
hours during the field test, calculate the dif-
ferences between the calibration concentra-
tion reading after zero and calibration ad-
justment, and the calibration concentration
reading 24 hours later after zero adjustment
but before calibration adjustment. Calculate
the mean value of these differences and the
confidence Interval using equations 2-1 and
2-2. Report the calibration drift (the sum of
the absolute mean and confidence Interval)
as a percentage of span. Use the example
sheet shown in Figure 2-5.
7.2.7 Response Time. Using the charts
from paragraph 6.3, calculate the time Inter-
val from concentration switching to 95 per-
cent to the final stable value for all upscale
and downscale tests. Report the mean of the
three upscale test times and the mean of the
three downscale test times. The two aver-
age times should not differ by more than 15
percent of the slower time. Report the slower
time as the system response time. Use the ex-
ample sheet shown in Figure 2-8.
7.2.8 Operational Test Period. During the
168-hour performance and operational test
period, the continuous monitoring system
shall not require any corrective maintenance,
repair, replacement, or adjustment other than
that clearly specified as required In the op-
eration and maintenance manuals as routine
and expected during a one-week period. If
the continuous monitoring system operates
within the specified performance parameters
and does not require corrective maintenance,
repair, replacement or adjustment other than
as specified above during the 168-hour test
period, the operational period will be success-
fully concluded. Failure of the continuous
monitoring system to meet this requirement
shall call for a repetition of the 168-hour test
period. Portions of the test which were .satis-
factorily completed need not be repeated.
Failure to meet any performance specifica-
tions shall call for a repetition of the one-
week performance test period and that por-
tion of the testing which is related to the
failed specification. All maintenance and ad-
justments required shall be recorded. Out-
put readings shall be recorded before and
after all adjustments.
8. References.
8.1 "Monitoring Instrumentation for the
Measurement of Sulfur Dioxide in Stationary
Source Emissions," Environmental Protection
Agency, Research Triangle Park, N.C., Feb-
ruary 1973.
8.2 "Instrumentation for the Determina-
tion of Nitrogen Oxides Content of Station-
ary Source Emissions," Environmental Pro-
tection Agency, Research Triangle Park, N.C.,
Volume 1, APTD-0847. October 1971; Vol-
ume 2, AFTD-0942, January 1972.
3.3 "Experimental Statistics," Department
of Commerce, Handbook 91, 1963. pp. 3-31,
paragraphs 3-3.1.4.
8.4 "Performance Specifications for Sta-
tionary-Source Monitoring Systems for Gases
and Visible Emissions," Environmental Pro-
tection Agency, Research Triangle Park, K.C.,
EPA-«50/2-74-013, January 1974.
Itfenmci HctHxl Uirrl
(ipttil tlllbmlan IU» Hl«tur«
Antrtgt
«f bllbmlin CM Mitvm
. Ill-Appendix B-6
-------
Calibration Gas Mixture Data (From Figure 2-1):.
Mid (502) ppm High (90Z)
Run f
Calibration Gas
Concentration.ppin
Measurement System
Reading, ppn
Differences, ppm
n
n
Hid High
Mean difference
Confidence interval
Calibration error =
T
Mean Difference + C.I.
Average Calibration Gas Concentration
•x 100
Calibration gas concentration - measurement system reading
"Absolute value
Figure 2-2. Calibration Error Determination
NO.
1 .
f
J
4
5
<.
7
^
,
lit (
bccur
• iMf
date
Ttne
• Reference Method Samples
Saq>?e 1
(PPO)
i
i.
reference •
value (S02)
«>f1dence 1
letlwd
nttrvals •
NO
Smpfe 1
(ppn)
NO, NO .
Saipfe 2 Sanpfe 3
(ppn) j (ppn)
Mean rtferei
test value
« DOB
NO Sesple
Avenge
(PJ»)
.
Analyier l-Nhir
Average (pp>)>
$02 NO,
i
ice ecthod
NO )
($0.) • «
Difference
(PP»)
Man of
tke differences
MB
hem of the Differences , ,5, Conf1«ence"lnterval _ ,~. .
**'" Keen reference Mthod value " --
lain and report Mtnod used to determine Inttgrcttd averages
\ •
,«,,
Fljure t-3. Accuracy OtUnilMtlon (SOj nd W^) 57
Ill-Appendix B-7
-------
TIM
Begin End
Zero
Riming
Zero
Drift
UZero)
$p.n
Spin
Drift
(tSpsn)
Calibration
Drift
( Spin- Zero)
9
10
11
12
Zero Brift • [Mean Zero Orift*
Calibration Drift " [Kean Span Drift*
•Absolute Value.
2-4^. Zero ind Calibration Drift (2 Hour)
Date Zero Span Calibration
and Zero Drift Reading Drift
Time Reading (iZero) (After zero adjustment) (aSpan)
Zero Drift * [Mean Zero Drift*
. + C.I. (Zero)
* [Instrument Span] x 100
Calibration Drift = [Mean Span Drift*
* [Instrument Span] x 100
* Absolute value
C.I. (Span)'
Figure 2-5. Zero and Calibration Drift (24-hour)
Ill-Appendix B-8
-------
Date of Test
Span Gas Concentration _
Analyzer Span Setting
Upscale
1
2
3
_seconds
jseeonds
seconds
Downscale
Average upscale response
_seconds
_seconds
seconds
seconds
Average downscale response
System average response -time (slower time) « _
seconds
seconds.
^deviation from slower
system average response
average upscale minus average dow
slower time
mseals
x 1002
Figure H-6. Response Time
Performance Specification 3—Performance
specifications and specification test proce-
dures for monitors of CO, and O, from sta-
tionary sources.
1. Principle and Applicability.
1.1 Principle. Effluent gases are continu-
ously sampled and are analyzed for carbon
dioxide or oxygen by a continuous monitor-
ing system. Tests of the system are performed.
during a minimum operating period to deter-
mine zero drift, calibration drift, and re-
sponse time characteristics.
1.2 Applicability. This performance speci-
fication is applicable to evaluation of con-
tinuous monitoring systems for measurement
of carbon dioxide or oxygen. These specifica-
tions contain test procedures. Installation re-
quirements, and data computation proce-
dures for evaluating the acceptability of the
continuous monitoring systems subject to
approval by the Administrator. Sampling
may Include either extractive or non-extrac-
tive (In-sltu) procedures.
2. Apparatus.
2.1 Continuous Monitoring System for
Carbon Dioxide or Oxygen.
2.2 Calibration Gas Mixtures. Mixture of
known concentrations of carbon dioxide or
oxygen in nitrogen or air. Midrange and 90
percent of span carbon dioxide or oxygen
concentrations are required. The 90 percent
of span gas mixture is to be used to set and
check the analyzer span and is referred to
aj span gas. For oxygen analyzers, If the
span Is higher than 21 percent O,, ambient
air may be used In place of the 90 percent of
span calibration gas mixture. Triplicate
analyses of the gas mixture (except ambient
air) shall be performed within two weeks
prior to use using Reference Method 3 of
this part.
2.3 Zero Oas. A gas containing less than 100
ppm of carbon dioxide or oxygen.
2.4 Data Recorder. Analog chart recorder
or other suitable device with Input voltage
range compatible with analyzer system out-
put. The resolution of the recorder's data
output shall .be sufficient to allow completion
of the test procedures within this specifica-
tion.
3. Definitions.
3.1 Continuous Monitoring System. The
total equipment required for the determina-
tion of carbon dioxide or oxygen In a given
source effluent. The system consists of three
major subsystems:
3.1.1 Sampling Interface.. That portion of
the continuous monitoring system that per-
forms one or more of the • following opera-
tions: delineation, acquisition, transporta-
tion,, and conditioning of a sample of the
source effluent or protection of the analyzer
from the hostile aspects of the sample or
source environment.
3.1.2 Analyzer. That portion of the con-
tinuous monitoring system which senses the
pollutant gas and generates a signal output
that U a function of the pollutant concen-
tration.
3.1.3 Data Recorder. That portion of the
continuous monitoring system that provides
a permanent record of the output signal in
terms of concentration units.
3.2 Span. The value of oxygen or carbon di-
oxide concentration at which the continuous
monitoring system Is set that produces the
maximum data display output. For the pur-
poses of this method, the span shall be set
no leas than 1.5 to 2.5 times the normal car-.
bon dioxide or normal oxygen concentration
In the stack gas of the affected facility.
3.3 Midrange. The value of oxygen or car-
bon, dioxide concentration that ds representa-
tive of the normal conditions in the stack
gas of. the effected facility at typical operat-
ing rates.
3.4 Zero Drill, i^ „ „„ m tne contin-
uous monitoring system output over a stated
period of time of normal continuous opera-
tion when the carbon dioxide or oxygen con-
centration at the time for the measurements
Is zero.
3.5 Calibration Drift. The change In the
continuous monitoring system output over a
stated time period of normal continuous op-
eration when the. carbon dioxide or oxygen
continuous - monitoring system Is measuring
the concentration of span gas. .
3.6 Operational Test Period. A minimum
period of time over which the continuous
monitoring system Is expected to" operate
within Certain performance specifications
without unscr-»duled maintenance, repair, or
adjustment.
3.7 Response mnv. iu« nine i« nl from
a step change in concentration ot the Input
to the continuous monitoring system to the
time at which 95 percent of the correspond-
ing final value Is displayed on the continuous
monitoring system date recorder.
4. Installation Specification.
Oxygen or carbon dioxide continuous mon-
itoring systems'1 shall-be Installed at a loca-
tion where measurements are directly repre-
sentative of the total effluent from the
• affected facility or representative of the same
effluent sampled by a SO. or NO, continuous
monitoring system. This" requirement shall
be complied with by use of applicable re-
quirements In Performance Specification 2 of
'this appendix as follows:
4.1 Installation of Oxygen or Carbon Di-
oxide Continuous Monitoring Systems Not
Used to Convert Pollutant Data. A sampling
location shall be selected In accordance with
the procedures under • paragraphs 4.2.1 or
. 4.2.2, or Performance Specification 2 of this
appendix. •
4.2 Installation of Oxygen or Carbon Di-
oxide Continuous Monitoring Systems Used
to Convert Pollutant Continuous Monitoring
System- Date to Units of Applicable Stand-
ards. The diluent continuous monitoring sys-
tem (oxygen or carbon dioxide) shall be In-
stalled at a sampling location where measure-
ments that can be made are representative of
the effluent gases sampled by the pollutant
continuous monitoring system(s). Conform-
ance with this requirement may be accom-
plished In any- of the following ways:
4.2.1 The sampling location for the diluent
system shalfbe near the sampling location for
the pollutant continuous monitoring system
such that the same approximate polnt(s)
(extractive systems) or path (in-sltu sys-
tems) In the cross section Is sampled or
viewed.
4.2.2 The diluent and pollutant continuous
monitoring systems may be Installed at dif-
ferent locations if the effluent gases at both
sampling locations are nonstratlfied as deter-
mined under paragraphs 4.1 or 4.3, Perform-
ance Specification 2 of this appendix and
there Is no in-leakage occurring between the
two sampling locations. If the effluent gases
are stratified at either location, the proce-
dures under paragraph 4.2.2, Performance
Specification 2 of this appendix shall be used
for installing continuous monitoring systems
at that location.
5. Continuous Monitoring System Perform-
ance Specifications.
The continuous monitoring system shall
meet the performance specifications In Table
3-1 to be considered acceptable under this
method.
6. Performance Specification Test Proce-
dures.
The following test procedures shall be used
to determine conformance with the require-
ments of paragraph 4. Due to the wide varia-
tion existing In analyzer designs and princi-
ples of operation, these- procedures are not
applicable to all analyzers. Where this occurs,
alternative procedures, subject to the ap-
proval of the Administrator, may be em-
ployed. Any such alternative procedures must
fulfill the same purposes (verify response,
drift, and accuracy) as the following proce-
dures, and must clearly demonstrate con-
formance with specifications In Table 3-1.
"' 6.1 Calibration Check, Establish a cali-
bration curve for the continuous moni-
toring system using zero, midrange, and
span concentration gas mixtures. Verify
that the resultant curve of analyzer read-
ing compared with the calibration gas
value is consistent with the expected re-
sponse curve as described by the analyzer
manufacturer. If the expected response
curve is not produced, additional cali-
bration gas measurements shall be made,
or additional steps undertaken to verify
Ill-Appendix B-9
-------
the accuracy of the response curve of the
analyzer.
6.2 Field Test for Zero Drift and Cali-
bration Drift. Install and operate the
continuous monitoring system in accord-
ance with the manufacturer's written in-
structions and drawings as follows:
TABLE 3-1.—Performance specifications
Parameter
Specification
1. Zero drift (2 h) i <0.4 pet Oj or CO).
2. Zero drift (24 h)'
-------
>ata
-------
Cstt of Test
Span Gas Concentration _ ppm
Analyzer Span Setting _ ppm
T; _ .^seconds
Upscale . 2. _ seconds
3. _ seconds
Average upscale response _ seconds
1 , _ seconds
Downs cale 2. _ seconds
3. , _ seconds
Average downscale response _ seconds
System average response time (slower time) = _ seconds
from slower _ average upscale minus average dcwnscale
system average response ~ slower time
Figure 3-3. Response
(4a
Ill-Appendix B-12
-------
C— DrWunMATion or EMISSION BATI
CHANQI
• *
1.1 The following method shall be used to determine
whether » physical or operational change to an existing
facility raenlted In an Incrane In the emission r»te to the
atmosphere. The method used la the Student's < test.
commonly used to make Inferences from small samples.
f.Dtta.
J.1 E»eh emission test shall consist of o nras (usually
three) wbteh produce • emission rates. Thus two sets of
emission rates are generated, one before and one after the
change. the two sets being of equal size.
2.2When using manual emission tacts, except as pro-
vided to I «MCW of this part, the reference methods of
Appendix A to this part shall be used In accordance with
the procedures specified In the applicable snbpart both
before and after the change to obtain the data.
24 Wbenusingeontinuonsmonitors.thefaclUtyshallbe
operated as If » manual emission test were being per-
lormed. Vattd data using the averaging time which would
be required If a manual emission test were being eon-
ducted sban be used.
8. Procedure.
fcl Subscripts a and b denote prechange and post-
""S^Calculate the arithmetic mean emtoslon rate, E, for
•aah set of data using Equation L
••+*• «„
S.4 Calculate the pooled estimate, 8* using Equa-
tion 8.
.._
K-EmlssIoh rate for the I th ruu;
•-number of runs
U CeJcolate the sample variance, &. tor each set of
data nata* Equation 2.
f-p*
J
i Calculate the test statistic, I, using Equation 4.
•J3._Tf_
< = -
4. Rtrutti.
4.1 If £»> E. and t>f, where C Is the critical value of
I obtained from Table 1, then with 95% confidence the
difference between Et and E. Is significant, and an In.
crease In emission rate to the atmosphere has occurred.
\ TABLE 1
f(W
percent
eonft-
tenet
Degree of freedom (n.-fu »-2): laxl)
2 1920
3.. „ - 2.353
4. „ .;. ., ^ 1182
8 2.0U
*'. IIIIIIIIIIIIIIIIIIIIIIIIIIIIIII L 943
7 — 1.895
Slllllllirill"""!. III L 8BO
For greater than 8 degrees of freedom, see any standard
statistical handbook or text.
6.1 Assume the two performance tests produced the
following set of data:
Testa:
Bun 1. 100.
Bun2. 96..
Bun*. 110.
Testb
— 115
120
: US
5.3 Using Equation 2—
(100-102)'+ (95-102)'+ (110-102)*
= 3-1
=58.5
S»J
(115-120)*+ (120- 120)»+ (125-120)'
«= 3-1
=25
S.4 Using Equation 3—
ft _["(3-l) (58.5) + (3-1) (25)-|«/» fl
S'=l - 3+3^2 - J ~6'46
5.5 Using jEqnatton 4—
120-102
«=-
=3.412
(3)
(.XTJslng Equation 1—
5.6 Since (m+m-2) -4, f-2.132 (from Table 1). Thus
since Of the difference In the values of E. and £» Is
significant, and there has been ah Increase in emission
rate to the atmosphere.
0. OmHauow Monttorine Data.
8.1 Hourly averages from conUnooos moMtortrn do-
Tjoee. where available, should be used as data {
the above procedure tallowed;
(Sec. 114. Clean Air Act
VJS.C. 7414)). °883
U kmended (42
Ill-Appendix B-13
-------
APPENDIX D—REQUIRED EMISSION INVENTORY
INFORMATION
(a) Completed NEDS point source form(s)
for the entire plant containing the desig-
nated facility. Including Information on the
applicable criteria pollutants. If data con-
cerning the plant 'are already In NEDS, only
that Information must be submitted which
Is necessary to update the existing NEDS
record for that plant. Plant and point identi-
fication codes for NEDS records shall cor-
respond to those previously assigned In
NEDS; for plants not In NEDS, these codes
shall be obtained from the appropriate
Regional Office.
(b) Accompanying the basic NEDS infor
matlon shall be the following information
on each designated facility:
(1) The state and county Identification
codes, as well as the complete plant and
point Identification codes of the designated
facility in NEDS. (The codes are needed to
match these data with the NEDS date.)
(2) A description of the designated facility
including, where appropriate:
(1) Process name.
(il) Description and quantity of each
product (maximum per hour and average per
year).
(ill) Description and quantity of raw ma-
terials bandied for each product (maximum
per hour and average per year).
(iv) Types of fuels burned, quantities and
characteristics (maximum and average
quantities per hour, average per year).
(v) Description and quantity of solid
wastes generated (per year) and method of
disposal.
• (3) A description of the air pollution con-
trol equipment In use or proposed to control
the designated pollutant. Including:
(1) Verbal description of equipment.
(11) Optimum control efficiency, In percent.
This shall be a combined efficiency when
more than one device operate in series. The
method of control efficiency determination!
shall be Indicated (e.g., design efficiency,'
measured efficiency, estimated efficiency).
(Ill) Annual average control efficiency. In
percent, taking Into account control equip-
ment down time. This shall be a combined
efficiency when more than one device operate
In series.
(4) An estimate of the designated pollu-
tant emissions from the designated facility
(maximum per hour and average per. year).
The method of emission determination ihall
also be specified* (e.g., stack test, material
balance. emlsHlon factor).
(Sec. 114. Clean Air Act U amended (43
U.S.C. 7414)1.6883
Til-Appendix B-14
-------
ADDENDA
-------
TABLE OF CONTENTS
IV. PROPOSED AMENDMENTS
Subpart Page
A General Provisions A-l
Definitions, see also Subpart JJ
Notification and recordkeeping, see Subpart VV
Compliance with standards and maintenance requirements,
see Subpart VV
Monitoring requirements, see Performance Specification
5 and Reference Methods 6 A/B
Priority list
B Adoption and Submittal of State Plans for Designated B-l
Facilities
D,Da Fossil Fuel-Fired Industrial Steam Generators D-l
Advance notice of proposed rulemaking
Fossil Fuel-Fired Steam Generators
Test methods, see Reference Method 6 A/B
Emission monitoring, see Reference Method 6 A/B
E Incinerators E-l
Review of standards
F Portland Cement Plants F-l
Review of standards
G Nitric Acid Plants
Review of standards G-l
H Sulfuric Acid Plants
Review of standards H-l
J Petroleum Refinery
Review of standards J-l
L Secondary Lead Smelters
Review of standards L-l
M Secondary Brass and Bronze Ingot Production
Review of standards M-l
N Iron and Steel Plants, Basic Oxygen Furnace
Review of standards N-l
0 Sewage Treatment Plants
Review of standards 0-1
T,U,V, Phosphate Fertilizer Plants T,U,V
W,X Review of standards W,X-1
Add. 1-1
-------
TABLE OF CONTENTS (continued)
Subpart Page
Z Ferroalloy Production Facilities Z-l
Review of standards
AA Electric Arc Furnaces (Steel Industry)
Review of standards AA-1
"BB Kraft Pulp Mills
Test methods, see Reference Method 16 A BB-1
EE Surface Coating of Metal Furniture
Proposed standards EE-1
FF Stationary Internal Combustion Engines
Proposed standards FF-1
JJ Organic Solvent Cleaners
Proposed standards JJ-1
MM Automobile and Light Duty Truck Surface Coating Operations
Notice of intent to review MM-1
00 Perchloroethylene Dry Cleaners
Proposed standards 00-1
QQ Graphic Arts Industry: Publication Rotogravure Printing
Proposed standards QQ-1
RR Pressure Sensitive Tape and Label Surface Coating Operations
Proposed standards RR-1
SS Industrial Surface Coating: Appliances
Proposed standards SS-1
TT Metal Coil Surface Coating
Proposed standards TT-1
UU Asphalt Processing and Asphalt Roofing Manufacture
Proposed standards UU-1
VV VOC Fugitive Emission Sources; Synthetic Organic Chemicals
Manufacturing Industry
Proposed standards VV-1
WW Beverage Can Surface Coating Industry
Proposed standards WW-1
XX Bulk Gasoline Terminals
Proposed standards XX-1
Add. 1-2
-------
TABLE OF CONTENTS (continued)
Subpart
APPENDIX A - REFERENCE METHODS
2A Direct Measure of Gas Volume through Pipes and Small
Ducts, see Subpart XX
2B Determination of Exhaust Gas Volume Flow Rate from
Gasoline Vapor Incinerators, see Subpart XX
6A Determination of Sulfur Dioxide, Moisture, and Carbon
Dioxide Emissions from Fossil Fuel Combustion Sources
6B Determination of Sulfur Dioxide and Carbon Dioxide
Daily Average Emissions from Fossil Fuel Combustion
Sources
16A Determination of Total Reduced Sulfur Emissions from
Stationary Sources
21 Determination of Volatile Organic Compound Leaks, see
Subpart VV
22 Visual Determination of Fugitive Emissions from Mate-
rial Processing Sources, see Subpart UU
23 Determination of Halogenated Organics from Stationary
Sources, see Subpart JJ
25A Determination of Total Gaseous Organic Concentration
Using A Flame lonization Analyzer, see Subpart XX
25B Determination of Total Gaseous Organic Concentration
Using A Nondispersive Infrared Analyzer, see Subpart XX
26 Determination of Particulate Emissions from the Asphalt
Processing and Asphalt Roofing Industry, see Subpart UU
27 Determination of Vapor Tightness of Gasoline Delivery
Tank Using Pressure - Vacuum Test, see Subpart XX
29 Determination of Volatile Matter Content and Density of
Printing Inks and Related Coatings, see Subpart QQ
Appendix A-4
Appendix A-7
Appendix A-10
APPENDIX B - PERFORMANCE SPECIFICATIONS
1 Specifications and Test Procedures for Opacity Contin-
uous Monitoring Systems in Stationary Sources
2 Specifications and Test Procedures for S02 and NO
Continuous Monitoring Systems in Stationary Sources
Add. 1-3
.Appendix B-3
Appendix B-12
-------
TABLE OF CONTENTS
Subpart Page
APPENDIX B - PERFORMANCE SPECIFICATIONS
3 Specifications and Test Procedures for C02 and 02
Continuous Monitors in Stationary Sources Appendix B-24
4 Specifications and Test Procedures for Carbon Monoxide
Continuous Monitoring Systems in Stationary Sources Appendix B-34
5 Specifications and Test Procedures for TRS Continuous
Emission Monitoring Systems in Stationary Sources Appendix B-43
APPENDIX E - SYNTHETIC ORGANIC CHEMICALS MANUFACTURING INDUSTRY,
see Subpart VV
Add. 1-4
-------
TABLE OF CONTENTS
V. FULL TEXT OF REVISIONS
Ref. Page
36 FR 5931, 3/31/71 - List of Categories of Stationary Sources.
36 FR 15704, 8/17/71 - Proposed Standards for Five Categories:
Fossil Fuel-Fired Steam Generators, Portland Cement
Plants, Nitric Acid Plants, and Sulfuric Acid Plants.
1. 36 FR 24876, 12/23/71 - Standards of Performance Promulgated for
Fossil Fuel-Fired Steam Generators, Incinerators, Port-
land Cement Plants, Nitric Acid Plants, and Sulfuric
Acid Plants. 1
1A. 37 FR 5767, 3/21/72 - Supplemental Statement in Connection with
Final Promulgation. 21
2. 37 FR 14877, 7/26/72 - Standard for Sulfur Dioxide; Correction. 25
37 FR 17214, 8/25/72 - Proposed Standards for Emissions During
Startup, Shutdown, and Malfunction.
3. 38 FR 13562, 5/23/73 - Amendment to Standards for Opacity and
Corrections to Certain Test Methods. 26
38 FR 15406, 6/11/73 - Proposed Standards of Performance for
Asphalt Concrete Plants, Petroleum Refineries, Storage
Vessels for Petroleum Liquids, Secondary Lead Smelters,
Brass and Bronze Ingot Production Plants, Iron and Steel
Plants, and Sewage Treatment Plants.
4. 38 FR 28564, 10/15/73 - Standards of Performance Promulgated for
Emissions During Startup, Shutdown, & Malfunction. 26
4A. 38 FR 10820, 5/2/73 - Proposed Standards of Performance for
Emissions During Startup, Shutdown, & Malfunction. 28
5. 39 FR 9308, 3/8/74 - Standards of Performance Promulgated for
Asphalt Concrete Plants, Petroleum Refineries, Storage
Vessels for Petroleum Liquids, Secondary Lead Smelters,
Brass and Bronze Ingot Production Plants, Iron and Steel
Plants, and Sewage Treatment Plants; and Miscellaneous
Amendments. 30
Add. 2-1
-------
6. 39^ FR 13776, 4/17/74 - Corrections to March 8, 1974 Federal
Register. 45
7. 39 FR 15396, 5/3/74 - Corrections to March 8, 1974 and April
17, 1974 Federal Register. 46
8. 39 FR 20790, 6/14/74 - Standards of Performance, Miscellaneous
Amendments. 46
39 FR 32852, 9/11/74 - Proposed Standards of Performance -
Emission Monitoring Requirements and Performance Test-
ing Methods.
39 FR 36102, 10/7/74 - Proposed Standards of Performance for
State Plans for the Control of Existing Facilities.
39 FR 36946, 10/15/74 - Proposed Standards of Performance for
Modification, Notification, and Reconstruction.
39 FR 37040, 10/16/74 - Proposed Standards of Performance for
Primary Copper, Zinc, and Lead Smelters.
39 FR 37470, 10/21/74 - Proposed Standards of Performance for
Ferroalloy Production Facilities.
39 FR 37466, 10/21/74 - Proposed Standards of Performance for
Steel Plants: Electric Arc Furnaces.
39 FR 37602, 10/22/74 - Proposed Standards of Performance -
Five Categories of Sources in the Phosphate Fertilizer
Industry.
39 FR 37730, 10/23/74 - Proposed Standards of Performance for
Primary Aluminum Reduction Plants.
39 FR 37922, 10/24/74 - Proposed Standards of Performance for
Coal Preparation Plants.
9. 39 FR 37987, 10/25/74 - Region V Office: New Address. 51
10. 39 FR 39872, 11/12/74 - Opacity Provisions for New Stationary
Sources Promulgated and Appendix A, Method 9 - Visual
Determination of the Opacity of Emissions from Station-
ary Sources. 51
39 FR 39909, 11/12/74 - Response to Remand, Portland Cement
Association v. Ruckelshaus, Reevaluation of Standards.
Add. 2-2
-------
40 FR 831, 1/3/75 - Reevaluation of Opacity Standards of Perform-
ance for New Sources - Asphalt Concrete Plants.
11. 40 FR 2803, 1/16/75 - Amended Standard for Coal Refuse (promul-
gated December 23, 1971). 57
40 FR 17778, 4/22/75 - Standards of Performance, Proposed Opa-
city Provisions, Request for Public Comment.
12. 40 FR 18169, 4/25/75 - Delegation of Authority to State of
Washington. 58
13. 40 FR 26677, 6/25/75 - Delegation of Authority to State of Idaho. 58
14. 40 FR 33152, 8/6/75 - Standards of Performance Promulgated for
Five'Categories of Sources in the Phosphate Fertilizer
Industry. 59
40 FR 39927, 8/29/75 - Standards of Performance for Sulfuric
Acid Plants - EPA Response to Remand.
40 FR 41834, 9/9/75 - Opacity Reevaluation - Asphalt Concrete,
Response to Public Comments.
40 FR 42028, 9/10/75 - Proposed Opacity Standards for Fossil
Fuel-Fired Steam Generators.
40 FR 42045, 9/10/75 - Standards of Performance for Fossil Fuel-
Fired Steam Generators - EPA Response to Remand.
15. 40 FR 42194, 9/11/75 - Delegation of Authority to State of
California. 74
16. 40 FR 43850, 9/23/75 - Standards of Performance Promulgated for
Electric Arc Furnaces in the Steel Industry. 75
17. 40 FR 45170, 10/1/75 - Delegation of Authority to State of
California. 80
18. 40 FR 46250, 10/6/75 - Standards of Performance Promulgated
for Emission Monitoring Requirements and Revisions
to Performance Testing Methods. 81
19. 40 FR 48347, 10/15/75 - Delegation of Authority to State of
New York. 102
20. 40 FR 50718, 10/31/75 - Delegation of Authority to State of
Colorado. 102
21. 40 FR 53340, 11/17/75 - Standards of Performance, Promulgation
of State Plans for the control of Certain Pollutants
from Existing Facilities (Subpart B and Appendix D). 103
Add. 2-3
-------
40 FR 53420, 11/18/75 - Reevaluation of Opacity Standards for
Secondary Brass and Bronze Plants and Secondary Lead
Smelters.
22. 40 FR 58416, 12/16/75 - Standards of Performance, Promulgation
of Modification, Notification and Reconstruction Pro-
visions. 113
23. 40 FR 59204, 12/22/75 - Corrections to October 6, 1975, Federal
Register. 118
24. 40 FR 59729, 12/30/75 - Delegation of Authority to State of
Maine. 118
25. 41 FR 1913, 1/13/76 - Delegation of Authority to State of
Michigan. ° 119
26. 41 FR 2231, 1/15/76 - Standards of Performance Promulgated for
Coal Preparation Plants. 119
26. 41 FR 2332, 1/15/76 - Standards of Performance Promulgated for
Primary Copper, Zinc and Lead Smelters. 123
27. 41 FR 3825, 1/26/76 - Standards of Performance Promulgated for
Primary Aluminum Reduction Plants. 133
28. 41 FR 4263,1/29/76 - Delegation of Authority to Washington Local
Authorities. 138
41 FR 7447, 2/18/76 - Reevaluation of Opacity Standards for
Municipal Sewage Sludge Incinerators.
29. 41 FR 7749, 2/20/76 - Delegation of Authority to State of
Oregon. 138
30. 41 FR 8346, 2/26/76 - Correction to the Primary Copper, Zinc,
and Lead Smelter Standards Promulgated on 1/15/76. 139
31. 41 FR 11820, 3/22/76 - Delegation of Authority to State of
Connecticut. 139
32. 41 FR 17549, 4/27/76 - Delegation of Authority to State of
South Dakota. 139
33. 41 FR 18498, 5/4/76 - Standards of Performance Promulgated for
Ferroalloy Production Facilities. 140
41 FR 19374, 5/12/76 - Revised Public Comment Summary for Mod-
ification, Notification, and Reconstruction.
41 FR 19584, 5/12/76 - Phosphate Fertilizer Plants, Draft Guide-
lines Document - Notice of Availability.
Add. 2-4
-------
34. 41 FR 19633, 5/13/76 - Delegation of Authority to Commonwealth
of Massachusetts and Delegation of Authority to State
of New Hampshire. 145
35. 41 FR 20659, 5/20/76 - Correction to Ferroalloy Production
Facilities Standards Promulgated on May 4, 1976. 146
36. 41 FR 21450, 5/26/76 - Delegation of Authority to State of
California. 146
41 FR 23059, 6/8/76 - Proposed Amendments to Reference Methods
1-8.
37. 41 FR 24124, 6/15/76 - Delegation of Authority to State of Utah. 146
38. 41 FR 24885, 6/21/76 - Delegation of Authority to State of
Georgia. 147
39. 41 FR 27967, 7/8/76 - Delegation of Authority to State of
California. 147
40. 41 FR 33264, 8/9/76 - Delegation of Authority to State of
California. 148
41. 41 FR 34628, 8/16/76 - Delegation of Authority to Virgin
Islands. 148
42. 41 FR 35185, 8/20/76 - Revision to Emission Monitoring
Requirements. 149
41 FR 36600, 8/30/76 - Proposed Revisions to Standards of
Performance for Petroleum Refinery Fluid Catalytic
Cracking Unit Catalyst Regenerators.
43. 41 FR 36918, 9/1/76 - Standards of Performance - Avail-
ability of Information. 149
44. 41 FR 40107, 9/17/76 - Delegation of Authority to
State of California. 149
45. 41 FR 40467, 9/20/76 - Delegation of Authority to State of
Alabama. 150
41 FR 42012, 9/24/76 - Proposed Standards of Performance for
Kraft Pulp Mills.
46. 41 FR 43148, 9/30/76 - Delegation of Authority to the State
State of Indiana. 150
41 FR 43866, 10/4/76 - Proposed Revisions to Standards of
Performance for Petroleum Refinery Sulfur Recovery
Plants.
Add. 2-5
-------
47. 41 FR 44859, 10/13/76 - Delegation of Authority to State of
North Dakota. 150
41 FR 46618, 10/22/76 - Advanced Notice of Proposed Rule-
making of Air Emission Regulations - Synthetic
Organic Chemical Manufacturing Industry.
41 FR 47495, 10/29/76 - Proposed Standards of Performance for
Kraft Pulp Mills; Correction.
48. 41 FR 48342, 11/3/76 - Delegation of Authority to State of
California. 151
41 FR 48706, 11/4/76 - Proposed Revisions to Emission Guide-
lines for the Control of Sulfuric Acid Mist from
Existing Sulfuric Acid Production Units.
49. 41 FR 51397, 11/22/76 - Amendments to Subpart D Promulgated. 151
41 FR 51621, 11/23/76 - Proposed Standards of Performance
for Kraft Pulp Mills - Extension of Comment Period.
41 FR 52079, 11/26/76 - Proposed Revision to Emission Guide-
lines for the Control of Sulfuric Acid Mist from
Existing Sulfuric Acid Production Units; Correction.
50. 41 FR 52299, 11/29/76 - Amendments to Reference Methods
13A and 13B Promulgated. 154
51. 41 FR 53017, 12/3/76 - Delegation of Authority to Pima
County Health Department; Arizona. 155
52. 41 FR 54757, 12/15/76 - Delegation of Authority to State of
California. 155
53. 41 FR 55531, 12/21/76 - Delegation of Authority to the State
of Ohio. 156
41 FR 55792, 12/22/76 - Proposed Revisions to Standards of
Performance for Lignite-Fired Steam Generators.
54. 41 FR 56805, 12/30/76 - Delegation of Authority to the States
of North Carolina, Nebraska, and Iowa. 156
55. 42 FR 1214, 1/6/77 - Delegation of Authority to State of
Vermont. 157
42 FR 2841, 1/13/77 - Proposed Standards of Performance for
Grain Elevators.
Add. 2-6
-------
56. 42 FR 4124, 1/24/77 - Delegation of Authority to the State
of South Carolina. 158
42 FR 4863, 1/26/77 - Proposed Revisions to Standards of
Performance for Sewage Sludge Incinerators.
42 FR 4883, 1/26/77 - Receipt of Application and Approval
of Alternative Test Method. 158
42 FR 5121, 1/27/77 - Notice of Study to Review Standards
for Fossil Fuel-Fired Steam Generators; SC^
Emissions.
57. 42 FR 5936, 1/31/77 - Revisions to Emission Monitoring
Requirements and to Reference Methods Promulgated. 159
58. 42 FR 6812, 2/4/77 - Delegation of Authority to City of
Philadelphia. 161
42 FR 10019, 2/18/77 - Proposed Standards for Sewage
Treatment Plants; Correction.
42 FR 12130, 3/2/77 - Proposed Revision to Standards of Per-
formance for Iron & Steel Plants; Basic Oxygen
Process Furnaces.
42 FR 13566, 3/11/77 - Proposed Standards of Performance for
Grain Elevators; Extension of Comment Period.
59. 42 FR 16777, 3/30/77 - Correction of Region V Address and
Delegation of Authority to the State of Wisconsin. 161
42 FR 18884, 4/11/77 - Notice of Public Hearing on Coal-
Fired Steam Generators S02 Emissions.
42 FR 22506, 5/3/77 - Proposed Standards of Performance for
Lime Manufacturing Plants.
60. 42 FR 26205, 5/23/77 - Revision of Compliance with
Standards and Maintenance Requirements. 162
42 FR 26222, 5/23/77 - Proposed Revision of Reference
Method 11.
42 FR 32264, 6/24/77 - Suspension of Proposed Standards of
Performance for Grain Elevators.
61. 42 FR 32426, 6/24/77 - Revisions to Standards of Performance
for Petroleum Refinery Fluid Catalytic Cracking Unit
Catalyst Regenerators Promulgated. 162
Add. 2-7
-------
62. 42 FR 37000, 7/19/77 - Revision and Reorganization of the
Units and Abbreviations. 164
42 FR 37213, 7/20/77 - Notice of Intent to Develop Standards
of Performance for Glass Melting Furnaces.
63. 42 FR 37386, 7/21/77 - Delegation of Authority to the State
of New Jersey. 165
64. 42 FR 37936, 7/25/77 - Applicability Dates Incorporated
into Existing Regulations. 165
65. 42 FR 38178, 7/27/77 - Standards of Performance for
Petroleum Refinery Fluid Catalytic Cracking Unit
Catalyst Regenerators and Units and Measures;
Corrections. 168
66. 42 FR 39389, 8/4/77 - Standards of Performance for Petroleum
Refinery Fluid Catalytic Cracking Unit Catalyst
Regenerators, Correction. 168
67. 42 FR 41122, 8/15/77 - Amendments to Subpart D; Correction. 168
68. 42 FR 41424, 8/17/77 - Authority Citations; Revision 169
69. 42 FR 41754, 8/18/77 - Revision to Reference Methods 1-8 170
Promulgated.
70. 42 FR 44544, 9/6/77 - Delegation of Authority to the State
of Montana. 206
71. 42 FR 44812, 9/7/77 - Standards of Performance, Applicability
Dates; Correction. 206
42 FR 45705, 9/12/77 - Notice of Delegation of Authority to
the State of Indiana.
72. 42 FR 46304, 9/15/77 - Delegation of Authority to the State
of Wyoming. 207
42 FR 53782, 10/3/77 - Proposed Standards of Performance
for Stationary Gas Turbines.
73. 42 FR 55796, 10/18/77 - Emission Guidelines for Sulfuric
Acid Mist Promulgated. 208
74. 42 FR 57125, 11/1/77 - Amendments to General Provisions
and Copper Smelter Standards Promulgated. 209
Add. 2-8
-------
75. 42 FR 58520, 11/10/77 - Amendment to Sewage Sludge Incin-
erators Promulgated. 211
76. 42 FR 61537, 12/5/77 - Opacity Provisions for Fossil-Fuel-
Fired Steam Generators Promulgated. 212
42 FR 61541, 12/5/77 - Opacity Standards for Fossil-Fuel -
Fired Steam Generators: Final EPA Response to
Remand.
77. 42 FR 62137, 12/9/77 - Delegation of Authority to the
Commonwealth of Puerto Rico. 214
42 FR 62164, 12/9/77 - Proposed Standards for Station-
ary Gas Turbines; Extension of Comment Period.
78. 43 FR 9, 1/3/78 - Delegation of Authority to the State
of Minnesota. 214
79. 43 FR 1494, 1/10/78 - Revision of Reference Method II
Promulgated. 215
80. 43 FR 3360, 1/25/78 - Delegation of Authority to the
Commonwealth of Kentucky. 219
81. 43 FR 6770, 2/16/78 - Delegation of Authority to the
State of Delaware. 220
82. 43 FR 7568, 2/23/78 - Standards of Performance Pro-
mulgated for Kraft Pulp Mills. 221
83. 43 FR 8800, 3/3/78 - Revision of Authority Citations. 249
84. 43 FR 9276, 3/7/78 - Standards of Performance Promul-
gated for Lignite-Fired Steam Generators. 250
85. 43 FR 9452, 3/7/78 - Standards of Performance Promul-
gated for Lime Manufacturing Plants. 253
86. 43 FR 10866, 3/15/78 - Standards of Performance Pro-
mulgated for Petroleum Refinery Claus Sulfur
Recovery Plants. 255
87. 43 FR 11984, 3/23/78 - Corrections and Amendments to
Reference Methods 1-8. 262
43 FR 14602, 4/6/78 - Notice of Regulatory Agenda.
Add. 2-9
-------
88. 43 FR 15600, 4/13/78 - Standards of Performance Promul-
gated for Basic Oxygen Process Furnaces: Opacity
Standard. 265
89. 43 FR 20986, 5/16/78 - Delegation of Authority to State/
Local Air Pollution Control Agencies in Arizona,
California, and Nevada. 268
43 FR 21616, 5/18/78 - Proposed Standards of Performance
for Storage Vessels for Petroleum Liquids.
43 FR 22221, 5/24/78 - Correction to Proposed Standards
of Performance for Storage Vessels for Petroleum
Liquids.
90. 43 FR 34340, 8/3/78 - Standards of Performance Promulgated
for Grain Elevators. 269
43 FR 34349, 8/3/78 - Reinstatement of Proposed Standards
for Grain Elevators.
91. 43 FR 34784, 8/7/78 - Amendments to Standards of Perform-
ance for Kraft Pulp Mills and Reference Method 16. 277
43 FR 34892, 8/7/78 - Proposed Regulatory Revisions Air
Quality Surveillance and Data Reporting.
43 FR 38872, 8/31/78 - Proposed Priority List for Standards
of Performance for New Stationary Sources.
43 FR 42154, 9/19/78 - Proposed Standards of Performance
for Electric Utility Steam Generating Units and
Announcement of Public Hearing on Proposed Stan-
dards.
43 FR 42186, 9/19/78 - Proposed Standards of Performance
for Primary Aluminum Industry.
92. 43 FR 47692, 10/16/78 - Delegation of Authority to the
State of Rhode Island. 278
43 FR 54959, 11/24/78 - Public Hearing on Proposed Stan-
dards for Electric Utility Steam Generating Units.
43 FR 55258, 11/27/78 - Electric Utility Steam Generating
Units; Correction and Additional Information.
43 FR 57834, 12/8/78 - Electric Utility Steam Generating
Units; Additional Information.
Add. 2-10
-------
93. 44 FR 2578, 1/12/79 - Amendments to Appendix A - Reference
Method 16. 279
94. 44 FR 3491, 1/17/79 - Wood Residue-Fired Steam Generators;
Applicability Determination. 280
95. 44 FR 7714, 2/7/79 - Delegation of Authority to State of Texas. 282
96. 44 FR 13480, 3/12/79 - Petroleum Refineries - Clarifying
Amendment. 282
44 FR 15742, 3/15/79 - Review of Performance Standards for
Sulfuric Acid Plants.
44 FR 17120, 3/20/79 - Proposed Amendment to Petroleum Refinery
Claus Sulfur Recovery Plants.
44 FR 17460, 3/21/79 - Review of Standards for Iron & Steel
Plants Basic Oxygen Furnaces.
44 FR 21754, 4/11/79 - Primary Aluminum Plants; Draft Guideline
Document; Availability.
97. 44 FR 23221, 4/19/79 - Delegation of Authority to Washington
Local Agency 284
44 FR 29828, 5/22/79 - Kraft Pulp Mills; Final Guideline Doc-
ument; Availability.
44 FR 31596, 5/31/79 - Definition of "Commenced" for Standards
of Performance for New Stationary Sources.
98. 44 FR 33580, 6/11/79 - Standards of Performance Promulgated for
Electric Utility Steam Generating Units. 285
44 FR 34193, 6/14/79 - Air Pollution Prevention and Control;
Addition to the List of Categories of Stationary Sources.
44 FR 34840, 6/15/79 - Proposed Standards of Performance for
New Stationary Sources; Glass Manufacturing Plants.
44 FR 35265, 6/19/79 - Review of Performance Standards: Nitric
Acid Plants.
44 FR 35953, 6/19/79 - Review of Performance Standards: Sec-
ondary Brass and Bronze Ingot Production.
44 FR 37632, 6/28/79 - Fossil-Fuel-Fired Industrial Steam
Generators; Advanced Notice of Proposed Rulemaking.
44 FR 37960, 6/29/79 - Proposed Adjustment of Opacity Standard
for Fossil-Fuel-Fired Steam Generators.
Add. 2-11
-------
44 FR 43152, 7/23/79 - Proposed Standards of Performance for
Stationary Internal Combustion Engines.
44 FR 47778, 8/15/79 - Proposed Standards for Glass Manufacturing
Plants; Extension of Comment Period.
99. 44 FR 49222, 8/21/79 - Priority List and Additions to the List of
Categories of Stationary Sources Promulgated. 331
44 FR 49298, 8/22/79 - Kraft Pulp Mills; Final Guideline Document;
Correction.
100. 44 FR 51225, 8/31/79 - Standards of Performance for Asphalt Con-
crete Plants; Review of Standards. 335
44 FR 52324, 9/7/79 - New Source Performance Standards for Sul-
furic Acid Plants; Final EPA Remand Response.
101. 44 FR 52792, 9/10/79 - Standards of Performance for New Station-
ary Sources; Gas Turbines 338
44 FR 54072, 9/18/79 - Standards of Performance for Stationary
Internal Combustion Engines; Extension of Comment Period.
44 FR 54970, 9/21/79 - Proposed Standards of Performance for
Phosphate Rock Plants.
102. 44 FR 55173, 9/25/79 - Standards of Performance for New Station-
ary Sources; General Provisions; Definitions. 354
44 FR 57792, 10/5/79 - Proposed Standards of Performance for
Automobile and Light-Duty Truck Surface Coating Operations.
44 FR 58602, 10/10/79 - Proposed Standards for Continuous
Monitoring Performance Specifications.
44 FR 60759, 10/22/79 - Review of Standards of Performance for
Petroleum Refineries.
44 FR 60761, 10/22/79 - Review of Standards of Performance for
Portland Cement Plants.
103. 44 FR 61542, 10/25/79 - Amendment to Standards of Performance
for Petroleum Refinery Claus Sulfur Recovery Plants. 356
44 FR 62914, 11/1/79 - Proposed Standards of Performance for
Phosphate Rock Plants; Extension of Comment Period.
104. 44 FR 65069, 11/9/79 - Amendment to Regulations for Ambient
Air Quality Monitoring and Data Reporting. 358
Add. 2-12
-------
44 FR 67934, 11/27/79 - Review of Standards of Performance
for Sewage Treatment Plants.
44 FR 67938, 11/27/79 - Review of Standards of Performance
for Incinerators.
105. 44 FR 69298, 12/3/79 - Delegation of Authority to the State
of Maryland. 358
106. 44 FR 70465, 12/7/79 - Delegation of Authority to the State
of Delaware. 359
44 FR 57408, 12/20/79 - Standards of Performance for Contin-
uous Monitoring Performance Specifications; Extension of
Comment Period.
107. 44 FR 76786, 12/28/79 - Amendments to Standards of Performance
for Fossil-Fuel-Fired Steam Generators. 360
45 FR 2790, 1/14/80 - Proposed Standards of Performance for
Lead-Acid Battery Manufacture.
108. 45 FR 3034, 1/16/80 - Delegation of Authority to Commonwealth
of Pennsylvania. 360
45 FR 3333, 1/17/80 - Proposed Standards of Performance for
Phosphate Rock Plants; Extension of Comment Period.
109. 45 FR 5616, 1/23/80 - Modification, Notification, and Recon-
struction; Amendment and Correction. 361
45 FR 7758, 2/4/80 - Proposed Standards of Performance for
Ammonium Sulfate Manufacture.
110. 45 FR 8211, 2/6/80 - Standards of Performance for Electric
Utility Steam Generating Units; Decision in Response
to Petitions for Reconsideration. 363
45 FR 11444, 2/20/80 - Proposed Standards of Performance
for Continuous Monitoring Specifications.
45 FR 13991, 3/3/80 - Proposed Clarifying Amendment for
Standards of Performance for Petroleum Refineries.
45 FR 20155, 3/27/80 - Notice of Determination of Applicabil-
ity of New Source Performance Standards (NSPS) to Potomac
Electric Power Co. (PEDCo) Chalk Point Unit 4.
45 FR 21302, 4/1/80 - Proposed Adjustment of Opacity Standard
for Fossil-Fuel-Fired Steam Generator.
Add. 2-13
-------
111. 45 FR 23374, 4/4/80 - Standards of Performance for Petroleum
Liquid Storage Vessels. 386
45 FR 26294, 4/17/80 - Primary Aluminum Plants; Notice of
Availability of Final Guideline Document.
45 FR 26304, 4/17/80 - Review of Standards of Performance
for Secondary Lead Smelters.
45 FR 26910, 4/21/80 - Review of Standards of Performance
for Electric Arc Furnaces (Steel Industry)
112. 45 FR 36077, 5/29/80 - Adjustment of Opacity Standard for
Fossil Fuel Fired Steam Generator. 394
45 FR 39766, 6/11/80 - Proposed Standards of Performance
for Organic Solvent Cleaners.
113. 45 FR 41852, 6/20/80 - Revised Reference Methods 13A and 13B. 395
114. 45 FR 44202, 6/30/80 - Amendments to Standards of Performance
for Primary Aluminum Industry. 401
45 FR 44329, 7/1/80 - Proposed Alternate Method 1 to Reference
Method 9 of Appendix A - Determination of the Opacity of
Emissions from Stationary Sources Remotely by Lidar;
Addition of an Alternate Method.
45 FR 44970, 7/2/80 - Proposed California Plan to Control
Fluoride Emissions from Existing Phosphate Fertilizer Plants.
115. 45 FR 47146, 7/14/80 - Adjustment of Opacity Standard for Fossil-
Fuel-Fired Steam Generator. 417
45 FR 47726, 7/16/80 - Notice of Applicability Determination for
the Schiller Station Power Plant of New Hampshire.
116. 45 FR 50751, 7/31/80 - Delegation of Authority to Commonwealth
of Pennsylvania; Correction. 417
45 FR 54385, 8/15/80 - Proposed Alternate Method 1 to Reference
Method 9 of Appendix A; Extension of Comment Period.
45 FR 56169, 8/22/80 - Notice of Applicability Determination for
New Source Performance Standards.
45 FR 56176, 8/22/80 - NSPS Applicability to Hooker Chemical and
Plastics Corp., Niagara Falls, N.Y.
Add. 2-14
-------
45 FR 56373, 8/25/80 - Proposed Standards of Performance for
Organic Solvent Cleaners; Extension of Comment Period and
Corrections.
117. 45 FR 65956, 10/3/80 - Promulgation of Reference Methods 24 and
25 to Appendix A. 418
118. 45 FR 66742, 10/7/80 - Standards of Performance Promulgated for
Glass Manufacturing Plants. 436
45 FR 67146, 10/9/80 - Air Pollution; Kraft Pulp Mills; Total
Reduced Sulfur Emission Guideline; Correction.
45 FR 68616, 10/15/80 - Proposed Standards of Performance for
Sodium Carbonate Plants.
45 FR 71538, 10/18/80 - Proposed Standards of Performance for
Graphic Arts Industry; Publication Rotogravure Printing.
.'
45 FR 73521, 11/5/80 - Proposed Standards of Performance for
Organic Solvent Cleaners; Extension of Comment Period.
119. 45 FR 74846, 11/12/80 - Standards of Performance Promulgated for
Ammonium Sulfate Manufacture. 447
120. 45 FR 75662, 11/17/80 - Delegation of Authority to the State of
Iowa; Change of Address. 453
45 FR 76404, 11/18/80 - Proposed Standards of Performance for
Asphalt Processing and Asphalt Roofing Manufacture.
45 FR 76427, 11/18/80 - Proposed Amendment to Priority List.
45 FR 77075, 11/21/80 - Review of Standards of Performance for
Phosphate Fertilizer Plants.
45 FR 77122, 11/21/80 - Applicability Determination for New
Source Performance Standards; Vickers Petroleum Corp. et
al.
45 FR 78174, 11/25/80 - Proposed Alternate Method 1 to Reference
Method 9 of Appendix A - Notice of Hearing.
Proposed Standards of Performance for Perch!oroethylene Dry
Cleaners.
45 FR 78980, 11/26/80 - Proposed Standards of Performance for
Beverage Can Surface Coating Industry.
45 FR 79390, 11/28/80 - Proposed Standards of Performance for
Surface Coating of Metal Furniture.
Add. 2-15
-------
121. 45 FR 79452, 12/1/80 - Clarifying Amendment for Standards of
Performance for Petroleum Refineries. 453
45 FR 81653, 12/11/80 - Notice of Denial of Petition to Revise
Standards of Performance for Stationary Gas Turbines.
45 FR 83126, 12/17/80 - Proposed Standards of Performance for
Bulk Gasoline Terminals.
122. 45 FR 83228, 12/18/80 - Standards of Performance for Petroleum
. Liquid Storage Vessels; Correction. 455
123. 45 FR 85016, 12/24/80 - Standards of Performance for Revised
Reference Methods 13A and 13B; Corrections. 456
45 FR 85085, 12/24/80 - Proposed Standards of Performance for
Industrial Surface Coating: Appliances.
45 FR 85099, 12/24/80 - Proposed Amendment to Priority List.
124. 45 FR 85410, 12/24/80 - Standards of Performance Promulgated for
Automobile and Light-Duty Truck Surface Coating Operations. 457
45 FR 86278, 12/30/80 - Proposed Standards of Performance for
Pressure Sensitive Tape and Label Surface Coating Operations.
46 FR 1102, 1/5/81 - Proposed Standards of Performance for Metal
Coil Surface Coating.
46 FR 1135, 1/5/81 - Proposed Standards of Performance; VOC
Fugitive Emission Sources; Synthetic Organic Chemicals
Manufacturing Industry.
46 FR 1317, 1/6/81 - Corrections to Proposed Standards of
Performance for Graphic Arts Industry: Publication
Rotogravure Printing.
46 FR 8033, 1/26/81 - Review of Standards of Performance for
Ferroalloy Production Facilities.
46 FR 8352, 1/26/81 - Proposed Revisions to General Provisions
and Additions to Appendix A, and Reproposal of Revisions to
Appendix B.
46 FR 8587, 1/27/81 - Proposed Standards of Performance for Bulk
Gasoline Terminals; Extension of Public Hearing and End of
Comment Period.
Proposed Standards of Performance for Graphic Arts Industry:
Publication Rotogravure Printing; Clarification.
Add. 2-16
-------
46 FR 9130, 1/28/81 - Corrections to Proposed Standards of
Performance for Industrial Surface Coating; Appliances.
46 FR 9131, 1/28/81 - Correction to Proposed Amendment to Priority
List.
46 FR 10752, 2/4/81 - Corrections to Proposed Standards of
Performance for Bulk Gasoline Terminals.
46 FR 11490, 2/6/81 - Proposed Waiver from New Source Performance
Standard for Homer City Unit No. 3 Steam Electric Generating
Station Indiana County, Pennsylvania.
46 FR 11557, 2/9/81 - Proposed Standards of Performance for Surface
Coating of Metal Furniture; Extension of Comment Period.
46 FR 12023, 2/12/81 - Proposed Standards of Performance for Metal
Coil Surface Coating; Extension of Comment Period.
46 FR 12106, 2/12/81 - Notice of Availability of Control Techniques
Guideline Documents.
46 FR 14358, 2/27/81 - Proposed Standards of Performance for the
Beverage Can Surface Coating Industry; Reopening of Comment
Period.
46 FR 14905, 3/3/81 - Correction to Proposed Standards of
Performance for Bulk Gasoline Terminals.
46 FR 21628, 4/13/81 - Notice of Intent for Standards of Performance
for New Stationary Sources „
46 FR 21789, 4/14/81 - VOC Fugitive Emission Sources; Synthetic
Organic Chemical Manufacturing Industry; Extension of Comment
Period.
125. 46 FR 21769, 4/14/81 - Review of Standards of Performance for Coal
Preparation Plants. 466
46 FR 22005, 4/15/81 - Proposed Revision to Standards of Performance
for Stationary Gas Turbines.
46 FR 22768, 4/21/81 - Amendment to Proposed Standards of Performance
for Organic Solvent Cleaners.
46 FR 23984, 4/29/81 - Notice of Proposed Equivalency Determinations
for Petroleum Liquid Storage Vessels.
46 FR 26501, 5/13/81 - Proposed Revisions to Priority List of
Categories.
Add. 2-17
-------
126. 46 FR 27341, 5/19/81 - Delegation of Authority to the State of
Missouri. 467
46 FR 28180, 5/16/81 - Amendments and Clarification to Proposed
Standards of Performance for Asphalt Processing and Asphalt
Roofing Manufacture.
127. 46 FR 28402, 5/27/81 - Delegation of Authority to the State of
Delaware. 468
128. 46 FR 29262, 6/1/81 - Delegation of Authority to the State of
Tennessee. 469
46 FR 29955, 6/4/81 - Correction to Proposed Standards of
Performance for Industrial Surface Coating: Appliances.
46 FR 31904, 6/18/81 - Proposed Reference Method 16A - Determination
of Total Reduced Sulfur Emissions from Stationary Sources.
46 FR 37287, 7/20/81 - Proposed Revisions to General Provisions and
Continuous Monitoring Performance Specifications.
129. 46 FR 39422, 7/31/81 - Delegation of Authority to the State of
Nebraska and Change of Address. 470
46 FR 41817, 8/18/81 - Proposed Adjustment of Opacity Standard
for Fossil-Fuel-Fired Steam Generator.
46 FR 42878, 8/25/81 - Proposed Alternative Performance Test
Requirement for Primary Aluminum Plant.
46 FR 46813, 9/22/81 - Withdrawal of Proposed Standards of
Performance for Sodium Carbonate Plants.
130. 46 FR 49853, 10/8/81 - Delegation of Authority to the State of
California. 471'
131. 46 FR 53144, 10/28/81 - Alternate Method 1 to Reference Method 9
of Appendix A Promulgated. 475
132. 46 FR 55975, 11/13/81 - Waiver from New Source Performance Standard
for Homer City Unit No. 3 Steam Electric Generating Station;
Indiana County, Pa. 494
133. 46 FR 57497, 11/24/81 - Adjustment of Opacity Standard for Fossil
Fuel Fired Steam Generator. 510
46 FR 59300, 12/4/81 - Notice of Applicability of New Source
Performance Standards to ADM Milling Co.; Missouri.
Add. 2-18
-------
46 FR 59630, 12/7/81 - Notice of Availability of Various Control
Techniques Guideline Documents.
134. 46 FR 61125, 12/15/81 - Alternative Test Requirements for Anaconda
Aluminum Company's Sebree Plant, Henderson, Kentucky. 511
135. 46 FR 62065, 12/22/81 - Additional Source Categories Delegated to
Ohio and Indiana. 512
136. 46 FR 62066, 12/22/81 - Additional Source Categories Delegated to
the State of Oregon. 513
137. 46 FR 62067, 12/22/81 - Additional Source Categories Delegated to
State of Utah. 514
138. 46 FR 62449, 12/24/81 - Subdelegation of Authority to a Washington
Local Agency. 515
139. 46 FR 63270, 12/31/81 - Interim Enforcement Policy for Sulfur
Dioxide Emission Limitations in Indiana. 516
140. 47 FR 950, 1/8/82 - Revisions to the Priority List of Categories
of Stationary Sources. 517
141. 47 FR 2314, 1/15/82 - Correction to Waiver from NSPS for Homer City
Unit No. 3 Steam Electric Generating Station, Indiana County,
Pa. 519
142. 47 FR 3767, 1/27/82 - Revised Standards of Performance for
Stationary Gas Turbines. 520
143. 47 FR 7665, 2/22/82 - Delegation of Authority to the State of
Louisiana and Delegation of Authority to the State of Arkansas. 524
144. 47 FR 12626, 3/24/82 - Delegation of Authority to the State of
Mississippi. 525
145. 47 FR 16564, 4/16/82 - Standards of Performance Promulgated for
Lead-Acid Battery Manufacture. 526
146. 47 FR 16582, 4/16/82 - Standards of Performance Promulgated for
Phosphate Rock Plants. . 542
147. 47 FR 17285, 4/22/82 - Delegation of Authority to the State of
Oklahoma. 551
148. 47 FR 17989, 4/27/82 - Delegation of Authority to the State of
Delaware. 551
Add. 2-19
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing/
1. REPORT NO.
2.
3. RECIPIENT'S ACCESSION NO.
EPA-340/l-82-005a
». TITLE AND SUBTITLE
Standards of Performance for New Stationary
Sources - A Compilation as of May 1, 1982
Volume 1: Introduction, Summary and Standards
5. REPORT DATE
June 1982
6. PERFORMING ORGANIZATION CODE
. AUTHOR(S)
8. PERFORMING ORGANIZATION REPORT NO.
PN 3660-1-42
. PERFORMING ORGANIZATION NAME AND ADDRESS
>EDCo Environmental, Incorporated
11499 Chester Road
Cincinnati, Ohio 45246
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-01-6310
Task No. 42
12. SPONSORING AGENCY NAME AND ADDRESS
J.S. Environmental Protection Agency
Stationary Source Compliance Division
Washington, D.C. 20460
13. TYPE OF REPORT AND PERIOD COVERED
Compilation to May 1982
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
DSSE Project Officer:
Kirk Foster, MD-7, Research Triangle
Park, NC 27711; (919) 541-4571
16. ABSTRACT
This document is a compilation of the New Source Performance Standards promulgated
under Section 111 of the Clean Air Act, represented in full as amended. The infor-
mation contained herein supersedes all compilations published by the Enviornmental
Protection Agency prior to 1982. Volume 1 contains Sections I through III including:
Introduction, Summary Table, and Regulations as amended. Volume 2 contains Section
IV, Proposed Regulations, and Volume 3 contains Section V, the full text of all regu-
lations promulgated since 1971.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
COS AT I Field/Group
Mr pollution control
Regulations; Enforcement
New Source Performance
Standards
13B
14B
18. DISTRIBUTION STATEMENT
Unlimited
19. SECURITY CLASS (ThisReport/
Unclassified
21. NO. OF PAGES
?0. SECURITY CLASS (Thispage)
Unclassified
22. PRICE
EPA Form 2220-1 (»-7J)
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