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
                                     xvn

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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

-------
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.
                                      1-3

-------
   SECTION II
SUMMARY OF STANDARDS
   AND REVISIONS

-------
                   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
                                     II-l

-------
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

   
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(&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

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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

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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.
   
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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

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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

-------
   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

-------
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

-------
    (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

-------
 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.

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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

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                                 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

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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
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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

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 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)
                                                     111-40

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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

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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

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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

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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

-------
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

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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

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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

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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 
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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

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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

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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.
           
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  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

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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

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    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

-------
•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

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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

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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.
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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

-------
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

-------
             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

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                                                      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
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                                                                                                         •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

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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

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  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

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       TRANSVERSE
        TUBE AXIS
                \
                            FACE
                          •OPENING
                           PLANES

                             (a)
                           A SIDE PLANE
J
LONGITUDINAL 7 Dt
TUBE AXIS *~ \ .*

. ,!.-
s "7
* 
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        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

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  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
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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

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  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

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 -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

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 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

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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

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                     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

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                      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
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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
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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]

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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

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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

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                                    i in IK  i IM. or  opt:imio>>
                  •••• ••< Ue«tUl:
                                           im»k.T:
            I.IU4K  OPIH4TOITS  NOTES
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            tl lit fl«U lilt i
            iMtttel •( 111*1:
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                 Illltllll tl 11111(1.
                                                      linn " siuiee
                 lull iicliiilin I* iifli is «» kiiitntil is 0 I
            •••MI lip* Mi (Mlilil 4>il|»tUi:
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                 ikinitlillllll (ilUi, iklft. HUB friiiil, «l( I :
QJ
H-
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"** Ml ll*M»ll'l Illll
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LO (!••< KKI: tl|IH



• ttllUIC TWS
li»«« tiled = lilii
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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

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  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

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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

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  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
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  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

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  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
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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

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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:
                        
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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

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                                                                                                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.

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                                                       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

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                    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

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           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

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  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

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  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.
          
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 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

                                                                               
-------
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-------
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H
H
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O-
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GLASS
CHAMBER



                                                       DILUENT
                                                      NITROGEN
        Figure 16-4. Apparatus for field calibration.
                Ill-Appendix  A-89

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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.

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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

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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.

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  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

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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

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  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

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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

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 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

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 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

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   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

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  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

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                                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

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  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

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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

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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

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          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

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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

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ADDENDA

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                               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

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                         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

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                         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

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                               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

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                               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

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 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

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     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

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     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

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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

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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

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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

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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

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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

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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

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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

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      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

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     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

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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

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     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

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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

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     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

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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

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     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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