[Title 40 CFR ]
[Code of Federal Regulations (annual edition) - July 1, 2004 Edition]
[From the U.S. Government Printing Office]



[[Page i]]



          40


          Part 63 (Sec. Sec.  63.8980-End)

                         Revised as of July 1, 2004


          Protection of Environment
          
          


________________________

          Containing a codification of documents of general 
          applicability and future effect

          As of July 1, 2004
          With Ancillaries
                    Published by
                    Office of the Federal Register
                    National Archives and Records
                    Administration
                    A Special Edition of the Federal Register

[[Page ii]]



               ----------------------------------------------------------
               As of July 1, 2004
               Title 40, Part 63 (Sec. Sec.  63.1440-End)
               Revised as of July 1, 2003
               Is Replaced by Two Volumes
               Title 40, Part 63 (Sec. Sec.  63.1440-63.8830)
               and Part 63 (Sec. Sec.  63.8980-End)

               ----------------------------------------------------------


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[[Page iii]]




                            Table of Contents



                                                                    Page
  Explanation.................................................       v

  Title 40:
          Chapter I--Environmental Protection Agency 
          (Continued)                                                3
  Finding Aids:
      Material Approved for Incorporation by Reference........     897
      Table of CFR Titles and Chapters........................     899
      Alphabetical List of Agencies Appearing in the CFR......     917
      List of CFR Sections Affected...........................     927

[[Page iv]]





                     ----------------------------

                     Cite this Code: CFR
                     To cite the regulations in 
                       this volume use title, 
                       part and section number. 
                       Thus, 40 CFR 63.8980 
                       refers to title 40, part 
                       63, section 8980.

                     ----------------------------

[[Page v]]



                               EXPLANATION

    The Code of Federal Regulations is a codification of the general and 
permanent rules published in the Federal Register by the Executive 
departments and agencies of the Federal Government. The Code is divided 
into 50 titles which represent broad areas subject to Federal 
regulation. Each title is divided into chapters which usually bear the 
name of the issuing agency. Each chapter is further subdivided into 
parts covering specific regulatory areas.
    Each volume of the Code is revised at least once each calendar year 
and issued on a quarterly basis approximately as follows:

Title 1 through Title 16as of January 1...........
Title 17 through Title 27as of April 1............
Title 28 through Title 41as of July 1.............
Title 42 through Title 50as of October 1..........

    The appropriate revision date is printed on the cover of each 
volume.

LEGAL STATUS

    The contents of the Federal Register are required to be judicially 
noticed (44 U.S.C. 1507). The Code of Federal Regulations is prima facie 
evidence of the text of the original documents (44 U.S.C. 1510).

HOW TO USE THE CODE OF FEDERAL REGULATIONS

    The Code of Federal Regulations is kept up to date by the individual 
issues of the Federal Register. These two publications must be used 
together to determine the latest version of any given rule.
    To determine whether a Code volume has been amended since its 
revision date (in this case, July 1, 2004), consult the ``List of CFR 
Sections Affected (LSA),'' which is issued monthly, and the ``Cumulative 
List of Parts Affected,'' which appears in the Reader Aids section of 
the daily Federal Register. These two lists will identify the Federal 
Register page number of the latest amendment of any given rule.

EFFECTIVE AND EXPIRATION DATES

    Each volume of the Code contains amendments published in the Federal 
Register since the last revision of that volume of the Code. Source 
citations for the regulations are referred to by volume number and page 
number of the Federal Register and date of publication. Publication 
dates and effective dates are usually not the same and care must be 
exercised by the user in determining the actual effective date. In 
instances where the effective date is beyond the cut-off date for the 
Code a note has been inserted to reflect the future effective date. In 
those instances where a regulation published in the Federal Register 
states a date certain for expiration, an appropriate note will be 
inserted following the text.

OMB CONTROL NUMBERS

    The Paperwork Reduction Act of 1980 (Pub. L. 96-511) requires 
Federal agencies to display an OMB control number with their information 
collection request.

[[Page vi]]

Many agencies have begun publishing numerous OMB control numbers as 
amendments to existing regulations in the CFR. These OMB numbers are 
placed as close as possible to the applicable recordkeeping or reporting 
requirements.

OBSOLETE PROVISIONS

    Provisions that become obsolete before the revision date stated on 
the cover of each volume are not carried. Code users may find the text 
of provisions in effect on a given date in the past by using the 
appropriate numerical list of sections affected. For the period before 
January 1, 2001, consult either the List of CFR Sections Affected, 1949-
1963, 1964-1972, 1973-1985, or 1986-2000, published in 11 separate 
volumes. For the period beginning January 1, 2001, a ``List of CFR 
Sections Affected'' is published at the end of each CFR volume.

INCORPORATION BY REFERENCE

    What is incorporation by reference? Incorporation by reference was 
established by statute and allows Federal agencies to meet the 
requirement to publish regulations in the Federal Register by referring 
to materials already published elsewhere. For an incorporation to be 
valid, the Director of the Federal Register must approve it. The legal 
effect of incorporation by reference is that the material is treated as 
if it were published in full in the Federal Register (5 U.S.C. 552(a)). 
This material, like any other properly issued regulation, has the force 
of law.
    What is a proper incorporation by reference? The Director of the 
Federal Register will approve an incorporation by reference only when 
the requirements of 1 CFR part 51 are met. Some of the elements on which 
approval is based are:
    (a) The incorporation will substantially reduce the volume of 
material published in the Federal Register.
    (b) The matter incorporated is in fact available to the extent 
necessary to afford fairness and uniformity in the administrative 
process.
    (c) The incorporating document is drafted and submitted for 
publication in accordance with 1 CFR part 51.
    Properly approved incorporations by reference in this volume are 
listed in the Finding Aids at the end of this volume.
    What if the material incorporated by reference cannot be found? If 
you have any problem locating or obtaining a copy of material listed in 
the Finding Aids of this volume as an approved incorporation by 
reference, please contact the agency that issued the regulation 
containing that incorporation. If, after contacting the agency, you find 
the material is not available, please notify the Director of the Federal 
Register, National Archives and Records Administration, Washington DC 
20408, or call (202) 741-6010.

CFR INDEXES AND TABULAR GUIDES

    A subject index to the Code of Federal Regulations is contained in a 
separate volume, revised annually as of January 1, entitled CFR Index 
and Finding Aids. This volume contains the Parallel Table of Statutory 
Authorities and Agency Rules (Table I). A list of CFR titles, chapters, 
and parts and an alphabetical list of agencies publishing in the CFR are 
also included in this volume.
    An index to the text of ``Title 3--The President'' is carried within 
that volume.
    The Federal Register Index is issued monthly in cumulative form. 
This index is based on a consolidation of the ``Contents'' entries in 
the daily Federal Register.
    A List of CFR Sections Affected (LSA) is published monthly, keyed to 
the revision dates of the 50 CFR titles.

[[Page vii]]


REPUBLICATION OF MATERIAL

    There are no restrictions on the republication of material appearing 
in the Code of Federal Regulations.

INQUIRIES

    For a legal interpretation or explanation of any regulation in this 
volume, contact the issuing agency. The issuing agency's name appears at 
the top of odd-numbered pages.
    For inquiries concerning CFR reference assistance, call 202-741-6000 
or write to the Director, Office of the Federal Register, National 
Archives and Records Administration, Washington, DC 20408 or e-mail 
[email protected].

SALES

    The Government Printing Office (GPO) processes all sales and 
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register. The NARA site also contains links to GPO Access.

                              Raymond A. Mosley,
                                    Director,
                          Office of the Federal Register.

July 1, 2004.

[[Page ix]]



                               THIS TITLE

    Title 40--Protection of Environment is composed of thirty volumes. 
The parts in these volumes are arranged in the following order: parts 1-
49, parts 50-51, part 52 (52.01-52.1018), part 52 (52.1019-End), parts 
53-59, part 60 (60.1-End), part 60 (Appendices), parts 61-62, part 63 
(63.1-63.599), part 63 (63.600-1-63.1199), part 63 (63.1200-63.1439), 
part 63 (63.1440-63.8830), part 63 (63.8980-End) parts 64-71, parts 72-
80, parts 81-85, part 86 (86.1-86.599-99) part 86 (86.600-1-End), parts 
87-99, parts 100-135, parts 136-149, parts 150-189, parts 190-259, parts 
260-265, parts 266-299, parts 300-399, parts 400-424, parts 425-699, 
parts 700-789, and part 790 to End. The contents of these volumes 
represent all current regulations codified under this title of the CFR 
as of July 1, 2004.

    Chapter I--Environmental Protection Agency appears in all thirty 
volumes. An alphabetical Listing of Pesticide Chemicals Index appears in 
parts 150-189. Regulations issued by the Council on Environmental 
Quality appear in the volume containing part 790 to End. The OMB control 
numbers for title 40 appear in Sec.  9.1 of this chapter.

    For this volume, Robert J. Sheehan was Chief Editor. The Code of 
Federal Regulations publication program is under the direction of 
Frances D. McDonald, assisted by Alomha S. Morris.

[[Page x]]




[[Page 1]]



                   TITLE 40--PROTECTION OF ENVIRONMENT




                      (This book contains part 63)

  --------------------------------------------------------------------
                                                                    Part

chapter i--Environmental Protection Agency (Continued)......          63

[[Page 3]]



         CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)




  --------------------------------------------------------------------


  Editorial Note: Nomenclature changes to chapter I appear at 65 FR 
47324, 47325, Aug. 2, 2000.

                 SUBCHAPTER C--AIR PROGRAMS (CONTINUED)
Part                                                                Page
63              National emission standards for hazardous 
                    air pollutants for source categories....           5

[[Page 5]]



                  SUBCHAPTER C_AIR PROGRAMS (CONTINUED)





PART 63_NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR 
SOURCE CATEGORIES--Table of Contents




Subpart NNNNN_National Emission Standards for Hazardous Air Pollutants: 
                      Hydrochloric Acid Production

                        What This Subpart Covers

63.8980 What is the purpose of this subpart?
63.8985 Am I subject to this subpart?
63.8990 What parts of my plant does this subpart cover?
63.8995 When do I have to comply with this subpart?

            Emission Limitations and Work Practice Standards

63.9000 What emission limitations and work practice standards must I 
          meet?

                     General Compliance Requirements

63.9005 What are my general requirements for complying with this 
          subpart?

               Testing and Initial Compliance Requirements

63.9010 By what date must I conduct performance tests?
63.9015 When must I conduct subsequent performance tests?
63.9020 What performance tests and other procedures must I use?
63.9025 What are my monitoring installation, operation, and maintenance 
          requirements?
63.9030 How do I demonstrate initial compliance with the emission 
          limitations and work practice standards?

                   Continuous Compliance Requirements

63.9035 How do I monitor and collect data to demonstrate continuous 
          compliance?
63.9040 How do I demonstrate continuous compliance with the emission 
          limitations and work practice standards?

                   Notifications, Reports, and Records

63.9045 What notifications must I submit and when?
63.9050 What reports must I submit and when?
63.9055 What records must I keep?
63.9060 In what form and how long must I keep my records?

                   Other Requirements and Information

63.9065 What parts of the General Provisions apply to me?
63.9070 Who implements and enforces this subpart?
63.9075 What definitions apply to this subpart?

Table 1 to Subpart NNNNN of Part 63--Emission Limits and Work Practice 
          Standards
Table 2 to Subpart NNNNN of Part 63--Operating Limits
Table 3 to Subpart NNNNN of Part 63--Performance Test Requirements for 
          HCl Production Affected Sources
Table 4 to Subpart NNNNN of Part 63--Initial Compliance with Emission 
          Limitations and Work Practice Standards
Table 5 to Subpart NNNNN of Part 63--Continuous Compliance with Emission 
          Limitations and Work Practice Standards
Table 6 to Subpart NNNNN of Part 63--Requirements for Reports
Table 7 to Subpart NNNNN of Part 63--Applicability of General Provisions 
          to Subpart NNNNN

Subpart OOOOO [Reserved]

 Subpart PPPPP_National Emission Standards for Hazardous Air Pollutants 
                      for Engine Test Cells/Stands

                        What This Subpart Covers

63.9280 What is the purpose of subpart PPPPP?
63.9285 Am I subject to this subpart?
63.9290 What parts of my plant does this subpart cover?
63.9295 When do I have to comply with this subpart?

                          Emission Limitations

63.9300 What emission limitation must I meet?
63.9301 What are my options for meeting the emission limits?
63.9302 What operating limits must I meet?

                     General Compliance Requirements

63.9305 What are my general requirements for complying with this 
          subpart?
63.9306 What are my continuous parameter monitoring system (CPMS) 
          installation, operation, and maintenance requirements?
63.9307 What are my continuous emissions monitoring system installation, 
          operation, and maintenance requirements?

               Testing and Initial Compliance Requirements

63.9310 By what date must I conduct the initial compliance 
          demonstrations?

[[Page 6]]

63.9320 What procedures must I use?
63.9321 What are the general requirements for performance tests?
63.9322 How do I determine the emission capture system efficiency?
63.9323 How do I determine the add-on control device emission 
          destruction or removal efficiency?
63.9324 How do I establish the emission capture system and add-on 
          control device operating limits during the performance test?
63.9330 How do I demonstrate initial compliance with the emission 
          limitation?

                   Continuous Compliance Requirements

63.9335 How do I monitor and collect data to demonstrate continuous 
          compliance?
63.9340 How do I demonstrate continuous compliance with the emission 
          limitation?

                   Notifications, Reports, and Records

63.9345 What notifications must I submit and when?
63.9350 What reports must I submit and when?
63.9355 What records must I keep?
63.9360 In what form and how long must I keep my records?

                   Other Requirements and Information

63.9365 What parts of the General Provisions apply to me?
63.9370 Who implements and enforces this subpart?
63.9375 What definitions apply to this subpart?

Table 1 to Subpart PPPPP of Part 63--Emission Limitations
Table 2 to Subpart PPPPP of Part 63--Operating Limits
Table 3 to Subpart PPPPP of Part 63--Requirements for Initial Compliance 
          Demonstrations
Table 4 to Subpart PPPPP of Part 63--Initial Compliance with Emission 
          Limitations
Table 5 to Subpart PPPPP of Part 63--Continuous Compliance with Emission 
          Limitations
Table 6 to Subpart PPPPP of Part 63--Requirements for Reports
Table 7 to Subpart PPPPP of Part 63--Applicability of General Provisions 
          to Subpart PPPPP

 Subpart QQQQQ_National Emission Standards for Hazardous Air Pollutants 
             for Friction Materials Manufacturing Facilities

                        What This Subpart Covers

63.9480 What is the purpose of this subpart?
63.9485 Am I subject to this subpart?
63.9490 What parts of my plant does this subpart cover?
63.9495 When do I have to comply with this subpart?

                          Emission Limitations

63.9500 What emission limitations must I meet?

                     General Compliance Requirements

63.9505 What are my general requirements for complying with this 
          subpart?

              Initial Compliance Demonstration Requirements

63.9510 By what date must I conduct my initial compliance demonstration?
63.9515 How do I demonstrate initial compliance with the emission 
          limitation that applies to me?
63.9520 What procedures must I use to demonstrate initial compliance?
63.9525 What are the installation, operation, and maintenance 
          requirements for my weight measurement device?

                   Continuous Compliance Requirements

63.9530 How do I demonstrate continuous compliance with the emission 
          limitation that applies to me?

                   Notifications, Reports, and Records

63.9535 What notifications must I submit and when?
63.9540 What reports must I submit and when?
63.9545 What records must I keep?
63.9550 In what form and how long must I keep my records?

                   Other Requirements and Information

63.9555 What parts of the General Provisions apply to me?
63.9560 Who implements and enforces this subpart?
63.9565 What definitions apply to this subpart?
63.9570 How do I apply for alternative compliance requirements?
63.9571-63.9579 [Reserved]

Table 1 to Subpart QQQQQ--Applicability of General Provisions to Subpart 
          QQQQQ

Subpart RRRRR_National Emission Standards for Hazardous Air Pollutants: 
                      Taconite Iron Ore Processing

                        What This Subpart Covers

63.9580 What is the purpose of this subpart?
63.9581 Am I subject to this subpart?
63.9582 What parts of my plant does this subpart cover?
63.9583 When do I have to comply with this subpart?

[[Page 7]]

            Emission Limitations and Work Practice Standards

63.9590 What emission limitations must I meet?
63.9591 What work practice standards must I meet?

                 Operation and Maintenance Requirements

63.9600 What are my operation and maintenance requirements?

                     General Compliance Requirements

63.9610 What are my general requirements for complying with this 
          subpart?

                     Initial Compliance Requirements

63.9620 On which units and by what date must I conduct performance tests 
          or other initial compliance demonstrations?
63.9621 What test methods and other procedures must I use to demonstrate 
          initial compliance with the emission limits for particulate 
          matter?
63.9622 What test methods and other procedures must I use to establish 
          and demonstrate initial compliance with the operating limits?
63.9623 How do I demonstrate initial compliance with the emission 
          limitations that apply to me?
63.9624 How do I demonstrate initial compliance with the work practice 
          standards that apply to me?
63.9625 How do I demonstrate initial compliance with the operation and 
          maintenance requirements that apply to me?

                   Continuous Compliance Requirements

63.9630 When must I conduct subsequent performance tests?
63.9631 What are my monitoring requirements?
63.9632 What are the installation, operation, and maintenance 
          requirements for my monitoring equipment?
63.9633 How do I monitor and collect data to demonstrate continuous 
          compliance?
63.9634 How do I demonstrate continuous compliance with the emission 
          limitations that apply to me?
63.9635 How do I demonstrate continuous compliance with the work 
          practice standards that apply to me?
63.9636 How do I demonstrate continuous compliance with the operation 
          and maintenance requirements that apply to me?
63.9637 What other requirements must I meet to demonstrate continuous 
          compliance?

                   Notifications, Reports, and Records

63.9640 What notifications must I submit and when?
63.9641 What reports must I submit and when?
63.9642 What records must I keep?
63.9643 In what form and how long must I keep my records?

                   Other Requirements and Information

63.9650 What parts of the General Provisions apply to me?
63.9651 Who implements and enforces this subpart?
63.9652 What definitions apply to this subpart?

Table 1 to Subpart RRRRR of Part 63--Emission Limits
Table 2 to Subpart RRRRR of Part 63--Applicability of General Provisions 
          to Subpart RRRRR of Part 63

 Subpart SSSSS_National Emission Standards for Hazardous Air Pollutants 
                  for Refractory Products Manufacturing

                        What This Subpart Covers

63.9780 What is the purpose of this subpart?
63.9782 Am I subject to this subpart?
63.9784 What parts of my plant does this subpart cover?
63.9786 When do I have to comply with this subpart?

            Emission Limitations and Work Practice Standards

63.9788 What emission limits, operating limits, and work practice 
          standards must I meet?
63.9790 What are my options for meeting the emission limits?

                     General Compliance Requirements

63.9792 What are my general requirements for complying with this 
          subpart?
63.9794 What do I need to know about operation, maintenance, and 
          monitoring plans?

               Testing and Initial Compliance Requirements

63.9796 By what date must I conduct performance tests?
63.9798 When must I conduct subsequent performance tests?
63.9800 How do I conduct performance tests and establish operating 
          limits?
63.9802 How do I develop an emissions profile?
63.9804 What are my monitoring system installation, operation, and 
          maintenance requirements?
63.9806 How do I demonstrate initial compliance with the emission 
          limits, operating limits, and work practice standards?

                   Continuous Compliance Requirements

63.9808 How do I monitor and collect data to demonstrate continuous 
          compliance?

[[Page 8]]

63.9810 How do I demonstrate continuous compliance with the emission 
          limits, operating limits, and work practice standards?

                   Notifications, Reports, and Records

63.9812 What notifications must I submit and when?
63.9814 What reports must I submit and when?
63.9816 What records must I keep?
63.9818 In what form and how long must I keep my records?

                   Other Requirements and Information

63.9820 What parts of the General Provisions apply to me?
63.9822 Who implements and enforces this subpart?
63.9824 What definitions apply to this subpart?

Table 1 to Subpart SSSSS of Part 63--Emission Limits
Table 2 to Subpart SSSSS of Part 63--Operating Limits
Table 3 to Subpart SSSSS of Part 63--Work Practice Standards
Table 4 to Subpart SSSSS to Part 63--Requirements for Performance Tests
Table 5 to Subpart SSSSS of Part 63--Initial Compliance with Emission 
          Limits
Table 6 to Subpart SSSSS of Part 63--Initial Compliance with Work 
          Practice Standards
Table 7 to Subpart SSSSS to Part 63--Continuous Compliance with Emission 
          Limits
Table 8 to Subpart SSSSS of Part 63--Continuous Compliance with 
          Operating Limits
Table 9 to Subpart SSSSS of Part 63--Continuous Compliance with Work 
          Practice Standards
Table 10 to Subpart SSSSS of Part 63--Requirements for Reports
Table 11 to Subpart SSSSS of Part 63--Applicability of General 
          Provisions to Subpart SSSSS

Subpart TTTTT_National Emissions Standards for Hazardous Air Pollutants 
                     for Primary Magnesium Refining

                        What This Subpart Covers

63.9880 What is the purpose of this subpart?
63.9881 Am I subject to this subpart?
63.9882 What parts of my plant does this subpart cover?
63.9883 When do I have to comply with this subpart?

            Emission Limitations and Work Practice Standards

63.9890 What emission limitations must I meet?
63.9891 What work practice standards must I meet for my fugitive dust 
          sources?

                 Operation and Maintenance Requirements

63.9900 What are my operation and maintenance requirements?

                     General Compliance Requirements

63.9910 What are my general requirements for complying with this 
          subpart?

                     Initial Compliance Requirements

63.9911 By what date must I conduct performance tests or other initial 
          compliance demonstrations?
63.9912 When must I conduct subsequent performance tests?
63.9913 What test methods and other procedures must I use to demonstrate 
          initial compliance with the emission limits for particulate 
          matter and PM10?
63.9914 What test methods and other procedures must I use to demonstrate 
          initial compliance with chlorine and hydrochloric acid 
          emission limits?
63.9915 What test methods and other procedures must I use to demonstrate 
          initial compliance with dioxin/furan emission limits?
63.9916 What test methods and other procedures must I use to establish 
          and demonstrate initial compliance with the operating limits?
63.9917 How do I demonstrate initial compliance with the emission 
          limitations and work practice standards that apply to me?
63.9918 How do I demonstrate initial compliance with the operation and 
          maintenance requirements that apply to me?

                   Continuous Compliance Requirements

63.9920 What are my monitoring requirements?
63.9921 What are the installation, operation, and maintenance 
          requirements for my monitors?
63.9922 How do I monitor and collect data to demonstrate continuous 
          compliance?
63.9923 How do I demonstrate continuous compliance with the emission 
          limitations and work practice standards that apply to me?
63.9924 How do I demonstrate continuous compliance with the operation 
          and maintenance requirements that apply to me?
63.9925 What other requirements must I meet to demonstrate continuous 
          compliance?

                   Notifications, Reports, and Records

63.9930 What notifications must I submit and when?
63.9931 What reports must I submit and when?
63.9932 What records must I keep?

[[Page 9]]

63.9933 In what form and how long must I keep my records?

                   Other Requirements and Information

63.9940 What parts of the General Provisions apply to me?
63.9941 Who implements and enforces this subpart?
63.9942 What definitions apply to this subpart?

Table 1 to Subpart TTTTT of Part 63--Emission Limits
Table 2 to Subpart TTTTT of Part 63--Toxic Equivalency Factors
Table 3 to Subpart TTTTT of Part 63--Initial Compliance with Emission 
          Limits
Table 4 to Subpart TTTTT of Part 63--Continuous Compliance with Emission 
          Limits
Table 5 to Subpart TTTTT of Part 63--Applicability of General Provisions 
          to Subpart TTTTT of Part 63
Appendix A to Part 63--Test Methods
Appendix B to Part 63--Sources Defined for Early Reduction Provisions
Appendix C to Part 63--Determination of the Fraction Biodegraded 
          (Fbio) in a Biological Treatment Unit
Appendix D to Part 63--Alternative Validation Procedure for EPA Waste 
          and Wastewater Methods
Appendix E to Part 63--Monitoring Procedure for Nonthoroughly Mixed Open 
          Biological Treatment Systems at Kraft Pulp Mills Under Unsafe 
          Sampling Conditions

    Authority: 42 U.S.C. 7401 et seq.

    Source: 57 FR 61992, Dec. 29, 1992, unless otherwise noted.



Subpart NNNNN_National Emission Standards for Hazardous Air Pollutants: 
                      Hydrochloric Acid Production

    Source: 68 FR 19090, Apr. 17, 2003, unless otherwise noted.

                        What This Subpart Covers



Sec. 63.8980  What is the purpose of this subpart?

    This subpart establishes national emission standards for hazardous 
air pollutants (NESHAP) and work practice standards for hazardous air 
pollutants (HAP) emitted from hydrochloric acid (HCl) production. This 
subpart also establishes requirements to demonstrate initial and 
continuous compliance with the emission limitations and work practice 
standards.



Sec. 63.8985  Am I subject to this subpart?

    (a) You are subject to this subpart if you own or operate an HCl 
production facility that produces a liquid HCl product at a 
concentration of 30 weight percent or greater during its normal 
operations and is located at, or is part of, a major source of HAP. This 
does not include HCl production facilities that only produce 
occasionally liquid HCl product at a concentration of 30 weight percent 
or greater.
    (1) An HCl production facility is the collection of unit operations 
and equipment associated with the production of liquid HCl product. The 
HCl production facility begins at the point where a gaseous stream 
containing HCl enters the HCl production unit. The HCl production 
facility includes all HCl storage tanks that contain liquid HCl product 
that is produced in the HCl production unit, with the exceptions noted 
in paragraph (a)(2) of this section. The HCl production facility also 
includes all HCl transfer operations that load HCl product produced in 
the HCl production unit into a tank truck, rail car, ship, or barge, 
along with the piping and other equipment in HCl service used to 
transfer liquid HCl product from the HCl production unit to the HCl 
storage tanks and/or HCl transfer operations. The HCl production 
facility ends at the point that the liquid HCl product produced in the 
HCl production unit is loaded into a tank truck, rail car, ship, or 
barge, at the point the HCl product enters another process on the plant 
site, or at the point the HCl product leaves the plant site via 
pipeline.
    (2) Storage tanks that are dedicated feedstock tanks for another 
process and storage tanks that store HCl dedicated for use in wastewater 
treatment are not considered part of an HCl production facility.
    (3) A major source of HAP emissions is any stationary source or 
group of stationary sources within a contiguous area under common 
control that emits or has the potential to emit any single HAP at a rate 
of 9.07 megagrams (10 tons) or more per year or any combination of HAP 
at a rate of 22.68 megagrams (25 tons) or more per year.

[[Page 10]]

    (b) An HCl production facility is not subject to this subpart if it 
is also subject to NESHAP under one of the subparts listed in paragraphs 
(b)(1) through (5) of this section.
    (1) 40 CFR part 63, subpart S, National Emission Standards for 
Hazardous Air Pollutants from the Pulp and Paper Industry.
    (2) 40 CFR part 63, subpart CCC, National Emission Standards for 
Hazardous Air Pollutants for Steel Pickling--HCl Process Facilities and 
Hydrochloric Acid Regeneration Plants.
    (3) 40 CFR part 63, subpart MMM, National Emission Standards for 
Hazardous Air Pollutants for Pesticide Active Ingredient Production.
    (4) 40 CFR part 63, subpart EEE, National Emission Standards for 
Hazardous Air Pollutants for Hazardous Waste Combustors.
    (5) 40 CFR part 63, subpart GGG, National Emission Standards for 
Pharmaceuticals Production.
    (c) An HCl production facility is not subject to this subpart if it 
is located following the incineration of chlorinated waste gas streams, 
waste liquids, or solid wastes, and the emissions from the HCl 
production facility are subject to one of the requirements listed in 
paragraphs (c)(1) through (3) of this section.
    (1) Section 63.113(c), subpart G, National Emission Standards for 
Organic Hazardous Air Pollutants from the Synthetic Organic Chemical 
Manufacturing Industry for Process Vents, Storage Vessels, Transfer 
Operations, and Wastewater.
    (2) Section 264.343(b), Standards for Owners and Operators of 
Hazardous Waste Treatment, Storage, and Disposal Facilities (subpart O, 
Incinerators).
    (3) Section 266.107, subpart H, Burning of Hazardous Waste in 
Boilers and Industrial Furnaces.
    (d) An HCl production facility is not subject to this subpart if it 
produces HCl through the direct synthesis of hydrogen and chlorine and 
is part of a chlor-alkali facility.
    (e) An HCl production facility is not subject to this subpart if it 
is a research and development facility.
    (f) An HCl production facility is not subject to this subpart if all 
of the gaseous streams containing HCl and chlorine (Cl2) from 
HCl process vents, HCl storage tanks, and HCl transfer operations are 
recycled or routed to another process prior to being discharged to the 
atmosphere.



Sec. 63.8990  What parts of my plant does this subpart cover?

    (a) This subpart applies to each new, reconstructed, or existing 
affected source at an HCl production facility.
    (b) The affected source is the group of one or more HCl production 
facilities at a plant site that are subject to this subpart, and all 
associated wastewater operations, which contain the collection of 
emission streams listed in paragraphs (b)(1) through (5) of this 
section.
    (1) Each emission stream from an HCl process vent.
    (2) Each emission stream from an HCl storage tank.
    (3) Each emission stream from an HCl transfer operation.
    (4) Each emission stream resulting from leaks from equipment in HCl/
Cl2 service.
    (5) Each emission stream from HCl wastewater operations. There are 
no emission limitations or other requirements in this subpart that apply 
to HCl wastewater operations.
    (c) An affected source is a new affected source if you commenced 
construction of the affected source after September 18, 2001 and you met 
the applicability criteria of Sec. 63.8985 at the time you commenced 
construction.
    (d) An affected source is reconstructed if you meet the criteria as 
defined in Sec. 63.2.
    (e) An affected source is existing if it is not new or 
reconstructed.



Sec. 63.8995  When do I have to comply with this subpart?

    (a) If you have a new or reconstructed affected source, you must 
comply with this subpart according to paragraphs (a)(1) or (2) of this 
section.
    (1) If you start up your affected source before April 17, 2003, you 
must comply with the emission limitations and work practice standards in 
this subpart no later than April 17, 2003.
    (2) If you start up your affected source after April 17, 2003, you 
must comply with the emission limitations

[[Page 11]]

and work practice standards in this subpart upon startup of your 
affected source.
    (b) If you have an existing affected source, you must comply with 
the emission limitations and work practice standards no later than 3 
years after April 17, 2003.
    (c) If you have an area source that increases its emissions or its 
potential to emit such that it becomes a major source of HAP, the 
provisions in paragraphs (c)(1) and (2) of this section apply.
    (1) Any portion of the existing facility that is a new affected 
source or a new reconstructed source must be in compliance with this 
subpart upon startup.
    (2) All other parts of the source must be in compliance with this 
subpart no later than the date 3 years after the area source becomes a 
major source.
    (d) You must meet the notification requirements in Sec. 63.9045 
according to the schedule in Sec. 63.9045 and in subpart A of this 
part. Some of the notifications must be submitted before you are 
required to comply with the emission limitations in this subpart.

            Emission Limitations and Work Practice Standards



Sec. 63.9000  What emission limitations and work practice standards must 
I meet?

    (a) With the exceptions noted in paragraph (c) of this section, you 
must meet the applicable emission limit and work practice standard in 
Table 1 to this subpart for each emission stream listed under Sec. 
63.8990(b)(1) through (4) that is part of your affected source.
    (b) With the exceptions noted in paragraph (c) of this section, you 
must meet the applicable operating limit in Table 2 to this subpart for 
each emission stream listed under Sec. 63.8990(b)(1) through (3) that 
is part of your affected source.
    (c) The emission streams listed in paragraphs (c)(1) through (3) of 
this section are exempt from the emission limitations, work practice 
standards, and all other requirements of this subpart.
    (1) Emission streams from HCl storage tanks that never store liquid 
HCl product with a concentration of 30 weight percent or greater.
    (2) Emission streams from HCl transfer operations that never load 
liquid HCl product with a concentration of 30 weight percent or greater.
    (3) Emission streams from HCl wastewater operations.

                     General Compliance Requirements



Sec. 63.9005  What are my general requirements for complying with this 
subpart?

    (a) You must be in compliance with the emission limitations and work 
practice standards in this subpart at all times, except during periods 
of startup, shutdown, and malfunction.
    (b) You must always operate and maintain your affected source, 
including air pollution control and monitoring equipment, according to 
the provisions in Sec. 63.6(e)(1)(i).
    (c) You must develop and implement a written startup, shutdown, and 
malfunction plan according to the provisions in Sec. 63.6(e)(3).
    (d) All monitoring equipment shall be installed, calibrated, 
maintained, and operated according to manufacturer's specifications or 
other written procedures that provide adequate assurance that the 
equipment would reasonably be expected to monitor accurately. For each 
monitoring system required in this section, you must develop, implement, 
and submit to the Administrator a site-specific monitoring plan that 
addresses the installation requirements in paragraphs (d)(1) through (3) 
of this section, the ongoing procedures in paragraphs (d)(4) through (6) 
of this section, and the requirements in Sec. 63.9025, as applicable. 
You must submit the plan with your Notification of Compliance Status. 
Upon request of the Administrator, you must promptly correct any 
deficiencies in a site-specific monitoring plan and submit the revised 
plan.
    (1) Installation of the continuous monitoring system (CMS) sampling 
probe or other interface at a measurement location relative to each 
affected process unit such that the measurement is representative of 
control of the exhaust emissions (e.g., on or downstream of the last 
control device).

[[Page 12]]

    (2) Performance and equipment specifications for the sample 
interface, the pollutant concentration or parametric signal analyzer, 
and the data collection and reduction system.
    (3) Performance evaluation procedures and acceptance criteria (e.g., 
calibrations).
    (4) Ongoing operation and maintenance (O&M) procedures in accordance 
with the general requirements of Sec. Sec. 63.8(c)(1), (3), (4)(ii), 
(7), and (8), and 63.9025.
    (5) Ongoing data quality assurance procedures in accordance with the 
general requirements of Sec. 63.8(d).
    (6) Ongoing recordkeeping and reporting procedures in accordance 
with the general requirements of Sec. 63.10(c) and (e)(1) and (2)(i).

               Testing and Initial Compliance Requirements



Sec. 63.9010  By what date must I conduct performance tests?

    (a) If you have a new or reconstructed affected source, you must 
conduct performance tests within 180 calendar days after the compliance 
date that is specified for your source in Sec. 63.8995(a) and according 
to the provisions in Sec. 63.7(a)(2).
    (b) If you have an existing affected source, you must conduct 
performance tests within 180 calendar days after the compliance date 
that is specified for your existing affected source in Sec. 63.8995(b) 
and according to the provisions in Sec. 63.7(a)(2).
    (c) If you commenced construction or reconstruction between 
September 18, 2001 and April 17, 2003, you must demonstrate initial 
compliance with either the proposed emission limitation or the 
promulgated emission limitation no later than 180 calendar days after 
April 17, 2003 or within 180 calendar days after startup of the source, 
whichever is later, according to Sec. 63.7(a)(2)(ix).



Sec. 63.9015  When must I conduct subsequent performance tests?

    (a) You must conduct all applicable performance tests according to 
the procedures in Sec. 63.9020 on the earlier of your title V operating 
permit renewal or within 5 years of issuance of your title V permit.
    (b) You must report the results of subsequent performance tests 
within 60 days after the completion of the test. This report should also 
verify that the operating limits for your affected source have not 
changed or provide documentation of revised operating limits established 
as specified in Table 2 to this subpart. The reports for all subsequent 
performance tests should include all applicable information required in 
Sec. 63.9050.



Sec. 63.9020  What performance tests and other procedures must I use?

    (a) You must conduct each performance test in Table 3 to this 
subpart that applies to you as directed in paragraphs (a)(1) through (4) 
of this section, except as noted in paragraphs (b) and (c) of this 
section.
    (1) You must develop a site-specific test plan according to Sec. 
63.7(c)(2) and conduct each performance test according to the site-
specific test plan.
    (2) You must conduct each performance test under representative 
conditions according to the requirements in Sec. 63.7(e)(1) and under 
the specific conditions that this subpart specifies in Table 3.
    (3) You may not conduct performance tests during periods of startup, 
shutdown, or malfunction, as specified in Sec. 63.7(e)(1).
    (4) You must conduct at least three separate test runs for each 
performance test required in this section, as specified in Sec. 
63.7(e)(3). Each test run must last at least 1 hour.
    (b) If you are complying with a percent reduction emission 
limitation, you must determine the percent reduction in accordance with 
paragraphs (b)(1) and (2) of this section.
    (1) Calculate the mass rate of either HCl or chlorine using 
Equations 1 and 2 of this section:
[GRAPHIC] [TIFF OMITTED] TR17AP03.000

where:

Ci, Co = Concentration of HCl or Cl2 in 
the gas stream at the inlet and outlet of the control device(s), 
respectively, dry basis, parts per million by volume.

[[Page 13]]

Ei, Eo = Mass rate of HCl or Cl2 at the 
inlet and outlet of the control device(s), respectively, dry basis, 
kilogram per hour.
Mi, Mo = Molecular weight of HCl or Cl2 
at the inlet and outlet of the control device(s), respectively, gram/
gram-mole.
Qi, Qo = Flow rate of gas stream at the inlet and 
outlet of the control device(s), respectively, dry standard cubic meter 
per minute.
K2 = Constant, 2.494 x 10-6 (parts per million)\-
1\ (gram-mole per standard cubic meter) (kilogram/gram) (minute/hour), 
where standard temperature (gram-mole per standard cubic meter) is 20 
[deg]C.

    (2) Calculate the percent reduction of HCl or Cl2 using 
Equation 3 of this section:
[GRAPHIC] [TIFF OMITTED] TR17AP03.001

where:

R = Control efficiency of control device(s).
Ei = Mass rate of HCl or Cl2 to the inlet to the 
control device(s), kilograms per hour.
Eo = Mass rate of HCl or Cl2 at the outlet of the 
control device(s), kilograms per hour.

    (c) You may prepare a design evaluation in lieu of conducting a 
performance test for HCl storage tanks and HCl transfer operations that 
are not routed to a control device that also controls HCl process vent 
emissions or any other continuous vent stream. The design evaluation 
shall include documentation demonstrating that the control technique 
being used achieves the required control efficiency when a liquid HCl 
product with a concentration of 30 weight percent or greater is being 
loaded into the storage tank, or a tank truck, rail car, ship, or barge.
    (1) If you use a caustic scrubber control device or a water scrubber 
control device, the design evaluation shall address the vent stream 
composition, constituent concentrations, liquid-to-vapor ratio, 
scrubbing liquid flow rate and concentration, temperature, and the 
reaction kinetics of the constituents with the scrubbing liquid. The 
design evaluation shall establish the design exhaust vent concentration 
level and shall include the additional information in paragraphs 
(c)(1)(i) and (ii) of this section for trays and a packed column 
scrubber.
    (i) Type and total number of theoretical and actual trays.
    (ii) Type and total surface area of packing for entire column and 
for individual packed sections, if the column contains more than one 
packed section.
    (2) If you use any other control device, the design evaluation shall 
address the composition and HAP concentration of the vent stream 
immediately preceding the control device, as well as other parameters 
necessary to demonstrate that the control technique being used achieves 
the required control efficiency when a liquid HCl product with a 
concentration of 30 weight percent or greater is being loaded into the 
storage tank, or a tank truck, rail car, ship, or barge.
    (d) You are not required to conduct a performance test for an 
emission point for which a performance test was conducted within the 
previous 5-year period, using the same test methods specified in this 
section and for which either no deliberate process changes have been 
made since the test, or the owner or operator can demonstrate that the 
results of the performance test, with or without adjustments, reliably 
demonstrate compliance despite process changes. The operating limits 
reported under the previous performance test shall be sufficient to meet 
the monitoring requirements in this subpart.
    (e) You must establish all operating limits with which you will 
demonstrate continuous compliance with the applicable emission limits in 
Table 1 to this subpart as described in paragraphs (e)(1) through (3) of 
this section.
    (1) If you use a caustic scrubber control device or water scrubber 
control device and you conduct a performance test, you must establish 
operating limits according to paragraphs (e)(1)(i) and (ii) of this 
section. If a series of control devices are used, you must establish 
separate operating limits for each device.
    (i) You must establish the minimum value as the operating limit for 
scrubber inlet liquid or recirculating liquid flow rate, as appropriate. 
The minimum value shall be based on the scrubber inlet liquid or 
recirculating liquid flow rate, as appropriate, values measured during 
the performance test.
    (ii) You must establish the minimum and maximum values as the 
operating limits for scrubber effluent pH. The

[[Page 14]]

minimum and maximum values shall be based on the scrubber effluent pH 
values measured during the performance test.
    (2) If you use any other control device and you conduct a 
performance test, you must establish operating limits according to your 
site-specific test plan submitted in accordance with Sec. 
63.7(c)(2)(i). The operating limits shall be based on the operating 
parameter values measured during the performance test. If a series of 
control devices are used, you must establish separate operating limits 
for each device.
    (3) If you do not conduct a performance test for a HCl storage tank 
or HCl transfer operation, you must use engineering assessments and/or 
manufacturer's recommendations to establish the operating limits 
specified in paragraphs (e)(1)(i) and (ii), or (e)(2), of this section.
    (4) As needed in applicability determinations, you must use ASTM 
E224 to determine the HCl concentration in liquid products.



Sec. 63.9025  What are my monitoring installation, operation, and maintenance 
requirements?

    (a) For each operating parameter that you are required by Sec. 
63.9020(d) to monitor, you must install, operate, and maintain each CMS 
according to the requirements in paragraphs (a)(1) through (6) of this 
section.
    (1) You must operate your CMS and collect data at all times the 
process is operating.
    (2) You must collect data from at least four equally spaced periods 
each hour.
    (3) For at least 75 percent of the operating hours in a 24-hour 
period, you must have valid data (as defined in your site-specific 
monitoring plan) for at least 4 equally spaced periods each hour.
    (4) For each hour that you have valid data from at least four 
equally spaced periods, you must calculate the hourly average value 
using all valid data or, where data are collected from an automated CMS, 
using at least one measured value per minute if measured more frequently 
than once per minute.
    (5) You must calculate the daily average using all of the hourly 
averages calculated according to paragraph (a)(4) of this section for 
the 24-hour period.
    (6) You must record the results for each inspection, calibration, 
and validation check as specified in your site-specific monitoring plan.
    (b) For scrubber control devices, you may request approval, in 
accordance with Sec. 63.8(f), to monitor parameters other than those 
specified in Sec. 63.9020(e). In accordance with Sec. 63.8(f), you 
must submit a monitoring plan to the Administrator and the plan must 
meet the requirements in paragraphs (a) and (b)(1) through (3) of this 
section. You must conduct monitoring in accordance with the plan 
submitted to the Administrator unless comments received from the 
Administrator require an alternate monitoring scheme.
    (1) Identify the operating parameter to be monitored to ensure that 
the control or capture efficiency measured during the initial compliance 
test is maintained.
    (2) Discuss why this parameter is appropriate for demonstrating 
ongoing compliance.
    (3) Identify the specific monitoring procedures.
    (c) For any other control device, you must ensure that the CMS is 
operated according to a monitoring plan submitted to the Administrator 
as required by Sec. 63.8(f). The monitoring plan must meet the 
requirements in paragraphs (a) and (c)(1) through (3) of this section. 
You must conduct monitoring in accordance with the plan submitted to the 
Administrator, as amended, unless comments received from the 
Administrator require an alternate monitoring scheme.
    (1) Identify the operating parameter to be monitored to ensure that 
the control or capture efficiency measured during the initial compliance 
test is maintained.
    (2) Discuss why this parameter is appropriate for demonstrating 
ongoing compliance.
    (3) Identify the specific monitoring procedures.

[[Page 15]]



Sec. 63.9030  How do I demonstrate initial compliance with the emission 
limitations and work practice standards?

    (a) You must demonstrate initial compliance with each emission limit 
and work practice standard that applies to you according to Table 4 to 
this subpart.
    (b) You must establish each site-specific operating limit in Table 2 
to this subpart that applies to you according to the requirements in 
Sec. 63.9020 and Table 3 to this subpart.
    (c) You must submit the Notification of Compliance Status containing 
the results of the initial compliance demonstration according to the 
requirements in Sec. 63.9045(e).

                   Continuous Compliance Requirements



Sec. 63.9035  How do I monitor and collect data to demonstrate continuous 
compliance?

    (a) You must monitor and collect data according to this section.
    (b) If you use a caustic scrubber or a water scrubber/absorber to 
meet the emission limits in Table 1 to this subpart, you must keep the 
records specified in paragraphs (b)(1) and (2) of this section to 
support your compliance demonstration.
    (1) Records of daily average scrubber inlet liquid or recirculating 
liquid flow rate, as appropriate.
    (2) Records of the daily average scrubber effluent pH.
    (c) If you use any other control device to meet the emission limits 
in Table 1 to this subpart, you must keep records of the operating 
parameter values identified in your monitoring plan in Sec. 63.9025(c) 
to support your compliance demonstration.
    (d) Except for monitor malfunctions, associated repairs, and 
required quality assurance or control activities (including, as 
applicable, calibration checks and required zero and span adjustments), 
you must monitor continuously (or collect data at all required 
intervals) at all times that the affected source is operating. This 
includes periods of startup, shutdown, or malfunction when the affected 
source is operating. A monitoring malfunction includes, but is not 
limited to, any sudden, infrequent, not reasonably preventable failure 
of the monitoring equipment to provide valid data. Monitoring failures 
that are caused in part by poor maintenance or careless operation are 
not malfunctions.
    (e) You may not use data recorded during monitoring malfunctions, 
associated repairs, and required quality assurance or control activities 
in data averages and calculations used to report emission or operating 
levels, nor may such data be used in fulfilling a minimum data 
availability requirement, if applicable. You must use all the data 
collected during all other periods in assessing the operation of the 
control device and associated control system.



Sec. 63.9040  How do I demonstrate continuous compliance with the emission 
limitations and work practice standards?

    (a) You must demonstrate continuous compliance with each emission 
limit and work practice standard in Table 1 to this subpart that applies 
to you according to Table 4 to this subpart.
    (b) You must demonstrate continuous compliance with each operating 
limit in Table 2 of this subpart that applies to you according to Tables 
4 and 5 to this subpart.
    (c) You must report each instance in which you did not meet an 
emission limit, work practice standard or operating limit in Table 1 or 
2 to this subpart, respectively, that applies to you. This includes 
periods of startup, shutdown, and malfunction. These instances are 
deviations from the emission limitations in this subpart. These 
deviations must be reported according to the requirements in Sec. 
63.9050.
    (d) During periods of startup, shutdown, or malfunction, you must 
operate in accordance with the startup, shutdown, and malfunction plan.
    (e) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations 
that occur during a period of startup, shutdown, or malfunction are not 
violations if you demonstrate to the Administrator's satisfaction that 
you were operating in accordance with the startup, shutdown,

[[Page 16]]

and malfunction plan. The Administrator will determine whether 
deviations that occur during a period of startup, shutdown, or 
malfunction are violations, according to the provisions in Sec. 
63.6(e).

                   Notifications, Reports, and Records



Sec. 63.9045  What notifications must I submit and when?

    (a) You must submit all of the notifications in Sec. Sec. 63.7(b) 
and (c), 63.8(f)(4) and (6), and 63.9 (b) through (h) that apply to you 
by the dates specified.
    (b) As specified in Sec. 63.9(b)(2), if you start up your affected 
source before April 17, 2003, you must submit an Initial Notification 
not later than 120 calendar days after April 17, 2003.
    (c) As specified in Sec. 63.9(b)(4), if you start up your new or 
reconstructed affected source on or after April 17, 2003, you must 
submit the application for construction or reconstruction required by 
Sec. 63.9(b)(1)(iii) in lieu of the initial notification.
    (d) You must submit a notification of intent to conduct a 
performance test at least 60 calendar days before the performance test 
is scheduled to begin, as required in Sec. 63.7(b)(1).
    (e) When you conduct a performance test as specified in Table 3 to 
this subpart, you must submit a Notification of Compliance Status 
according to Sec. 63.9(h)(2)(ii).
    (f) You must submit the Notification of Compliance Status, including 
the performance test results, before the close of business on the 60th 
calendar day following the completion of the performance test according 
to Sec. 63.10(d)(2).
    (g) The Notification of Compliance Status must also include the 
information in paragraphs (g)(1) through (2) of this section that 
applies to you.
    (1) Each operating parameter value averaged over the full period of 
the performance test (for example, average pH).
    (2) Each operating parameter range within which HAP emissions are 
reduced to the level corresponding to meeting the applicable emission 
limits in Table 1 to this subpart.



Sec. 63.9050  What reports must I submit and when?

    (a) You must submit each report in Table 6 to this subpart that 
applies to you.
    (b) Unless the Administrator has approved a different schedule for 
submission of reports under Sec. 63.10(a), you must submit each report 
according to paragraphs (b)(1) through (5) of this section.
    (1) The first compliance report must cover the period beginning on 
the compliance date that is specified for your affected source in Sec. 
63.8995 and ending on June 30 or December 31, whichever date is the 
first date following the end of the first calendar half after the 
compliance date that is specified for your source in Sec. 63.8995.
    (2) The first compliance report must be postmarked or delivered no 
later than July 31 or January 31, whichever date follows the end of the 
first calendar half after the compliance date that is specified for your 
affected source in Sec. 63.8995.
    (3) Each subsequent compliance report must cover the semiannual 
reporting period from January 1 through June 30 or the semiannual 
reporting period from July 1 through December 31.
    (4) Each subsequent compliance report must be postmarked or 
delivered no later than July 31 or January 31, whichever date is the 
first date following the end of the semiannual reporting period.
    (5) For each affected source that is subject to permitting 
regulations pursuant to 40 CFR part 70 or 71, and if the permitting 
authority has established dates for submitting semiannual reports 
pursuant to 40 CFR 70.6 (a)(3)(iii)(A) or 71.6 (a)(3)(iii)(A), you may 
submit the first and subsequent compliance reports according to the 
dates the permitting authority has established instead of according to 
the dates in paragraphs (b)(1) through (4) of this section.
    (c) The compliance report must contain the following information in 
paragraphs (c)(1) through (7) of this section.
    (1) Company name and address.
    (2) Statement by a responsible official with that official's name, 
title, and

[[Page 17]]

signature, certifying the truth, accuracy, and completeness of the 
content of the report.
    (3) Date of report and beginning and ending dates of the reporting 
period.
    (4) If you had a startup, shutdown, or malfunction during the 
reporting period and you took actions consistent with your startup, 
shutdown, and malfunction plan, the compliance report must include the 
information in Sec. 63.10(d)(5)(i).
    (5) If there are no deviations from any emission limitations that 
apply to you, a statement that there were no deviations from the 
emission limitations during the reporting period.
    (6) If there were no periods during which the CMS was out-of-control 
in accordance with the monitoring plan, a statement that there were no 
periods during which the CMS was out-of-control during the reporting 
period.
    (7) Verification that you continue to use the equipment LDAR plan 
and information that explains any periods when the procedures in the 
plan were not followed and the corrective actions were not taken.
    (d) For each deviation from an emission limitation occurring at an 
affected source where you are using a CMS to comply with the emission 
limitation in this subpart, you must include the information in 
paragraphs (c)(1) through (6) of this section and the following 
information in paragraphs (d)(1) through (9) of this section. This 
includes periods of startup, shutdown, and malfunction.
    (1) The date and time that each malfunction started and stopped.
    (2) The date and time that each CMS was inoperative, except for zero 
(low-level) and high-level checks.
    (3) The date, time, and duration that each CMS was out-of-control, 
including the information in Sec. 63.8(c)(8).
    (4) The date and time that each deviation started and stopped, and 
whether each deviation occurred during a period of startup, shutdown, or 
malfunction or during another period.
    (5) A summary of the total duration of the deviation during the 
reporting period and the total duration as a percent of the total source 
operating time during that reporting period.
    (6) A breakdown of the total duration of the deviations during the 
reporting period into those that are due to startup, shutdown, control 
equipment problems, process problems, other known causes, and other 
unknown causes.
    (7) A summary of the total duration of CMS downtime during the 
reporting period, and the total duration of CMS downtime as a percent of 
the total source operating time during that reporting period.
    (8) A brief description of the process units.
    (9) A description of any changes in CMS, processes, or controls 
since the last reporting period.
    (e) Each affected source that has obtained a title V operating 
permit pursuant to 40 CFR part 70 or 71 must report all deviations as 
defined in this subpart in the semiannual monitoring report required by 
40 CFR 70.6(a)(3)(iii)(A) or 71.6(a)(3)(iii)(A). If an affected source 
submits a compliance report pursuant to Table 6 to this subpart along 
with, or as part of, the semiannual monitoring report required by 40 CFR 
70.6(a)(3)(iii)(A) or 71.6(a)(3)(iii)(A), and the compliance report 
includes all required information concerning deviations from any 
emission limitation in this subpart, submission of the compliance report 
shall be deemed to satisfy any obligation to report the same deviations 
in the semiannual monitoring report. However, submission of a compliance 
report shall not otherwise affect any obligation the affected source may 
have to report deviations from permit requirements to the permit 
authority.
    (f) For each startup, shutdown, or malfunction during the reporting 
period that is not consistent with your startup, shutdown, and 
malfunction plan you must submit an immediate startup, shutdown and 
malfunction report. Unless the Administrator has approved a different 
schedule for submission of reports under Sec. 63.10(a), you must submit 
each report according to paragraphs (f)(1) and (2) of this section.
    (1) An initial report containing a description of the actions taken 
for the event must be submitted by fax or telephone within 2 working 
days after starting actions inconsistent with the plan.

[[Page 18]]

    (2) A follow-up report containing the information listed in Sec. 
63.10(d)(5)(ii) must be submitted within 7 working days after the end of 
the event unless you have made alternative reporting arrangements with 
the permitting authority.



Sec. 63.9055  What records must I keep?

    (a) You must keep a copy of each notification and report that you 
submitted to comply with this subpart, including all documentation 
supporting any Initial Notification or Notification of Compliance Status 
that you submitted, as required in Sec. 63.10(b)(2)(xiv).
    (b) You must also keep the following records specified in paragraphs 
(b)(1) through (5) of this section.
    (1) The records in Sec. 63.6(e)(3)(iii) through (v) related to 
startup, shutdown, and malfunction.
    (2) Records of performance tests as required in Sec. 
63.10(b)(2)(viii).
    (3) Records of operating parameter values that are consistent with 
your monitoring plan.
    (4) Records of the date and time that each deviation started and 
stopped and whether the deviation occurred during a period of startup, 
shutdown, or malfunction or during another period.
    (5) Copies of the current versions of the site-specific monitoring 
plan and the equipment LDAR plan. You also must submit copies of these 
plans and any revisions or updates to the Administrator for comment only 
(not for approval).



Sec. 63.9060  In what form and how long must I keep my records?

    (a) Your records must be in a form suitable and readily available 
for expeditious inspection and review, according to Sec. 63.10(b)(1).
    (b) As specified in Sec. 63.10(b)(1), you must keep each record for 
5 years following the date of each occurrence, measurement, maintenance, 
corrective action, report, or record.
    (c) You must keep each record on site, or readily accessible from on 
site through a computer or other means, for at least 2 years after the 
date of each occurrence, measurement, maintenance, corrective action, 
report, or record, according to Sec. 63.10(b)(1). You can keep the 
records off site for the remaining 3 years. Records may be maintained in 
hard copy or computer-readable format including, but not limited to, on 
paper, microfilm, hard disk drive, floppy disk, compact disk, magnetic 
tape, or microfiche.
    (d) You must keep each previous (i.e., superseded) version of the 
site-specific monitoring plan and the LDAR plan for a period of 5 years 
after revision of the plan. If, at any time after adoption of a site-
specific monitoring plan or an LDAR plan, your affected source ceases 
operation or is otherwise no longer subject to the provisions of this 
subpart, you must retain a copy of the most recent plan for 5 years from 
the date your source ceases operation or is no longer subject to this 
subpart.

                   Other Requirements and Information



Sec. 63.9065  What parts of the General Provisions apply to me?

    (a) Table 7 to this subpart shows which parts of the General 
Provisions in Sec. Sec. 63.1 through 63.15 apply to you.



Sec. 63.9070  Who implements and enforces this subpart?

    (a) This subpart can be implemented and enforced by us, the U.S. 
EPA, or a delegated authority such as your State, local, or tribal 
agency. If the U.S. EPA Administrator has delegated authority to your 
State, local, or tribal agency, then that agency, as well as U.S. EPA, 
has the authority to implement and enforce this subpart. You should 
contact your U.S. EPA Regional Office to find out if this subpart is 
delegated to your State, local, or tribal agency.
    (b) In delegating implementation and enforcement authority of this 
subpart to a State, local, or tribal agency under section 40 CFR part 
63, subpart E, the authorities contained in paragraph (c) of this 
section are retained by the Administrator of U.S. EPA and are not 
transferred to the State, local, or tribal agency.
    (c) The authorities in paragraphs (c)(1) through (4) of this section 
that cannot be delegated to State, local, or tribal agencies are as 
follows.
    (1) Approval of alternatives to requirements in Sec. Sec. 63.8980, 
63.8985, 63.8990, 63.8995, and 63.9000.

[[Page 19]]

    (2) Approval of major changes to test methods under Sec. 
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
    (3) Approval of major changes to monitoring under Sec. 63.8(f) and 
as defined in Sec. 63.90.
    (4) Approval of major changes to recordkeeping and reporting under 
Sec. 63.10(f) and as defined in Sec. 63.90.



Sec. 63.9075  What definitions apply to this subpart?

    Terms used in this subpart are defined in the Clean Air Act in 40 
CFR 63.2 and in this section as follows:
    Caustic scrubber control device means any add-on device that mixes 
an aqueous stream or slurry containing a caustic substance with the 
exhaust gases from an HCl process vent, HCl storage tank, or HCl 
transfer operation to control emissions of HCl and/or Cl2.
    Chlor-alkali facility means a facility where chlorine and sodium or 
potassium hydroxide are produced as co-products and hydrogen is produced 
as a by-product in an electrolytic process using either mercury cells, 
diaphragm cells, or membrane cells.
    Continuous monitoring system, for purposes of the final rule, means 
liquid flow monitoring devices that meet the performance specifications 
given in Sec. 63.9025(a); or pH monitoring devices that meet the 
performance specifications given in Sec. 63.9025(a); or other control 
devices as mentioned in 63.9025(a) and (b) or Sec. 63.9025(a) and (c).
    Control device means an add-on device used to reduce HCl and/or 
Cl2 emissions from an HCl process vent, HCl storage tank, or 
HCl transfer operation at an HCl production facility. An HCl production 
unit is not a control device.
    Deviation means any instance in which an affected source subject to 
this subpart, or an owner or operator of such a source:
    (1) Fails to meet any requirement or obligation established by this 
subpart, including but not limited to any emission limitation or work 
practice standard;
    (2) Fails to meet any term or condition that is adopted to implement 
an applicable requirement in this subpart and that is included in the 
operating permit for any affected source required to obtain such a 
permit; or
    (3) Fails to meet any emission limitation or work practice standard 
in this subpart during startup, shutdown, or malfunction, regardless of 
whether or not such failure is permitted by this subpart.
    Emission limitation means any emission limit or operating limit.
    Emission stream means a gaseous stream from an HCl process vent, an 
HCl storage tank, an HCl transfer operation, leaking equipment in HCl 
service, or HCl wastewater operations that is discharged to the 
atmosphere. Gaseous streams from HCl process vents, HCl storage tanks, 
and HCl transfer operations that are routed to another process or 
recycled for reaction or other use (i.e., for pH control) of the HCl 
and/or Cl2 are not emission streams. Gaseous streams from HCl 
transfer operations that are vapor balanced to an HCl storage tank 
subject to this subpart are not emission streams.
    Equipment in HCl service means each pump, compressor, agitator, 
pressure relief device, sampling connection system, open-ended valve or 
line, valve, connector, and instrumentation system that contains 30 
weight percent or greater of liquid HCl or 5 weight percent or greater 
of gaseous HCl at any time.
    HCl process vent means the point of discharge to the atmosphere, or 
point of entry into a control device, of a gaseous stream that 
originates from an HCl production unit. The following points of 
discharge are not HCl process vents:
    (1) A leak from equipment in HCl service subject to this subpart.
    (2) An exit from a control device used to comply with this subpart.
    (3) An HCl storage tank vent or HCl transfer operation vent subject 
to this subpart.
    (4) A HCl wastewater operation vent subject to this subpart.
    (5) A point of discharge from a relief valve.
    (6) A point of discharge from an analyzer.
    HCl production facility is defined in Sec. 63.8985(a)(i).
    HCl production unit means an absorber or other vessel in which a 
liquid

[[Page 20]]

HCl product is manufactured by absorbing gaseous HCl into either water 
or an aqueous HCl solution.
    HCl storage tank means a tank or other vessel that is used to store 
liquid HCl product. Tanks or vessels permanently attached to motor 
vehicles (such as trucks, railcars, barges, or ships) are not HCl 
storage tanks.
    HCl transfer operation means the loading, into a tank truck, 
railcar, ship, or barge, of liquid HCl from a transfer (or loading) rack 
(as defined in this section) for which the predominant use is liquid 
HCl. The predominant use of a transfer (or loading) rack is the material 
that is loaded by the transfer (or loading) rack in the greatest amount.
    HCl wastewater operation means an operation that handles and 
processes water containing HCl that is discarded from an HCl production 
facility.
    Plant site means all contiguous or adjoining property that is under 
common control, including properties that are separated only by a road 
or other public right-of-way. Common control includes properties that 
are owned, leased, or operated by the same entity, parent entity, 
subsidiary, or any combination thereof.
    Research and development facility means laboratory and pilot plant 
operations whose primary purpose is to conduct research and development 
into new processes and products, where the operations are under close 
supervision of technically trained personnel, and the operations are not 
engaged in the manufacture of products for commercial sale, except in a 
de minimis manner.
    Responsible official means responsible official as defined in 40 CFR 
70.2 of this chapter.
    Transfer (or loading) rack means the collection of loading arms and 
loading hoses, at a single loading rack, that are used to fill tank 
trucks, railcars, ships, and/or barges. Transfer rack includes the 
associated pumps, meters, shutoff valves, relief valves, and other 
piping and valves.
    Vapor balanced means connected to a piping system that is designed 
to collect vapors displaced from tank trucks, rail cars, ships, or 
barges during loading, and to route the collected vapors to the storage 
vessel from which the liquid being loaded originated, or to another 
storage vessel connected by a common header.
    Vent means the point of discharge to the atmosphere or to a control 
device from either an HCl process vent, an HCl storage tank, or an HCl 
transfer operation.
    Water scrubber control device means any add-on device that mixes an 
aqueous stream not containing a caustic substance with the exhaust gases 
from an HCl process vent, HCl storage tank, or HCl transfer operation to 
control emissions of HCl and/or Cl2.

 Table 1 to Subpart NNNNN of Part 63--Emission Limits and Work Practice 
                                Standards

    As stated in Sec. 63.9000(a), you must comply with the following 
emission limits and work practice standards for each emission stream 
that is part of an affected source.

------------------------------------------------------------------------
 
 
 
------------------------------------------------------------------------
1. Emission stream from an HCl process   a. Reduce HCl emissions by 99
 vent at an existing source.              percent or greater or to an
                                          outlet concentration of 20 ppm
                                          by volume or less; and
                                         b. Reduce Cl2 emissions by 99
                                          percent or greater or to an
                                          outlet concentration of 100
                                          ppm by volume or less.
----------------------------------------
2. Emission stream from an HCl storage   Reduce HCl emissions by 99
 tank at an existing source.              percent or greater or to an
                                          outlet concentration of 120
                                          ppm by volume or less.
----------------------------------------
3. Emission stream from an HCl transfer  Reduce HCl emissions by 99
 operation at an existing source.         percent or greater or to an
                                          outlet concentration of 120
                                          ppm by volume or less.
----------------------------------------
4. Emission stream from leaking          a. Prepare and operate at all
 equipment in HCl/Cl2 service at          times according to an
 existing sources.                        equipment LDAR plan that
                                          describes in detail the
                                          measures that will be put in
                                          place to detect leaks and
                                          repair them in a timely
                                          fashion; and
                                         b. Submit the plan to the
                                          Administrator for comment only
                                          with your notification of
                                          Compliance Status; and

[[Page 21]]

 
                                         c. You may incorporate by
                                          reference in such plan
                                          existing manuals that describe
                                          the measures in place to
                                          control leaking equipment
                                          emissions required as part of
                                          other federally enforceable
                                          requirements, provided that
                                          all manuals that are
                                          incorporated by reference are
                                          submitted to the
                                          Administrator.
----------------------------------------
5. Emission stream from an HCl process   a. Reduce HCl emissions by 99.4
 vent at a new source.                    percent or greater or to an
                                          outlet concentration of 12 ppm
                                          by volume or less; and
                                         b. Reduce Cl2 emissions by 99.8
                                          percent or greater or to an
                                          outlet concentration of 20 ppm
                                          by volume or less.
----------------------------------------
6. Emission stream from an HCl storage   Reduce HCl emissions by 99.9
 tank at a new source.                    percent or greater or to an
                                          outlet concentration of 12 ppm
                                          by volume or less.
----------------------------------------
7. Emission stream from an HCl transfer  Reduce HCl emissions by 99
 operation at a new source.               percent or greater or to an
                                          outlet concentration of 120
                                          ppm by volume or less.
------------------------------------------------------------------------

          Table 2 to Subpart NNNNN of Part 63--Operating Limits

    As stated in Sec. 63.9000(b), you must comply with the following 
operating limits for each emission stream that is part of an affected 
source that is vented to a control device.

------------------------------------------------------------------------
 
------------------------------------------------------------------------
1. Caustic scrubber or water scrubber/   a. Maintain the daily average
 absorber.                                scrubber inlet liquid or
                                          recirculating liquid flow
                                          rate, as appropriate, above
                                          the operating limit; and
                                         b. Maintain the daily average
                                          scrubber effluent pH within
                                          the operating limits; or
                                         c. Instead of a. and b.,
                                          maintain your operating
                                          parameter(s) within the
                                          operating limits established
                                          according to your monitoring
                                          plan established under Sec.
                                          63.8(f).
----------------------------------------
2. Other type of control device to       Maintain your operating
 which HCl emissions are ducted.          parameter(s) within the limits
                                          established during the
                                          performance test and according
                                          to your monitoring plan.
------------------------------------------------------------------------

 Table 3 to Subpart NNNNN of Part 63--Performance Test Requirements for 
                     HCl Production Affected Sources

    As stated in Sec. 63.9020, you must comply with the following 
requirements for performance tests for HCl production for each affected 
source.

------------------------------------------------------------------------
 
 
 
 
 
 
------------------------------------------------------------------------
1. Select sampling port       a. Method 1 or 1A in  i. If complying with
 location(s) and the number    appendix A to 40      a percent reduction
 of traverse points.           CFR part 60 of this   emission
                               chapter.              limitation,
                                                     sampling sites must
                                                     be located at the
                                                     inlet and outlet of
                                                     the control device
                                                     prior to any
                                                     releases to the
                                                     atmosphere (or, if
                                                     a series of control
                                                     devices are used,
                                                     at the inlet of the
                                                     first control
                                                     device and at the
                                                     outlet of the final
                                                     control device
                                                     prior to any
                                                     releases to the
                                                     atmosphere); or
                                                    ii. If complying
                                                     with an outlet
                                                     concentration
                                                     emission
                                                     limitation, the
                                                     sampling site must
                                                     be located at the
                                                     outlet of the final
                                                     control device and
                                                     prior to any
                                                     releases to the
                                                     atmosphere.
-----------------------------
2. Determine velocity and     Method 2, 2A, 2C,
 volumetric flow rate.         2D, 2F, or 2G in
                               appendix A to 40
                               CFR part 60 of this
                               chapter.
-----------------------------
3. Determine gas molecular    a. Not applicable...  i. Assume a
 weight.                                             molecular weight of
                                                     29 (after moisture
                                                     correction) for
                                                     calculation
                                                     purposes.
-----------------------------

[[Page 22]]

 
4. Measure moisture content   Method 4 in appendix
 of the stack gas.             A to 40 CFR part 60
                               of this chapter.
-----------------------------
5. Measure HCl concentration  a. Method 26A in      i. An owner or
 and Cl2 concentration from    Appendix A to 40      operator may be
 HCl process vents.            CFR part 60 of this   exempted from
                               chapter.              measuring the Cl2
                                                     concentration from
                                                     an HCl process vent
                                                     provided that a
                                                     demonstration that
                                                     Cl2 is not likely
                                                     to be present in
                                                     the stream is
                                                     submitted as part
                                                     of the site-
                                                     specific test plan
                                                     required by Sec.
                                                     63.9020(a)(2). This
                                                     demonstration may
                                                     be based on process
                                                     knowledge,
                                                     engineering
                                                     judgement, or
                                                     previous test
                                                     results.
-----------------------------
6. Establish operating
 limits with which you will
 demonstrate continuous
 compliance with the
 emission limits in Table 1
 to this subpart, in
 accordance with Sec.
 63.9020(e)(1) or (2).
------------------------------------------------------------------------

 Table 4 to Subpart NNNNN of Part 63--Initial Compliance With Emission 
                 Limitations and Work Practice Standards

    As stated in Sec. 63.9030, you must comply with the following 
requirements to demonstrate initial compliance with the applicable 
emission limits for each affected source vented to a control device and 
each work practice standard.

------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. HCl process vent and each  a. In Table 1 to      i. The average
 HCl storage tank and HCl      this subpart.         percent reduction
 transfer operation for                              of HCl and Cl2 (if
 which you are conducting a                          applicable),
 performance test.                                   measured over the
                                                     period of the
                                                     performance test
                                                     conducted according
                                                     to Table 3 of this
                                                     subpart and
                                                     determined in
                                                     accordance with
                                                     Sec. 63.9020(b),
                                                     is greater than or
                                                     equal to the
                                                     applicable percent
                                                     reduction emission
                                                     limitation
                                                     specified in Table
                                                     1 of this subpart;
                                                     or
                                                    ii. The average HCl
                                                     and Cl2 (if
                                                     applicable)
                                                     concentration,
                                                     measured over the
                                                     period of the
                                                     performance test
                                                     conducted according
                                                     to Table 3 of this
                                                     subpart, is less
                                                     than or equal to
                                                     the applicable
                                                     concentration
                                                     emission limitation
                                                     specified in Table
                                                     1 of this subpart.
-----------------------------
2. HCl storage tank and HCl   a. In Table 1 to      i. The percent
 transfer operation for        this subpart.         reduction of HCl,
 which you are preparing a                           demonstrated by a
 design evaluation in lieu                           design evaluation
 of conducting a performance                         prepared in
 test.                                               accordance with
                                                     Sec. 63.9020(c),
                                                     is greater than or
                                                     equal to the
                                                     applicable percent
                                                     reduction emission
                                                     limitation
                                                     specified in Table
                                                     1 of this subpart;
                                                     or
                                                    ii. The HCl
                                                     concentration,
                                                     demonstrated by a
                                                     design evaluation
                                                     prepared in
                                                     accordance with
                                                     Sec. 63.9020(c),
                                                     is less than or
                                                     equal to the
                                                     applicable
                                                     concentration
                                                     emission limitation
                                                     specified in Table
                                                     1 of this subpart.
-----------------------------
3. Leaking equipment........  a. In Table 1 to      i. You certify in
                               this subpart.         your Notification
                                                     of Compliance
                                                     Status that you
                                                     have developed and
                                                     implemented your
                                                     LDAR plan and
                                                     submitted it to the
                                                     Administrator for
                                                     comment only.
------------------------------------------------------------------------


[[Page 23]]

Table 5 to Subpart NNNNN of Part 63--Continuous Compliance With Emission 
                 Limitations and Work Practice Standards

    As stated in Sec. 63.9040, you must comply with the following 
requirements to demonstrate continuous compliance with the applicable 
emission limitations for each affected source vented to a control device 
and each work practice standard.

------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. Affected source using a    a. In Tables 1 and 2  i. Collecting the
 caustic scrubber or water     to this subpart.      scrubber inlet
 scrubber/absorber.                                  liquid or
                                                     recirculating
                                                     liquid flow rate,
                                                     as appropriate, and
                                                     effluent pH
                                                     monitoring data
                                                     according to Sec.
                                                     63.9025, consistent
                                                     with your
                                                     monitoring plan;
                                                     and
                                                    ii. Reducing the
                                                     data to 1-hour and
                                                     daily block
                                                     averages according
                                                     to the requirements
                                                     in Sec. 63.9025;
                                                     and
                                                    iii. Maintaining the
                                                     daily average
                                                     scrubber inlet
                                                     liquid or
                                                     recirculating
                                                     liquid flow rate,
                                                     as appropriate,
                                                     above the operating
                                                     limit; and
                                                    iv. Maintaining the
                                                     daily average
                                                     scrubber effluent
                                                     pH within the
                                                     operating limits.
-----------------------------
2. Affected source using any  a. In Tables 1 and 2  i. Conducting
 other control device.         to this subpart.      monitoring
                                                     according to your
                                                     monitoring plan
                                                     established under
                                                     Sec. 63.8(f) in
                                                     accordance with
                                                     Sec. 63.9025(c);
                                                     and
                                                    ii. Collecting the
                                                     parameter data
                                                     according to your
                                                     monitoring plan
                                                     established under
                                                     Sec. 63.8(f); and
                                                    iii. Reducing the
                                                     data to 1-hour and
                                                     daily block
                                                     averages according
                                                     to the requirements
                                                     in Sec. 63.9025;
                                                     and
                                                    iv. Maintaining the
                                                     daily average
                                                     parameter values
                                                     within the
                                                     operating limits
                                                     established
                                                     according to your
                                                     monitoring plan
                                                     established under
                                                     Sec. 63.8(f).
-----------------------------
3. Leaking equipment          a. In Table 1 to      i. Verifying that
 affected source.              this subpart.         you continue to use
                                                     a LDAR plan; and
                                                    ii. Reporting any
                                                     instances where you
                                                     deviated from the
                                                     plan and the
                                                     corrective actions
                                                     taken.
------------------------------------------------------------------------

      Table 6 to Subpart NNNNN of Part 63--Requirements for Reports

    As stated in Sec. 63.9050(a), you must submit a compliance report 
that includes the information in Sec. 63.9050(c) through (e) as well as 
the information in the following table. You must also submit startup, 
shutdown, and malfunction (SSM) reports according to the requirements in 
Sec. 63.9050(f) and the following:

------------------------------------------------------------------------
 
 
------------------------------------------------------------------------
1. There are no deviations from any      There were no deviations from
 emission limitations that apply to you.  any emission limitations that
                                          apply to you during the
                                          reporting period.
----------------------------------------
2. There were no periods during which    There were no periods during
 the operating parameter monitoring       which the CMS were out-of-
 systems were out-of-control in           control during the reporting
 accordance with the monitoring plan.     period.
----------------------------------------
3. There was a deviation from any        Contains the information in
 emission limitation during the           Sec. 63.9050(d).
 reporting period.
----------------------------------------
4. There were periods during which the   Contains the information in
 operating parameter monitoring systems   Sec. 63.9050(d).
 were out-of-control in accordance with
 the monitoring plan.
----------------------------------------
5. There was a SSM during the reporting  Contains the information in
 period that is not consistent with       Sec. 63.9050(f).
 your SSM plan.
----------------------------------------

[[Page 24]]

 
6. There were periods when the           Contains the information in
 procedures in the LDAR plan were not     Sec. 63.9050(c)(7).
 followed.
------------------------------------------------------------------------

Table 7 to Subpart NNNNN of Part 63--Applicability of General Provisions 
                            to Subpart NNNNN

    As stated in Sec. 63.9065, you must comply with the applicable 
General Provisions requirements according to the following:

----------------------------------------------------------------------------------------------------------------
 
----------------------------------------------------------------------------------------------------------------
Sec. 63.1.......................  Initial applicability  Yes.                             ....................
                                     determination;
                                     applicability after
                                     standard
                                     established; permit
                                     requirements;
                                     extensions;
                                     notifications.
-----------------------------------
Sec. 63.2.......................  Definitions..........  Yes............................  Additional
                                                                                             definitions are
                                                                                             found in Sec.
                                                                                             63.9075.
-----------------------------------
Sec. 63.3.......................  Units and              Yes.                             ....................
                                     abbreviations.
-----------------------------------
Sec. 63.4.......................  Prohibited             Yes.                             ....................
                                     activities;
                                     compliance date;
                                     circumvention,
                                     severability.
-----------------------------------
Sec. 63.5.......................  Construction/          Yes.                             ....................
                                     reconstruction
                                     applicability;
                                     applications;
                                     approvals.
-----------------------------------
Sec. 63.6(a)....................  Compliance with        Yes.                             ....................
                                     standards and
                                     maintenance
                                     requirements--applic
                                     ability.
-----------------------------------
Sec. 63.6(b)(1)-(4).............  Compliance dates for   Yes............................  Sec. 63.8995
                                     new or reconstructed                                    specifies
                                     sources.                                                compliance dates.
-----------------------------------
Sec. 63.6(b)(5).................  Notification if        Yes.                             ....................
                                     commenced
                                     construction or
                                     reconstruction after
                                     proposal.
-----------------------------------
Sec. 63.6(b)(6).................  [Reserved]...........  Yes.                             ....................
-----------------------------------
Sec. 63.6(b)(7).................  Compliance dates for   Yes............................  Sec. 63.8995
                                     new or reconstructed                                    specifies
                                     area sources that                                       compliance dates.
                                     become major.
-----------------------------------
Sec. 63.6(c)(1)-(2).............  Compliance dates for   Yes............................  Sec. 63.8995
                                     existing sources.                                       specifies
                                                                                             compliance dates.
-----------------------------------
Sec. 63.6(c)(3)-(4).............  [Reserved]...........  Yes.                             ....................
-----------------------------------
Sec. 63.6(c)(5).................  Compliance dates for   Yes............................  Sec. 63.8995
                                     existing area                                           specifies
                                     sources that become                                     compliance dates.
                                     major.
-----------------------------------
Sec. 63.6(d)....................  [Reserved]...........  Yes.                             ....................
-----------------------------------
Sec. 63.6(e)(1)-(2).............  Operation and          Yes.                             ....................
                                     maintenance
                                     requirements.
-----------------------------------
Sec. 63.6(e)(3).................  SSM plans............  Yes.                             ....................
-----------------------------------
Sec. 63.6(f)(1).................  Compliance except      Yes.                             ....................
                                     during SSM.
-----------------------------------
Sec. 63.6(f)(2)-(3).............  Methods for            Yes.                             ....................
                                     determining
                                     compliance.
-----------------------------------
Sec. 63.6(g)....................  Use of an alternative  Yes.                             ....................
                                     nonopacity emission
                                     standard.
-----------------------------------

[[Page 25]]

 
Sec. 63.6(h)....................  Compliance with        No.............................  Subpart NNNNN does
                                     opacity/visible                                         not specify opacity
                                     emission standards.                                     or visible emission
                                                                                             standards.
-----------------------------------
Sec. 63.6(i)....................  Extension of           Yes.                             ....................
                                     compliance with
                                     emission standards.
-----------------------------------
Sec. 63.6(j)....................  Presidential           Yes.                             ....................
                                     compliance exemption.
-----------------------------------
Sec. 63.7(a)(1)-(2).............  Performance test       Yes............................  Except for existing
                                     dates.                                                  affected sources as
                                                                                             specified in Sec.
                                                                                             63.9010(b).
-----------------------------------
Sec. 63.7(a)(3).................  Administrator's Clean  Yes.                             ....................
                                     Air Act section 114
                                     authority to require
                                     a performance test.
-----------------------------------
Sec. 63.7(b)....................  Notification of        Yes.                             ....................
                                     performance test and
                                     rescheduling.
-----------------------------------
Sec. 63.7(c)....................  Quality assurance      Yes.                             ....................
                                     program and site-
                                     specific test plans.
-----------------------------------
Sec. 63.7(d)....................  Performance testing    Yes.                             ....................
                                     facilities.
-----------------------------------
Sec. 63.7(e)(1).................  Conditions for         Yes.                             ....................
                                     conducting
                                     performance tests.
-----------------------------------
Sec. 63.7(f)....................  Use of an alternative  Yes.                             ....................
                                     test method.
-----------------------------------
Sec. 63.7(g)....................  Performance test data  Yes.                             ....................
                                     analysis,
                                     recordkeeping, and
                                     reporting.
-----------------------------------
Sec. 63.7(h)....................  Waiver ofperformance   Yes.                             ....................
                                     tests.
-----------------------------------
Sec. 63.8(a)(1)-(3).............  Applicability of       Yes............................  Additional
                                     monitoring                                              monitoring
                                     requirements.                                           requirements are
                                                                                             found in Sec.
                                                                                             63.9005(d) and
                                                                                             63.9035.
-----------------------------------
Sec. 63.8(a)(4).................  Monitoring with        No.............................  Subpart NNNNN does
                                     flares.                                                 not refer directly
                                                                                             or indirectly to
                                                                                             Sec. 63.11.
-----------------------------------
Sec. 63.8(b)....................  Conduct of monitoring  Yes.                             ....................
                                     and procedures when
                                     there are multiple
                                     effluents and
                                     multiple monitoring
                                     systems.
-----------------------------------
Sec. 63.8(c)(1)-(3).............  Continuous monitoring  Yes............................  Applies as modified
                                     system O&M.                                             by Sec.
                                                                                             63.9005(d).
-----------------------------------
Sec. 63.8(c)(4).................  Continuous monitoring  Yes............................  Applies as modified
                                     system requirements                                     by Sec.
                                     during breakdown,                                       63.9005(d).
                                     out-of-control,
                                     repair, maintenance,
                                     and high-level
                                     calibration drifts.
-----------------------------------
Sec. 63.8(c)(5).................  Continuous opacity     No.............................  Subpart NNNNN does
                                     monitoring system                                       not have opacity or
                                     (COMS) minimum                                          visible emmission
                                     procedures.                                             standards.
-----------------------------------
Sec. 63.8(c)(6).................  Zero and high level    Yes............................  Applies as modified
                                     calibration checks.                                     by Sec.
                                                                                             63.9005(d).
-----------------------------------
Sec. 63.8(c)(7)(8)..............  Out-of-control         Yes.                             ....................
                                     periods, including
                                     reporting.
-----------------------------------
Sec. 63.8(d)-(e)................  Quality control        No.............................  Applies as modified
                                     program and CMS                                         by Sec.
                                     performance                                             63.9005(d).
                                     evaluation.
-----------------------------------

[[Page 26]]

 
Sec. 63.8(f)(1)-(5).............  Use of an alternative  Yes.                             ....................
                                     monitoring method.
-----------------------------------
Sec. 63.8(f)(6).................  Alternative to         No.............................  Only applies to
                                     relative accuracy                                       sources that use
                                     test.                                                   continuous
                                                                                             emissions
                                                                                             monitoring systems
                                                                                             (CEMS).
-----------------------------------
Sec. 63.8(g)....................  Data reduction.......  Yes............................  Applies as modified
                                                                                             by Sec.
                                                                                             63.9005(d).
-----------------------------------
Sec. 63.9(a)....................  Notification           Yes.                             ....................
                                     requirements--applic
                                     ability.
-----------------------------------
Sec. 63.9(b)....................  Initial notifications  Yes............................  Except Sec.
                                                                                             63.9045(c) requires
                                                                                             new or
                                                                                             reconstructed
                                                                                             affected sources to
                                                                                             submit the
                                                                                             application for
                                                                                             construction or
                                                                                             reconstruction
                                                                                             required by Sec.
                                                                                             63.9(b)(1) (iii) in
                                                                                             lieu of the initial
                                                                                             notification.
-----------------------------------
Sec. 63.9(c)....................  Request for            Yes.                             ....................
                                     compliance extension.
-----------------------------------
Sec. 63.9(d)....................  Notification that a    Yes.                             ....................
                                     new source is
                                     subject to special
                                     compliance
                                     requirements.
-----------------------------------
Sec. 63.9(e)....................  Notification of        Yes.                             ....................
                                     performance test.
-----------------------------------
Sec. 63.9(f)....................  Notification of        No.............................  Subpart NNNNN does
                                     visible emissions/                                      not have opacity or
                                     opacity test.                                           visible emission
                                                                                             standards.
-----------------------------------
Sec. 63.9(g)(1).................  Additional CMS         Yes.                             ....................
                                     notifications--date
                                     of CMS performance
                                     evaluation.
-----------------------------------
Sec. 63.9(g)(2).................  Use of COMS data.....  No.............................  Subpart NNNNN does
                                                                                             not require the use
                                                                                             of COMS.
-----------------------------------
Sec. 63.9(g)(3).................  Alternative to         No.............................  Applies only to
                                     relative accuracy                                       sources with CEMS.
                                     testing.
-----------------------------------
Sec. 63.9(h)....................  Notification of        Yes.                             ....................
                                     compliance status.
-----------------------------------
Sec. 63.9(i)....................  Adjustment of          Yes.                             ....................
                                     submittal deadlines.
-----------------------------------
Sec. 63.9(j)....................  Change in previous     Yes.                             ....................
                                     information.
-----------------------------------
Sec. 63.10(a)...................  Recordkeeping/         Yes.                             ....................
                                     reporting
                                     applicability.
-----------------------------------
Sec. 63.10(b)(1)................  General recordkeeping  Yes............................  Sec. Sec. 63.9055
                                     requirements.                                           and 63.9060 specify
                                                                                             additional
                                                                                             recordkeeping
                                                                                             requirements.
-----------------------------------
Sec. 63.10(b)(2)(i)-(xi)........  Records related to     Yes.                             ....................
                                     SSM periods and CMS.
-----------------------------------
Sec. 63.10(b)(2)(xii)...........  Records when under     Yes.                             ....................
                                     waiver.
-----------------------------------
Sec. 63.10(b)(2)(xiii)..........  Records when using     No.............................  Applies only to
                                     alternative to                                          sources with CEMS.
                                     relative accuracy
                                     test.
-----------------------------------
Sec. 63.10(b)(2)(xiv)...........  All documentation      Yes.                             ....................
                                     supporting initial
                                     notification and
                                     notification of
                                     compliance status.
-----------------------------------

[[Page 27]]

 
Sec. 63.10(b)(3)................  Recordkeeping          Yes.                             ....................
                                     requirements for
                                     applicability
                                     determinations.
-----------------------------------
Sec. 63.10(c)...................  Additional             Yes............................  Applies as modified
                                     recordkeeping                                           by Sec.
                                     requirements for                                        63.9005(d).
                                     sources with CMS.
-----------------------------------
Sec. 63.10(d)(1)................  General reporting      Yes............................  Sec. 63.9050
                                     requirements.                                           specifies
                                                                                             additional
                                                                                             reporting
                                                                                             requirements.
-----------------------------------
Sec. 63.10(d)(2)................  Performance test       Yes.                             ....................
                                     results.
-----------------------------------
Sec. 63.10(d)(3)................  Opacity or visible     No.............................  Subpart NNNNN does
                                     emissions                                               not specify opacity
                                     observations.                                           or visible emission
                                                                                             standards.
-----------------------------------
Sec. 63.10(d)(4)................  Progress reports for   Yes.                             ....................
                                     sources with
                                     compliance
                                     extensions.
-----------------------------------
Sec. 63.10(d)(5)................  SSM reports..........  Yes.                             ....................
-----------------------------------
Sec. 63.10(e)(1)................  Additional CMS         Yes............................  Applies as modified
                                     reports--general.                                       by Sec.
                                                                                             63.9005(d).
-----------------------------------
Sec. 63.10(e)(2)(i).............  Results of CMS         Yes............................  Applies as modified
                                     performance                                             by Sec.
                                     evaluations.                                            63.9005(d).
-----------------------------------
Sec. 63.10(e)(2)(ii)............  Results of COMS        No.............................  Subpart NNNNN does
                                     performance                                             not require the use
                                     evaluations.                                            of COMS.
-----------------------------------
Sec. 63.10(e)(3)................  Excess emissions/CMS   Yes.                             ....................
                                     performance reports.
-----------------------------------
Sec. 63.10(e)(4)................  Continuous opacity     No.............................  Subpart NNNNN does
                                     monitoring system                                       not require the use
                                     data reports.                                           of COMS.
-----------------------------------
Sec. 63.10(f)...................  Recordkeeping/         Yes.                             ....................
                                     reporting waiver.
-----------------------------------
Sec. 63.11......................  Control device         No.............................  Facilities subject
                                     requirements--applic                                    to subpart NNNNN do
                                     ability.                                                not use flares as
                                                                                             control devices.
-----------------------------------
Sec. 63.12......................  State authority and    Yes............................  Sec. 63.9070 lists
                                     delegations.                                            those sections of
                                                                                             subparts NNNNN and
                                                                                             A that are not
                                                                                             delegated.
-----------------------------------
Sec. 63.13......................  Addresses............  Yes.                             ....................
-----------------------------------
Sec. 63.14......................  Incorporation by       Yes............................  Subpart NNNNN does
                                     reference.                                              not incorporate any
                                                                                             material by
                                                                                             reference.
-----------------------------------
Sec. 63.15......................  Availability of        Yes.                             ....................
                                     information/
                                     confidentiality.
----------------------------------------------------------------------------------------------------------------



                        Subpart OOOOO [Reserved]



 Subpart PPPPP_National Emission Standards for Hazardous Air Pollutants 
                      for Engine Test Cells/Stands

    Source: 68 FR 28785, May 27, 2003, unless otherwise noted.

                        What This Subpart Covers



Sec. 63.9280  What is the purpose of subpart PPPPP?

    This subpart PPPPP establishes national emission standards for 
hazardous air pollutants (NESHAP) for engine test cells/stands located 
at major sources of hazardous air pollutants (HAP) emissions. This 
subpart also establishes requirements to demonstrate initial and 
continuous compliance with

[[Page 28]]

the emission limitations contained in this NESHAP.



Sec. 63.9285  Am I subject to this subpart?

    You are subject to this subpart if you own or operate an engine test 
cell/stand that is located at a major source of HAP emissions.
    (a) An engine test cell/stand is any apparatus used for testing 
uninstalled stationary or uninstalled mobile (motive) engines.
    (b) An uninstalled engine is an engine that is not installed in, or 
an integrated part of, the final product.
    (c) A major source of HAP emissions is a plant site that emits or 
has the potential to emit any single HAP at a rate of 10 tons (9.07 
megagrams) or more per year or any combination of HAP at a rate of 25 
tons (22.68 megagrams) or more per year.



Sec. 63.9290  What parts of my plant does this subpart cover?

    This subpart applies to each new, reconstructed, or existing 
affected source.
    (a) Affected source. An affected source is the collection of all 
equipment and activities associated with engine test cells/stands used 
for testing uninstalled stationary or uninstalled mobile (motive) 
engines located at a major source of HAP emissions.
    (1) Existing affected source. An affected source is existing if you 
commenced construction or reconstruction of the affected source on or 
before May 14, 2002. A change in ownership of an existing affected 
source does not make that affected source a new or reconstructed 
affected source.
    (2) New affected source. An affected source is new if you commenced 
construction of the affected source after May 14, 2002.
    (3) Reconstructed affected source. An affected source is 
reconstructed if you meet the definition of reconstruction in Sec. 63.2 
of subpart A of this part and reconstruction is commenced after May 14, 
2002. Changes made to an existing affected source primarily for the 
purpose of complying with revisions to engine testing requirements under 
40 CFR parts 80, 86, 89, 90, 91, or 92 are not considered a modification 
or reconstruction. In addition, passive measurement and control 
instrumentation and electronics are not included as part of any affected 
source reconstruction evaluation.
    (b) Existing affected sources do not have to meet the requirements 
of this subpart and of subpart A of this part.
    (c) Any portion of a new or reconstructed affected source located at 
a major source that is used exclusively for testing internal combustion 
engines with rated power of less than 25 horsepower (hp) (19 
kilowatts(kW)) does not have to meet the requirements of this subpart 
and of subpart A of this part except for the initial notification 
requirements of Sec. 63.9345(b).
    (d) Any portion of a new or reconstructed affected source located at 
a major source that meets any of the criteria specified in paragraphs 
(d)(1) through (4) of this section does not have to meet the 
requirements of this subpart and of subpart A of this part.
    (1) Any portion of the affected source used exclusively for testing 
combustion turbine engines.
    (2) Any portion of the affected source used exclusively for testing 
rocket engines.
    (3) Any portion of the affected source used in research and teaching 
activities at facilities that are not engaged in the development of 
engines or engine test services for commercial purposes.
    (4) Any portion of the affected source operated to test or evaluate 
fuels (such as knock engines), transmissions, or electronics.



Sec. 63.9295  When do I have to comply with this subpart?

    (a) Affected sources.
    (1) If you start up your new or reconstructed affected source before 
May 27, 2003, you must comply with the emission limitations in this 
subpart no later than May 27, 2003.
    (2) If you start up your new or reconstructed affected source on or 
after May 27, 2003, you must comply with the emission limitations in 
this subpart upon startup.
    (b) Area sources that become major sources. If your new or 
reconstructed affected source is located at an area source that 
increases its emissions or

[[Page 29]]

its potential to emit such that it becomes a major source of HAP, your 
new or reconstructed affected source must be in compliance with this 
subpart when the area source becomes a major source.
    (c) You must meet the notification requirements in Sec. 63.9345 and 
in 40 CFR part 63, subpart A.

                          Emission Limitations



Sec. 63.9300  What emission limitations must I meet?

    For each new or reconstructed affected source that is used in whole 
or in part for testing internal combustion engines with rated power of 
25 hp (19 kW) or more and that is located at a major source, you must 
comply with the emission limitations in Table 1 to this subpart. (Tables 
are found at the end of this subpart.)



Sec. 63.9301  What are my options for meeting the emission limits?

    You may use either a continuous parameter monitoring system (CPMS) 
or a continuous emission monitoring system (CEMS) to demonstrate 
compliance with the emission limitations. Continuous monitoring systems 
must meet the requirements in Sec. 63.9306 (CPMS) and Sec. 63.9307 
(CEMS).



Sec. 63.9302  What operating limits must I meet?

    (a) For any new or reconstructed affected source on which you use 
add-on controls, you must meet the operating limits specified in Table 2 
to this subpart. These operating limits must be established during the 
performance test according to the requirements in Sec. 63.9324. You 
must meet the operating limits at all times after you establish them.
    (b) If you use an add-on control device other than those listed in 
Table 2 to this subpart, or wish to monitor an alternative parameter and 
comply with a different operating limit, you must apply to the 
Administrator for approval of alternative monitoring under Sec. 
63.8(f).

                     General Compliane Requirements



Sec. 63.9305  What are my general requirements for complying with 
this subpart?

    (a) You must be in compliance with the emission limitation that 
applies to you at all times, except during periods of startup, shutdown, 
or malfunction (SSM) of your control device or associated monitoring 
equipment.
    (b) If you must comply with the emission limitation, you must 
operate and maintain your engine test cell/stand, air pollution control 
equipment, and monitoring equipment in a manner consistent with good air 
pollution control practices for minimizing emissions at all times.
    (c) You must develop and implement a written SSM plan (SSMP) for 
emission control devices and associated monitoring equipment according 
to the provisions in Sec. 63.6(e)(3). The plan will apply only to 
emission control devices, and not to engine test cells/stands.



Sec. 63.9306  What are my continuous parameter monitoring system 
(CPMS) installation, operation, and maintenance requirements?

    (a) General. You must install, operate, and maintain each CPMS 
specified in paragraphs (c) and (d) of this section according to 
paragraphs (a)(1) through (7) of this section. You must install, 
operate, and maintain each CPMS specified in paragraph (b) of this 
section according to paragraphs (a)(3) through (5) of this section.
    (1) The CPMS must complete a minimum of one cycle of operation for 
each successive 15-minute period. You must have a minimum of four 
equally spaced successive cycles of CPMS operation in 1 hour.
    (2) You must determine the average of all recorded readings for each 
successive 3-hour period of the emission capture system and add-on 
control device operation.
    (3) You must record the results of each inspection, calibration, and 
validation check of the CPMS.
    (4) You must maintain the CPMS at all times and have available 
necessary parts for routine repairs of the monitoring equipment.
    (5) You must operate the CPMS and collect emission capture system 
and

[[Page 30]]

add-on control device parameter data at all times that an engine test 
cell/stand is operating, except during monitoring malfunctions, 
associated repairs, and required quality assurance or control activities 
(including, if applicable, calibration checks and required zero and span 
adjustments).
    (6) You must not use emission capture system or add-on control 
device parameter data recorded during monitoring malfunctions, 
associated repairs, out-of-control periods, or required quality 
assurance or control activities when calculating data averages. You must 
use all the data collected during all other periods in calculating the 
data averages for determining compliance with the emission capture 
system and add-on control device operating limits.
    (7) A monitoring malfunction is any sudden, infrequent, not 
reasonably preventable failure of the CPMS to provide valid data. 
Monitoring failures that are caused in part by poor maintenance or 
careless operation are not malfunctions. Any period for which the 
monitoring system is out-of-control and data are not available for 
required calculations is a deviation from the monitoring requirements.
    (b) Capture system bypass line. You must meet the requirements of 
paragraphs (b)(1) and (2) of this section for each emission capture 
system that contains bypass lines that could divert emissions away from 
the add-on control device to the atmosphere.
    (1) You must monitor or secure the valve or closure mechanism 
controlling the bypass line in a nondiverting position in such a way 
that the valve or closure mechanism cannot be opened without creating a 
record that the valve was opened. The method used to monitor or secure 
the valve or closure mechanism must meet one of the requirements 
specified in paragraphs (b)(1)(i) through (iv) of this section.
    (i) Flow control position indicator. Install, calibrate, maintain, 
and operate according to the manufacturer's specifications a flow 
control position indicator that takes a reading at least once every 15 
minutes and provides a record indicating whether the emissions are 
directed to the add-on control device or diverted from the add-on 
control device. The time of occurrence and flow control position must be 
recorded, as well as every time the flow direction is changed. The flow 
control position indicator must be installed at the entrance to any 
bypass line that could divert the emissions away from the add-on control 
device to the atmosphere.
    (ii) Car-seal or lock-and-key valve closures. Secure any bypass line 
valve in the closed position with a car-seal or a lock-and-key type 
configuration. You must visually inspect the seal or closure mechanism 
at least once every month to ensure that the valve is maintained in the 
closed position, and the emissions are not diverted away from the add-on 
control device to the atmosphere.
    (iii) Valve closure monitoring. Ensure that any bypass line valve is 
in the closed (nondiverting) position through monitoring of valve 
position at least once every 15 minutes. You must inspect the monitoring 
system at least once every month to verify that the monitor will 
indicate valve position.
    (iv) Automatic shutdown system. Use an automatic shutdown system in 
which the engine testing operation is stopped when flow is diverted by 
the bypass line away from the add-on control device to the atmosphere 
when an engine test cell/stand is operating. You must inspect the 
automatic shutdown system at least once every month to verify that it 
will detect diversions of flow and shut down the engine test cell/stand 
in operation.
    (2) If any bypass line is opened, you must include a description of 
why the bypass line was opened and the length of time it remained open 
in the semiannual compliance reports required in Sec. 63.9350.
    (c) Thermal oxidizers and catalytic oxidizers. If you are using a 
thermal oxidizer or catalytic oxidizer as an add-on control device, you 
must comply with the requirements in paragraphs (c)(1) through (3) of 
this section.
    (1) For a thermal oxidizer, install a gas temperature monitor in the 
firebox of the thermal oxidizer or in the duct immediately downstream of 
the firebox before any substantial heat exchange occurs.
    (2) For a catalytic oxidizer, you must install a gas temperature 
monitor in

[[Page 31]]

the gas stream immediately before the catalyst bed, and if you 
established operating limits according to Sec. 63.9324(b)(1) and (2), 
also install a gas temperature monitor in the gas stream immediately 
after the catalyst bed.
    (i) If you establish operating limits according to Sec. 
63.9324(b)(1) and (2), then you must install the gas temperature 
monitors both upstream and downstream of the catalyst bed. The 
temperature monitors must be in the gas stream immediately before and 
after the catalyst bed to measure the temperature difference across the 
bed.
    (ii) If you establish operating limits according to Sec. 
63.9324(b)(3) and (4), then you must install a gas temperature monitor 
upstream of the catalyst bed. The temperature monitor must be in the gas 
stream immediately before the catalyst bed to measure the temperature.
    (3) For all thermal oxidizers and catalytic oxidizers, you must meet 
the requirements in paragraphs (a) and (c)(3)(i) through (vii) of this 
section for each gas temperature monitoring device.
    (i) Locate the temperature sensor in a position that provides a 
representative temperature.
    (ii) Use a temperature sensor with a measurement sensitivity of 4 
degrees Fahrenheit or 0.75 percent of the temperature value, whichever 
is larger.
    (iii) Shield the temperature sensor system from electromagnetic 
interference and chemical contaminants.
    (iv) If a gas temperature chart recorder is used, it must have a 
measurement sensitivity in the minor division of at least 20 degrees 
Fahrenheit.
    (v) Perform an electronic calibration at least semiannually 
according to the procedures in the manufacturer's owner's manual. 
Following the electronic calibration, you must conduct a temperature 
sensor validation check in which a second or redundant temperature 
sensor placed near the process temperature sensor must yield a reading 
within 30 degrees Fahrenheit of the process temperature sensor reading.
    (vi) Conduct calibration and validation checks anytime the sensor 
exceeds the manufacturer's specified maximum operating temperature range 
or install a new temperature sensor.
    (vii) At least monthly, inspect components for integrity and 
electrical connections for continuity, oxidation, and galvanic 
corrosion.
    (d) Emission capture systems. The capture system monitoring system 
must comply with the applicable requirements in paragraphs (d)(1) and 
(2) of this section.
    (1) For each flow measurement device, you must meet the requirements 
in paragraphs (a) and (d)(1)(i) through (iv) of this section.
    (i) Locate a flow sensor in a position that provides a 
representative flow measurement in the duct from each capture device in 
the emission capture system to the add-on control device.
    (ii) Reduce swirling flow or abnormal velocity distributions due to 
upstream and downstream disturbances.
    (iii) Conduct a flow sensor calibration check at least semiannually.
    (iv) At least monthly, inspect components for integrity, electrical 
connections for continuity, and mechanical connections for leakage.
    (2) For each pressure drop measurement device, you must comply with 
the requirements in paragraphs (a) and (d)(2)(i) through (vi) of this 
section.
    (i) Locate the pressure sensor(s) in or as close to a position that 
provides a representative measurement of the pressure drop across each 
opening you are monitoring.
    (ii) Minimize or eliminate pulsating pressure, vibration, and 
internal and external corrosion.
    (iii) Check pressure tap pluggage daily.
    (iv) Using an inclined manometer with a measurement sensitivity of 
0.0002 inch water, check gauge calibration quarterly and transducer 
calibration monthly.
    (v) Conduct calibration checks any time the sensor exceeds the 
manufacturer's specified maximum operating pressure range or install a 
new pressure sensor.
    (vi) At least monthly, inspect components for integrity, electrical 
connections for continuity, and mechanical connections for leakage.

[[Page 32]]



Sec. 63.9307  What are my continuous emissions monitoring system 
installation, operation, and maintenance requirements?

    (a) You must install, operate, and maintain each CEMS to monitor 
carbon monoxide (CO) or total hydrocarbons (THC) and oxygen 
(O2) at the outlet of the exhaust system of the engine test 
cell/stand or at the outlet of the emission control device.
    (b) To comply with the CO or THC percent reduction emission 
limitation, you may install, operate, and maintain a CEMS to monitor CO 
or THC and O2 at both the inlet and the outlet of the 
emission control device.
    (c) To comply with either emission limitations, the CEMS must be 
installed and operated according to the requirements described in 
paragraphs (c)(1) through (4) of this section.
    (1) You must install, operate, and maintain each CEMS according to 
the applicable Performance Specification (PS) of 40 CFR part 60, 
appendix B (PS-3 or PS-4A).
    (2) You must conduct a performance evaluation of each CEMS according 
to the requirements in 40 CFR 63.8 and according to PS-3 of 40 CFR part 
60, appendix B, using Reference Method 3A or 3B for the O2 
CEMS, and according to PS-4A of 40 CFR part 60, appendix B, using 
Reference Method 10 or 10B for the CO CEMS. If the fuel used in the 
engines being tested is natural gas, you may use ASTM D 6522-00, 
Standard Test Method for Determination of Nitrogen Oxides, Carbon 
Monoxide and Oxygen Concentrations in Emissions from Natural Gas Fired 
Reciprocating Engines, Combustion Turbines, Boilers, and Process Heaters 
Using Portable Analyzers (incorporated by reference, see Sec. 63.14). 
As an alternative to Method 3B, you may use ANSI/ASME PTC 19.10-1981, 
``Flue and Exhaust Gas Analyses [Part 10, Instruments and Apparatus],'' 
(incorporated by reference, see Sec. 63.14).
    (3) As specified in Sec. 63.8(c)(4)(ii), each CEMS must complete a 
minimum of one cycle of operation (sampling, analyzing, and data 
recording) for each successive 15-minute period. You must have at least 
two data points, each representing a different 15-minute period within 
the same hour, to have a valid hour of data.
    (4) All CEMS data must be reduced as specified in Sec. 63.8(g)(2) 
and recorded as CO concentration in parts per million by volume, dry 
basis (ppmvd), corrected to 15 percent O2 content.
    (d) If you have CEMS that are subject to paragraph (a) or (b) of 
this section, you must properly maintain and operate the monitors 
continuously according to the requirements described in paragraphs 
(d)(1) and (2) of this section.
    (1) Proper Maintenance. You must maintain the monitoring equipment 
at all times that the engine test cell/stand is operating, including but 
not limited to, maintaining necessary parts for routine repairs of the 
monitoring equipment.
    (2) Continued Operation. You must operate your CEMS according to 
paragraphs (d)(2)(i) and (ii) of this section.
    (i) You must conduct all monitoring in continuous operation at all 
times that the engine test cell/stand is operating, except for, as 
applicable, monitoring malfunctions, associated repairs, and required 
quality assurance or control activities (including, as applicable, 
calibration drift checks and required zero and high-level adjustments). 
Quality assurance or control activities must be performed according to 
procedure 1 of 40 CFR part 60, appendix F.
    (ii) Data recorded during monitoring malfunctions, associated 
repairs, out-of-control periods, and required quality assurance or 
control activities must not be used for purposes of calculating data 
averages. You must use all of the data collected from all other periods 
in assessing compliance. A monitoring malfunction is any sudden, 
infrequent, not reasonably preventable failure of the monitoring 
equipment to provide valid data. Monitoring failures that are caused in 
part by poor maintenance or careless operation are not malfunctions. Any 
period for which the monitoring system is out-of-control and data are 
not available for required calculations constitutes a deviation from the 
monitoring requirements.

[[Page 33]]

               Testing and Initial Compliance Requirements



Sec. 63.9310  By what date must I conduct the initial compliance 
demonstrations?

    You must conduct the initial compliance demonstrations that apply to 
you in Table 3 to this subpart within 180 calendar days after the 
compliance date that is specified for your new or reconstructed affected 
source in Sec. 63.9295 and according to the provisions in Sec. 
63.7(a)(2).



Sec. 63.9320  What procedures must I use?

    (a) You must conduct each initial compliance demonstration that 
applies to you in Table 3 to this subpart.
    (b) You must conduct an initial performance evaluation of each 
capture and control system according to Sec. Sec. 63.9321, 63.9322, 
63.9323 and 63.9324, and each CEMS according to the requirements in 40 
CFR 63.8 and according to the applicable Performance Specification of 40 
CFR part 60, appendix B (PS-3 or PS-4A).
    (c) The initial demonstration of compliance with the carbon monoxide 
(CO) or total hydrocarbon (THC) concentration limitation consists of the 
first 4-hour rolling average CO or THC concentration recorded after 
completion of the CEMS performance evaluation. You must correct the CO 
or THC concentration at the outlet of the engine test cell/stand or the 
emission control device to a dry basis and to 15 percent O2 
content according to Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.002

Where:

Cc = concentration of CO or THC, corrected to 15 percent oxygen, ppmvd
Cunc = total uncorrected concentration of CO or THC, ppmvd
%O2d = concentration of oxygen measured in gas stream, dry basis, 
percent by volume.

    (d) The initial demonstration of compliance with the CO or THC 
percent reduction emission limitation consists of the first 4-hour 
rolling average percent reduction in CO or THC recorded after completion 
of the performance evaluation of the capture/control system and/or CEMS. 
You must complete the actions described in paragraphs (d)(1) through (2) 
of this section.
    (1) Correct the CO or THC concentrations at the inlet and outlet of 
the emission control device to a dry basis and to 15 percent 
O2 content using Equation 1 of this section.
    (2) Calculate the percent reduction in CO or THC using Equation 2 of 
this section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.003

Where:

R = percent reduction in CO or THC
Ci = corrected CO or THC concentration at inlet of the emission control 
device
Co = corrected CO or THC concentration at the outlet of the emission 
control device.



Sec. 63.9321  What are the general requirements for performance tests?

    (a) You must conduct each performance test required by Sec. 63.9310 
according to the requirements in Sec. 63.7(e)(1) and under the 
conditions in this section unless you obtain a waiver of the performance 
test according to the provisions in Sec. 63.7(h).
    (1) Representative engine testing conditions. You must conduct the 
performance test under representative operating conditions for the test 
cell/stand. Operations during periods of SSM, and during periods of 
nonoperation do not constitute representative conditions. You must 
record the process information that is necessary to document operating 
conditions during the test and explain why the conditions represent 
normal operation.
    (2) Representative emission capture system and add-on control device 
operating conditions. You must conduct the performance test when the 
emission capture system and add-on control device are operating at a 
representative flow rate, and the add-on control device is operating at 
a representative inlet concentration. You must record information that 
is necessary to document emission capture system and add-on control 
device operating conditions during the test and explain why the 
conditions represent normal operation.
    (b) You must conduct each performance test of an emission capture 
system according to the requirements in

[[Page 34]]

Sec. 63.9322. You must conduct each performance test of an add-on 
control device according to the requirements in Sec. 63.9323.



Sec. 63.9322  How do I determine the emission capture system efficiency?

    You must use the procedures and test methods in this section to 
determine capture efficiency as part of the performance test required by 
Sec. 63.9310.
    (a) Assuming 100 percent capture efficiency. You may assume the 
capture system efficiency is 100 percent if both conditions in 
paragraphs (a)(1) and (2) of this section are met:
    (1) The capture system meets the criteria in Method 204 of appendix 
M to 40 CFR part 51 for a potential to emit (PTE) and directs all the 
exhaust gases from the enclosure to an add-on control device.
    (2) All engine test operations creating exhaust gases for which the 
test is applicable are conducted within the capture system.
    (b) Measuring capture efficiency. If the capture system does not 
meet the criteria in paragraphs (a)(1) and (2) of this section, then you 
must use one of the two protocols described in paragraphs (c) and (d) of 
this section to measure capture efficiency. The capture efficiency 
measurements use total volatile hydrocarbon (TVH) capture efficiency as 
a surrogate for organic HAP capture efficiency. For the protocol in 
paragraph (c) of this section, the capture efficiency measurement must 
consist of three test runs. Each test run must be at least 3 hours in 
duration or the length of a production run, whichever is longer, up to 8 
hours. For the purposes of this test, a production run means the time 
required for a single engine test to go from the beginning to the end.
    (c) Gas-to-gas protocol using a temporary total enclosure or a 
building enclosure. The gas-to-gas protocol compares the mass of TVH 
emissions captured by the emission capture system to the mass of TVH 
emissions not captured. Use a temporary total enclosure or a building 
enclosure and the procedures in paragraphs (c)(1) through (5) of this 
section to measure emission capture system efficiency using the gas-to-
gas protocol.
    (1) Either use a building enclosure or construct an enclosure around 
the engine test cell/stand and all areas where emissions from the engine 
testing subsequently occur. The enclosure must meet the applicable 
definition of a temporary total enclosure or building enclosure in 
Method 204 of appendix M to 40 CFR part 51.
    (2) Use Method 204B or 204C of appendix M to 40 CFR part 51 to 
measure the total mass, kg, of TVH emissions captured by the emission 
capture system during each capture efficiency test run as measured at 
the inlet to the add-on control device. To make the measurement, 
substitute TVH for each occurrence of the term VOC in the methods.
    (i) The sampling points for the Method 204B or 204C of appendix M to 
40 CFR part 51 measurement must be upstream from the add-on control 
device and must represent total emissions routed from the capture system 
and entering the add-on control device.
    (ii) If multiple emission streams from the capture system enter the 
add-on control device without a single common duct, then the emissions 
entering the add-on control device must be simultaneously measured in 
each duct, and the total emissions entering the add-on control device 
must be determined.
    (3) Use Method 204D or 204E of appendix M to 40 CFR part 51 to 
measure the total mass, kg, of TVH emissions that are not captured by 
the emission capture system; they are measured as they exit the 
temporary total enclosure or building enclosure during each capture 
efficiency test run. To make the measurement, substitute TVH for each 
occurrence of the term VOC in the methods.
    (i) Use Method 204D of appendix M to 40 CFR part 51 if the enclosure 
is a temporary total enclosure.
    (ii) Use Method 204E of appendix M to 40 CFR part 51 if the 
enclosure is a building enclosure. During the capture efficiency 
measurement, all organic compound emitting operations inside the 
building enclosure, other than the engine test cell/stand operation for 
which capture efficiency is being determined, must be shut down, but all 
fans and blowers must be operating normally.

[[Page 35]]

    (4) For each capture efficiency test run, determine the percent 
capture efficiency of the emission capture system using Equation 1 of 
this section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.004

Where:

CE = capture efficiency of the emission capture system vented to the 
add-on control device, percent
TVH captured = total mass of TVH captured by the emission capture system 
as measured at the inlet to the add-on control device during the 
emission capture efficiency test run, kg, determined according to 
paragraph (c)(2) of this section
TVH uncaptured = total mass of TVH that is not captured by the emission 
capture system and that exits from the temporary total enclosure or 
building enclosure during the capture efficiency test run, kg, 
determined according to paragraph (c)(3) of this section.

    (5) Determine the capture efficiency the emission capture system as 
the average of the capture efficiencies measured in the three test runs.
    (d) Alternative capture efficiency protocol. As an alternative to 
the procedure specified in paragraph (c) of this section, you may 
determine capture efficiency using any other capture efficiency protocol 
and test methods that satisfy the criteria of either the data quality 
objective or lower control limit approach as described in appendix A to 
subpart KK of this part.



Sec. 63.9323  How do I determine the add-on control device emission 
destruction or removal efficiency?

    You must use the procedures and test methods in this section to 
determine the add-on control device emission destruction or removal 
efficiency as part of the performance test required by Sec. 63.9310. 
You must conduct three test runs as specified in Sec. 63.7(e)(3), and 
each test run must last at least 1 hour.
    (a) For all types of add-on control devices, use the test methods 
specified in paragraphs (a)(1) through (5) of this section.
    (1) Use Method 1 or 1A of appendix A to 40 CFR part 60, as 
appropriate, to select sampling sites and velocity traverse points.
    (2) Use Method 2, 2A, 2C, 2D, 2F, or 2G of appendix A to 40 CFR part 
60, as appropriate, to measure gas volumetric flow rate.
    (3) Use Method 3, 3A, or 3B of appendix A to 40 CFR part 60, as 
appropriate, for gas analysis to determine dry molecular weight. The 
ANSI/ASME PTC 19.10-1981 Part 10 is an acceptable alternative to Method 
3B (incorporated by reference, see Sec. 63.14).
    (4) Use Method 4 of appendix A to 40 CFR part 60, to determine stack 
gas moisture.
    (5) Methods for determining gas volumetric flow rate, dry molecular 
weight, and stack gas moisture must be performed, as applicable, during 
each test run.
    (b) Measure total gaseous organic mass emissions as carbon at the 
inlet and outlet of the add-on control device simultaneously, using 
either Method 25 or 25A of appendix A to 40 CFR part 60, as specified in 
paragraphs (b)(1) through (3) of this section. You must use the same 
method for both the inlet and outlet measurements.
    (1) Use Method 25 of appendix A to 40 CFR part 60 if the add-on 
control device is an oxidizer, and you expect the total gaseous organic 
concentration as carbon to be more than 50 parts per million at the 
control device outlet.
    (2) Use Method 25A of appendix A to 40 CFR part 60 if the add-on 
control device is an oxidizer, and you expect the total gaseous organic 
concentration as carbon to be 50 ppm or less at the control device 
outlet.
    (c) For each test run, determine the total gaseous organic emissions 
mass flow rates for the inlet and the outlet of the add-on control 
device, using Equation 1 of this section. If there is more than one 
inlet or outlet to the

[[Page 36]]

add-on control device, you must calculate the total gaseous organic mass 
flow rate using Equation 1 of this section for each inlet and each 
outlet and then total all of the inlet emissions and total all of the 
outlet emissions.
[GRAPHIC] [TIFF OMITTED] TR27MY03.005

Where:

Mf = total gaseous organic emissions mass flow rate, kg/hour 
(kg/h)
Cc = concentration of organic compounds as carbon in the vent 
gas, as determined by Method 25 or Method 25A, parts per million by 
volume (ppmv), dry basis
Qsd = volumetric flow rate of gases entering or exiting the 
add-on control device, as determined by Method 2, 2A, 2C, 2D, 2F, or 2G, 
dry standard cubic meters/hour (dscm/h)
0.0416 = conversion factor for molar volume, kg-moles per cubic meter 
(mol/m\3\) (@ 293 Kelvin [K] and 760 millimeters of mercury [mmHg]).

    (d) For each test run, determine the add-on control device organic 
emissions destruction or removal efficiency, using Equation 2 of this 
section:
[GRAPHIC] [TIFF OMITTED] TR27MY03.006

Where:

DRE = organic emissions destruction or removal efficiency of the add-on 
control device, percent
Mfi = total gaseous organic emissions mass flow rate at the inlet(s) to 
the add-on control device, using Equation 1 of this section, kg/h
Mfo = total gaseous organic emissions mass flow rate at the outlet(s) of 
the add-on control device, using Equation 1 of this section, kg/h.

    (e) Determine the emission destruction or removal efficiency of the 
add-on control device as the average of the efficiencies determined in 
the three test runs and calculated in Equation 2 of this section.



Sec. 63.9324  How do I establish the emission capture system and 
add-on control device operating limits during the performance test?

    During the performance test required by Sec. 63.9310, you must 
establish the operating limits required by Sec. 63.9302 according to 
this section, unless you have received approval for alternative 
monitoring and operating limits under Sec. 63.8(f) as specified in 
Sec. 63.9302.
    (a) Thermal oxidizers. If your add-on control device is a thermal 
oxidizer, establish the operating limits according to paragraphs (a)(1) 
and (2) of this section.
    (1) During the performance test, you must monitor and record the 
combustion temperature at least once every 15 minutes during each of the 
three test runs. You must monitor the temperature in the firebox of the 
thermal oxidizer or immediately downstream of the firebox before any 
substantial heat exchange occurs.
    (2) Use the data collected during the performance test to calculate 
and record the average combustion temperature maintained during the 
performance test. This average combustion temperature is the minimum 
operating limit for your thermal oxidizer.
    (b) Catalytic oxidizers. If your add-on control device is a 
catalytic oxidizer, establish the operating limits according to either 
paragraphs (b)(1) and (2) or paragraphs (b)(3) and (4) of this section.
    (1) During the performance test, you must monitor and record the 
temperature just before the catalyst bed and the temperature difference 
across the catalyst bed at least once every 15 minutes during each of 
the three test runs.
    (2) Use the data collected during the performance test to calculate 
and record the average temperature just before the catalyst bed and the 
average temperature difference across the catalyst bed maintained during 
the performance test. These are the minimum operating limits for your 
catalytic oxidizer.
    (3) As an alternative to monitoring the temperature difference 
across the catalyst bed, you may monitor the

[[Page 37]]

temperature at the inlet to the catalyst bed and implement a site-
specific inspection and maintenance plan for your catalytic oxidizer as 
specified in paragraph (b)(4) of this section. During the performance 
test, you must monitor and record the temperature just before the 
catalyst bed at least once every 15 minutes during each of the three 
test runs. Use the data collected during the performance test to 
calculate and record the average temperature just before the catalyst 
bed during the performance test. This is the minimum operating limit for 
your catalytic oxidizer.
    (4) You must develop and implement an inspection and maintenance 
plan for your catalytic oxidizer(s) for which you elect to monitor 
according to paragraph (b)(3) of this section. The plan must address, at 
a minimum, the elements specified in paragraphs (b)(4)(i) through (iii) 
of this section.
    (i) Annual sampling and analysis of the catalyst activity (i.e., 
conversion efficiency) following the manufacturer's or catalyst 
supplier's recommended procedures.
    (ii) Monthly inspection of the oxidizer system, including the burner 
assembly and fuel supply lines for problems and, as necessary, adjust 
the equipment to assure proper air-to-fuel mixtures.
    (iii) Annual internal and monthly external visual inspection of the 
catalyst bed to check for channeling, abrasion, and settling. If 
problems are found, you must take corrective action consistent with the 
manufacturer's recommendation and conduct a new performance test to 
determine destruction efficiency according to Sec. 63.9323.
    (c) Emission capture system. For each capture device that is not 
part of a PTE that meets the criteria of Sec. 63.9322(a), establish an 
operating limit for either the gas volumetric flow rate or duct static 
pressure, as specified in paragraphs (c)(1) and (2) of this section. The 
operating limit for a PTE is specified in Table 3 to this subpart.
    (1) During the capture efficiency determination required by Sec. 
63.9310, you must monitor and record either the gas volumetric flow rate 
or the duct static pressure for each separate capture device in your 
emission capture system at least once every 15 minutes during each of 
the three test runs at a point in the duct between the capture device 
and the add-on control device inlet.
    (2) Calculate and record the average gas volumetric flow rate or 
duct static pressure for the three test runs for each capture device. 
This average gas volumetric flow rate or duct static pressure is the 
minimum operating limit for that specific capture device.



Sec. 63.9330  How do I demonstrate initial compliance with the emission 
limitation?

    (a) You must demonstrate initial compliance with the emission 
limitation that applies to you according to Table 3 to this subpart.
    (b) You must submit the Notification of Compliance Status containing 
results of the initial compliance demonstration according to the 
requirements in Sec. 63.9345(c).

                   Continuous Compliance Requirements



Sec. 63.9335  How do I monitor and collect data to demonstrate continuous 
compliance?

    (a) Except for monitor malfunctions, associated repairs, and 
required quality assurance or quality control activities (including, as 
applicable, calibration drift checks and required zero and high-level 
adjustments of the monitoring system), you must conduct all monitoring 
in continuous operation at all times the engine test cell/stand is 
operating.
    (b) Do not use data recorded during monitor malfunctions, associated 
repairs, and required quality assurance or quality control activities 
for meeting the requirements of this subpart, including data averages 
and calculations. You must use all the data collected during all other 
periods in assessing the performance of the emission control device or 
in assessing emissions from the new or reconstructed affected source.



Sec. 63.9340  How do I demonstrate continuous compliance with the emission 
limitations?

    (a) You must demonstrate continuous compliance with the emission 
limitation in Table 1 to this subpart

[[Page 38]]

that applies to you according to methods specified in Table 5 to this 
subpart.
    (b) You must report each instance in paragraphs (b)(1) and (2) of 
this section. These instances are deviations from the emission 
limitation in this subpart and must be reported according to the 
requirements in Sec. 63.9350.
    (1) You must report each instance in which you did not meet the 
emission limitation that applies to you.
    (2) You must report each instance in which you did not meet the 
requirements in Table 7 to this subpart that apply to you.
    (c) Startups, shutdowns, and malfunctions. During periods of SSM of 
control device and associated monitoring equipment, you must operate in 
accordance with your SSMP.
    (1) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations 
that occur during a period of SSM of control devices and associated 
monitoring equipment are not violations if you demonstrate to the 
Administrator's satisfaction that you were operating in accordance with 
the SSMP.
    (2) The Administrator will determine whether deviations that occur 
during a period of SSM of control devices and associated monitoring 
equipment are violations, according to the provisions in Sec. 63.6(e).

                   Notifications, Reports, and Records



Sec. 63.9345  What notifications must I submit and when?

    (a) You must submit all of the notifications in Sec. Sec. 63.8(e), 
63.8(f)(4) and (6), and 63.9(b), (g)(1), (g)(2) and (h) that apply to 
you by the dates specified.
    (b) If you own or operate a new or reconstructed test cell/stand 
used for testing internal combustion engines, you are required to submit 
an Initial Notification as specified in paragraphs (b)(1) through (3) of 
this section.
    (1) As specified in Sec. 63.9(b)(2), if you start up your new or 
reconstructed affected source before the effective date of this subpart, 
you must submit an Initial Notification not later than 120 calendar days 
after May 27, 2003.
    (2) As specified in Sec. 63.9(b), if you start up your new or 
reconstructed affected source on or after the effective date of this 
subpart, you must submit an Initial Notification not later than 120 
calendar days after you become subject to this subpart.
    (3) If you are required to submit an Initial Notification but are 
otherwise not affected by the requirements of this subpart, in 
accordance with Sec. 63.9290(c), your notification should include the 
information in Sec. 63.9(b)(2)(i) through (v) and a statement that your 
new or reconstructed engine test cell/stand has no additional 
requirements and explain the basis of the exclusion (for example, that 
the test cell/stand is used exclusively for testing internal combustion 
engines with rated power of less than 25 hp (19 kW)).
    (c) If you are required to comply with the emission limitations in 
Table 1 to this subpart, you must submit a Notification of Compliance 
Status according to Sec. 63.9(h)(2)(ii). For each initial compliance 
demonstration with the emission limitation, you must submit the 
Notification of Compliance Status before the close of business on the 
30th calendar day following the completion of the initial compliance 
demonstration.
    (d) You must submit a notification of initial performance evaluation 
of your CEMS or performance testing of your control device at least 60 
calendar days before the performance testing/evaluation is scheduled to 
begin as required in Sec. 63.8(e)(2).



Sec. 63.9350  What reports must I submit and when?

    (a) If you own or operate a new or reconstructed affected source 
that must meet the emission limitation, you must submit a semiannual 
compliance report according to Table 6 to this subpart by the applicable 
dates specified in paragraphs (a)(1) through (6) of this section, unless 
the Administrator has approved a different schedule.
    (1) The first semiannual compliance report must cover the period 
beginning on the compliance date specified in Sec. 63.9295 and ending 
on June 30 or December 31, whichever date is the first date following 
the end of the first calendar half after the compliance date specified 
in Sec. 63.9295.
    (2) The first semiannual compliance report must be postmarked or 
delivered no later than July 31 or January 31,

[[Page 39]]

whichever date follows the end of the first calendar half after the 
compliance date that is specified in Sec. 63.9295.
    (3) Each subsequent semiannual compliance report must cover the 
semiannual reporting period from January 1 through June 30 or the 
semiannual reporting period from July 1 through December 31.
    (4) Each subsequent semiannual compliance report must be postmarked 
or delivered no later than July 31 or January 31, whichever date is the 
first date following the end of the semiannual reporting period.
    (5) For each new or reconstructed engine test cell/stand that is 
subject to permitting regulations pursuant to 40 CFR part 70 or 71, and 
if the permitting authority has established the date for submitting 
semiannual reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance 
reports according to the dates the permitting authority has established 
instead of according to the dates in paragraphs (a)(1) through (4) of 
this section.
    (6) If you had an SSM of a control device or associated monitoring 
equipment during the reporting period and you took actions consistent 
with your SSMP, the compliance report must include the information in 
paragraphs Sec. 63.10(d)(5)(i).
    (b) If there is no deviation from the applicable emission limitation 
and the CEMS or CPMS was not out-of-control, according to Sec. 
63.8(c)(7), the semiannual compliance report must contain the 
information described in paragraphs (b)(1) through (4) of this section.
    (1) Company name and address.
    (2) Statement by a responsible official, with that official's name, 
title, and signature, certifying the truth, accuracy, and completeness 
of the content of the report.
    (3) Date of report and beginning and ending dates of the reporting 
period.
    (4) A statement that no deviation from the emission limit occurred 
during the reporting period and that no CEMS or CPMS was out-of-control, 
according to Sec. 63.8(c)(7).
    (c) For each deviation from an emission limit, the semiannual 
compliance report must include the information in paragraphs (b)(1) 
through (3) of this section and the information included in paragraphs 
(c)(1) through (4) of this section.
    (1) The date and time that each deviation started and stopped.
    (2) The total operating time of each new or reconstructed engine 
test cell/stand during the reporting period.
    (3) A summary of the total duration of the deviation during the 
reporting period (recorded in 4-hour periods), and the total duration as 
a percent of the total operating time during that reporting period.
    (4) A breakdown of the total duration of the deviations during the 
reporting period into those that are due to control equipment problems, 
process problems, other known causes, and other unknown causes.
    (d) For each CEMS or CPMS deviation, the semiannual compliance 
report must include the information in paragraphs (b)(1) through (3) of 
this section and the information included in paragraphs (d)(1) through 
(10) of this section.
    (1) The date and time that each CEMS or CPMS was inoperative except 
for zero (low-level) and high-level checks.
    (2) The date and time that each CEMS or CPMS was out-of-control 
including the information in Sec. 63.8(c)(8).
    (3) A summary of the total duration of CEMS or CPMS downtime during 
the reporting period (reported in 4-hour periods), and the total 
duration of CEMS or CPMS downtime as a percent of the total engine test 
cell/stand operating time during that reporting period.
    (4) A breakdown of the total duration of CEMS or CPMS downtime 
during the reporting period into periods that are due to monitoring 
equipment malfunctions, nonmonitoring equipment malfunctions, quality 
assurance/quality control calibrations, other known causes and other 
unknown causes.
    (5) The monitoring equipment manufacturer(s) and model number(s) of 
each monitor.
    (6) The date of the latest CEMS or CPMS certification or audit.
    (7) The date and time period of each deviation from an operating 
limit in Table 2 to this subpart; date and time period of any bypass of 
the add-on control device; and whether each deviation

[[Page 40]]

occurred during a period of SSM or during another period.
    (8) A summary of the total duration of each deviation from an 
operating limit in Table 2 to this subpart, each bypass of the add-on 
control device during the semiannual reporting period, and the total 
duration as a percent of the total source operating time during that 
semiannual reporting period.
    (9) A breakdown of the total duration of the deviations from the 
operating limits in Table 2 to this subpart and bypasses of the add-on 
control device during the semiannual reporting period by identifying 
deviations due to startup, shutdown, control equipment problems, process 
problems, other known causes, and other unknown causes.
    (10) A description of any changes in CEMS, CPMS, or controls since 
the last reporting period.
    (e) If you had an SSM of a control device or associated monitoring 
equipment during the semiannual reporting period that was not consistent 
with your SSMP, you must submit an immediate SSM report according to the 
requirements in Sec. 63.10(d)(5)(ii).



Sec. 63.9355  What records must I keep?

    (a) You must keep the records as described in paragraphs (a)(1) 
through (5) of this section.
    (1) A copy of each notification and report that you submitted to 
comply with this subpart, including all documentation supporting any 
Initial Notification or Notification of Compliance Status that you 
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
    (2) Records of performance evaluations as required in Sec. 
63.10(b)(2)(viii).
    (3) Records of the occurrence and duration of each malfunction of 
the air pollution control equipment, if applicable, as required in Sec. 
63.10(b)(2)(ii).
    (4) Records of all maintenance on the air pollution control 
equipment, if applicable, as required in Sec. 63.10(b)(iii).
    (5) The calculation of the mass of organic HAP emission reduction by 
emission capture systems and add-on control devices.
    (b) For each CPMS, you must keep the records as described in 
paragraphs (b)(1) through (7) of this section.
    (1) For each deviation, a record of whether the deviation occurred 
during a period of SSM of the control device and associated monitoring 
equipment.
    (2) The records in Sec. 63.6(e)(3)(iii) through (v) related to SSM.
    (3) The records required to show continuous compliance with each 
operating limit specified in Table 2 to this subpart that applies to 
you.
    (4) For each capture system that is a PTE, the data and 
documentation you used to support a determination that the capture 
system meets the criteria in Method 204 of appendix M to 40 CFR part 51 
for a PTE and has a capture efficiency of 100 percent, as specified in 
Sec. 63.9322(a).
    (5) For each capture system that is not a PTE, the data and 
documentation you used to determine capture efficiency according to the 
requirements specified in Sec. Sec. 63.9321 and 63.9322(b) through (e), 
including the records specified in paragraphs (b)(5)(i) and (ii) of this 
section that apply to you.
    (i) Records for a gas-to-gas protocol using a temporary total 
enclosure or a building enclosure. Records of the mass of TVH emissions 
captured by the emission capture system as measured by Method 204B or C 
of appendix M to 40 CFR part 51 at the inlet to the add-on control 
device, including a copy of the test report. Records of the mass of TVH 
emissions not captured by the capture system that exited the temporary 
total enclosure or building enclosure during each capture efficiency 
test run as measured by Method 204D or E of appendix M to 40 CFR part 
51, including a copy of the test report. Records documenting that the 
enclosure used for the capture efficiency test met the criteria in 
Method 204 of appendix M to 40 CFR part 51 for either a temporary total 
enclosure or a building enclosure.
    (ii) Records for an alternative protocol. Records needed to document 
a capture efficiency determination using an alternative method or 
protocol as specified in Sec. 63.9322(e), if applicable.
    (6) The records specified in paragraphs (b)(6)(i) and (ii) of this 
section for each add-on control device organic HAP destruction or 
removal efficiency determination as specified in Sec. 63.9323.

[[Page 41]]

    (i) Records of each add-on control device performance test conducted 
according to Sec. Sec. 63.9321, 63.9322, and 63.9323.
    (ii) Records of the engine testing conditions during the add-on 
control device performance test showing that the performance test was 
conducted under representative operating conditions.
    (7) Records of the data and calculations you used to establish the 
emission capture and add-on control device operating limits as specified 
in Sec. 63.9324 and to document compliance with the operating limits as 
specified in Table 2 to this subpart.
    (c) For each CEMS, you must keep the records as described in 
paragraphs (c)(1) through (4) of this section.
    (1) Records described in Sec. 63.10(b)(2)(vi) through (xi).
    (2) Previous (i.e., superceded) versions of the performance 
evaluation plan as required in Sec. 63.8(d)(3).
    (3) Request for alternatives to the relative accuracy test for CEMS 
as required in Sec. 63.8(f)(6)(i), if applicable.
    (4) The records in Sec. 63.6(e)(3)(iii) through (v) related to SSM 
of the control device and associated monitoring equipment.
    (d) You must keep the records required in Table 5 to this subpart to 
show continuous compliance with each emission limitation that applies to 
you.



Sec. 63.9360  In what form and how long must I keep my records?

    (a) You must maintain all applicable records in such a manner that 
they can be readily accessed and are suitable for inspection according 
to Sec. 63.10(b)(1).
    (b) As specified in Sec. 63.10(b)(1), you must keep each records 
for 5 years following the date of each occurrence, measurement, 
maintenance, corrective action, report, or record.
    (c) You must retain your records of the most recent 2 years on site, 
or your records must be accessible on site. Your records of the 
remaining 3 years may be retained off site.

                   Other Requirements and Information



Sec. 63.9365  What parts of the General Provisions apply to me?

    Table 7 to this subpart shows which parts of the General Provisions 
in Sec. Sec. 63.1 through 63.15 apply to you.



Sec. 63.9370  Who implements and enforces this subpart?

    (a) This subpart can be implemented and enforced by us, the U.S. 
EPA, or a delegated authority such as your State, local, or tribal 
agency. If the U.S. EPA Administrator has delegated authority to your 
State, local, or tribal agency, then that agency, in addition to the 
U.S. EPA, has the authority to implement and enforce this subpart. You 
should contact your U.S. EPA Regional Office to find out if 
implementation and enforcement of this subpart is delegated to your 
State, local, or tribal agency.
    (b) In delegating implementation and enforcement authority of this 
subpart to a State, local, or tribal agency under section 40 CFR part 
63, subpart E, the authorities contained in paragraph (c) of this 
section are retained by the Administrator of U.S. EPA and are not 
transferred to the State, local, or tribal agency.
    (c) The authorities that cannot be delegated to State, local, or 
tribal agencies are described in paragraphs (c)(1) through (4) of this 
section.
    (1) Approval of alternatives to the emission limitations in Sec. 
63.9300 under Sec. 63.6(g).
    (2) Approval of major changes to test methods under Sec. 
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
    (3) Approval of major changes to monitoring under Sec. 63.8(f) and 
as defined in Sec. 63.90.
    (4) Approval of major changes to recordkeeping and reporting under 
Sec. 63.10(f) and as defined in Sec. 63.90.



Sec. 63.9375  What definitions apply to this subpart?

    Terms used in this subpart are defined in the CAA; in 40 CFR 63.2, 
and in this section:
    CAA means the Clean Air Act (42 U.S.C. 7401 et seq., as amended by 
Public Law 101-549, 104 Statute 2399).
    Area source means any stationary source of HAP that is not a major 
source as defined in this part.
    Combustion turbine engine means a device in which air is compressed 
in a compressor, enters a combustion chamber, and is compressed further 
by the combustion of fuel injected into the

[[Page 42]]

combustion chamber. The hot compressed combustion gases then expand over 
a series of curved vanes or blades arranged on a central spindle that 
rotates.
    Deviation means any instance in which an affected source subject to 
this subpart, or an owner or operator of such a source:
    (1) Fails to meet any requirement or obligation established by this 
subpart, including but not limited to any emission limitations;
    (2) Fails to meet any term or condition that is adopted to implement 
an applicable requirement in this subpart and that is included in the 
operating permit for any affected source required to obtain such a 
permit; or
    (3) Fails to meet any emission limitation in this subpart during 
malfunction, regardless or whether or not such failure is permitted by 
this subpart.
    Engine means any internal combustion engine, any combustion turbine 
engine, or any rocket engine.
    Engine Test Cell/Stand means any apparatus used for testing 
uninstalled stationary or uninstalled mobile (motive) engines.
    Hazardous Air Pollutant (HAP) means any air pollutant listed in or 
pursuant to section 112(b) of the CAA.
    Internal combustion engine means a device in which air enters a 
combustion chamber, is mixed with fuel, compressed in the chamber, and 
combusted. Fuel may enter the combustion chamber with the air or be 
injected into the combustion chamber. Expansion of the hot combustion 
gases in the chamber rotates a shaft, either through a reciprocating or 
rotary action. For purposes of this subpart, this definition does not 
include combustion turbine engines.
    Major source, as used in this subpart, shall have the same meaning 
as in Sec. 63.2.
    Malfunction means any sudden, infrequent, and not reasonably 
preventable failure of air pollution control equipment, process 
equipment, or a process to operate in a normal or usual manner. Failures 
that are caused in part by poor maintenance or careless operation are 
not malfunctions.
    Rated power means the maximum power output of an engine in use.
    Potential to emit means the maximum capacity of a stationary source 
to emit a pollutant under its physical and operational design. Any 
physical or operational limitation on the capacity of the stationary 
source to emit a pollutant, including air pollution control equipment 
and restrictions on hours of operation or on the type or amount of 
material combusted, stored, or processed, shall be treated as part of 
its design if the limitation or the effect it would have on emissions is 
federally enforceable.
    Responsible official means responsible official as defined by 40 CFR 
70.2.
    Rocket engine means a device consisting of a combustion chamber in 
which materials referred to as propellants, which provide both the fuel 
and the oxygen for combustion, are burned. Combustion gases escape 
through a nozzle, providing thrust.
    Uninstalled engine means an engine not installed in, or an 
integrated part of, the final product.

        Table 1 to Subpart PPPPP of Part 63--Emission Limitations

    You must comply with the emission limits that apply to your affected 
source in the following table as required by Sec. 63.9300.

------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. internal combustion engines with      a. limit the concentration of
 rated power of 25 hp (19 kW) or more.    CO or THC to 20 ppmvd or less
                                          (corrected to 15 percent O2
                                          content); or
                                         b. achieve a reduction in CO or
                                          THC of 96 percent or more
                                          between the inlet and outlet
                                          concentrations (corrected to
                                          15 percent O2 content) of the
                                          emission control device.
------------------------------------------------------------------------


[[Page 43]]

          Table 2 to Subpart PPPPP of Part 63--Operating Limits

    If you are required to comply with operating limits in Sec. 
63.9302, you must comply with the applicable operating limits in the 
following table:

------------------------------------------------------------------------
 
 
 
 
 
 
------------------------------------------------------------------------
1. Thermal oxidizer.........  a. The average        i. Collecting the
                               combustion            combustion
                               temperature in any    temperature data
                               3-hour period must    according to Sec.
                               not fall below the    63.9306(c);
                               the combustion       ii. Reducing the
                               temperature limit     data to 3-hour
                               established           block averages; and
                               according to Sec. iii. Maintaining the
                               63.9324(a).           3-hour average
                                                     combustion
                                                     temperature at or
                                                     above the
                                                     temperature limit.
-----------------------------
2. Catalytic oxidizer.......  a. The average        i. Collecting the
                               temperature           temperature data
                               measured just         according to Sec.
                               before the catalyst   63.9306(c);
                               bed in any 3-hour    ii. Reducing the
                               period must not       data to 3-hour
                               fall below the        block averages; and
                               limit established    iii. Maintaining the
                               according to Sec. 3-hour average
                               63.9324(b).           temperature before
                                                     the catalyst bed at
                                                     or above the
                                                     temperature limit.
                              b. Either ensure      i. Either collecting
                               that the average      the temperature
                               temperature           data according to
                               difference across     Sec. 63.9306(c),
                               the catalyst bed in   reducing the data
                               any 3-hour period     to 3-hour block
                               does not fall below   averages, and
                               the temperature       maintaining the 3-
                               difference limit      hour average
                               established           temperature
                               according to Sec. difference at or
                               63.9324(b)(2) or      above the
                               develop and           temperature
                               implement an          difference limit;
                               inspection and        or
                               maintenance plan     ii. Complying with
                               according to Sec. the inspection and
                               63.9324(b)(3) and     maintenance plan
                               (4).                  developed according
                                                     to Sec.
                                                     63.9324(b)(3) and
                                                     (4).
-----------------------------
3. Emission capture system    a. The direction of   i. Collecting the
 that is a PTE according to    the air flow at all   direction of air
 Sec. 63.9322(a).            times must be into    flow; and either
                               the enclosure; and    the facial velocity
                               either                of air through all
                                                     natural draft
                                                     openings according
                                                     to Sec.
                                                     63.9306(d)(1) or
                                                     the pressure drop
                                                     across the
                                                     enclosure according
                                                     to Sec.
                                                     63.9306(d)(2); and
                                                    ii. Maintaining the
                                                     facial velocity of
                                                     air flow through
                                                     all natural draft
                                                     openings or the
                                                     pressure drop at or
                                                     above the facial
                                                     velocity limit or
                                                     pressure drop
                                                     limit, and
                                                     maintaining the
                                                     direction of air
                                                     flow into the
                                                     enclosure at all
                                                     times.
                              b. The average        Follow the
                               facial velocity of    requirements in 3ai
                               air through all       and ii of this
                               natural draft         table.
                               openings in the
                               enclosure must be
                               at least 200 feet
                               per minute; or
                              c. The pressure drop  Follow the
                               across the            requirements in 3ai
                               enclosure must be     and ii of this
                               at least 0.007 inch   table.
                               H2O, as established
                               in Method 204 of
                               appendix M to 40
                               CFR part 51.
-----------------------------
4. Emission capture system    a. The average gas    i. Collecting the
 that is not a PTE according   volumetric flow       gas volumetric flow
 to Sec. 63.9322(a).         rate or duct static   rate or duct static
                               pressure in each      pressure for each
                               duct between a        capture device
                               capture device and    according to Sec.
                               add-on control        63.9306(d);
                               device inlet in any  ii. Reducing the
                               3-hour period must    data to 3-hour
                               not fall below the    block averages; and
                               average volumetric   iii. Maintaining the
                               flow rate or duct     3-hour average gas
                               static pressure       volumetric flow
                               limit established     rate or duct static
                               for that capture      pressure for each
                               device according      capture device at
                               Sec. 63.9306(d).    or above the gas
                                                     volumetric flow
                                                     rate or duct static
                                                     pressure limit.
------------------------------------------------------------------------

Table 3 to Subpart PPPPP of Part 63--Requirements for Initial Compliance 
                             Demonstrations

    As stated in Sec. 63.9321, you must demonstrate initial compliance 
with each emission limitation that applies to you according to the 
following table:

[[Page 44]]



----------------------------------------------------------------------------------------------------------------
 
 
 
----------------------------------------------------------------------------------------------------------------
1. The CO or THC outlet concentration  a. Demonstrate CO or     i. EPA Methods 3A and    You must demonstrate
 emission limitation.                   THC emissions are 20     10 of appendix A to 40   that the outlet
                                        ppmvd or less.           CFR part 60 for CO       concentration of CO or
                                                                 measurement or EPA       THC emissions from the
                                                                 Method 25A of appendix   test cell/stand or
                                                                 A to 40 CFR part 60      emission control
                                                                 for THC measurement;     device is 20 ppmvd or
                                                                 or                       less, corrected to 15
                                                                                          percent O2 content,
                                                                                          using the first 4-hour
                                                                                          rolling average after
                                                                                          a successful
                                                                                          performance
                                                                                          evaluation.
                                                                ii. A CEMS for CO or     This demonstration is
                                                                 THC and O2 at the        conducted immediately
                                                                 outlet of the engine     following a successful
                                                                 test cell/stand or       performance evaluation
                                                                 emission control         of the CEMS as
                                                                 device.                  required in Sec.
                                                                                          63.9320(b). The
                                                                                          demonstration consists
                                                                                          of the first 4-hour
                                                                                          rolling average of
                                                                                          measurements. The CO
                                                                                          or THC concentration
                                                                                          must be corrected to
                                                                                          15 percent O2 content,
                                                                                          dry basis using
                                                                                          Equation 1 in Sec.
                                                                                          63.9320.
--------------------------------------
2. The CO or THC percent reduction     a. Demonstrate a         i. You must conduct an   You must demonstrate
 emission limitation.                   reduction in CO or THC   initial performance      that the reduction in
                                        of 96 percent or more.   test to determine the    CO or THC emissions is
                                                                 capture and control      at least 96 percent
                                                                 efficiencies of the      using the first 4-hour
                                                                 equipment and to         rolling average after
                                                                 establish operating      a successful
                                                                 limits to be achieved    performance
                                                                 on a continuous basis;   evaluation. Your inlet
                                                                 or                       and outlet
                                                                                          measurements must be
                                                                                          on a dry basis and
                                                                                          corrected to 15
                                                                                          percent O2 content.
                                                                ii. A CEMS for CO or     This demonstration is
                                                                 THC and O2 at both the   conducted immediately
                                                                 inlet and outlet of      following a successful
                                                                 the emission control     performance evaluation
                                                                 device.                  of the CEMS as
                                                                                          required in Sec.
                                                                                          63.9320(b). The
                                                                                          demonstration consists
                                                                                          of the first 4-hour
                                                                                          rolling average of
                                                                                          measurements. The
                                                                                          inlet and outlet CO or
                                                                                          THC concentrations
                                                                                          must be corrected to
                                                                                          15 percent O2 content
                                                                                          using Equation 1 in
                                                                                          Sec. 63.9320. The
                                                                                          reduction in CO or THC
                                                                                          is calculated using
                                                                                          Equation 2 in Sec.
                                                                                          63.9320.
----------------------------------------------------------------------------------------------------------------

 Table 4 to Subpart PPPPP of Part 63--Initial Compliance With Emission 
                               Limitations

    As stated in Sec. 63.9330, you must demonstrate initial compliance 
with each emission limitation that applies to you according to the 
following table:

------------------------------------------------------------------------
 
             For the . . .
------------------------------------------------------------------------
1. CO or THC concentration emission      The first 4-hour rolling
 limitation.                              average CO or THC
                                          concentration is 20 ppmvd or
                                          less, corrected to 15 percent
                                          O2 content.
----------------------------------------
2. CO or THC percent reduction emission  The first 4-hour rolling
 limitation.                              average reduction in CO or THC
                                          is 96 percent or more, dry
                                          basis, corrected to 15 percent
                                          O2 content.
------------------------------------------------------------------------


[[Page 45]]

Table 5 to Subpart PPPPP of Part 63--Continuous Compliance with Emission 
                               Limitations

    As stated in Sec. 63.9340, you must demonstrate continuous 
compliance with each emission limitation that applies to you according 
to the following table:

------------------------------------------------------------------------
 
------------------------------------------------------------------------
1. CO or THC concentration    a. Demonstrate CO or  i. Collecting the
 emission limitation.          THC emissions are     CPMS data according
                               20 ppmvd or less      to Sec.
                               over each 4-hour      63.9306(a),
                               rolling averaging     reducing the
                               period.               measurements to 1-
                                                     hour averages; or
                                                    ii. Collecting the
                                                     CEMS data according
                                                     to Sec.
                                                     63.9307(a),
                                                     reducing the
                                                     measurements to 1-
                                                     hour averages,
                                                     correcting them to
                                                     15 percent O2
                                                     content, dry basis,
                                                     according to Sec.
                                                     63.9320;
-----------------------------
2. CO or THC percent          a. Demonstrate a      i. Collecting the
 reduction emission            reduction in CO or    CPMS data according
 limitation.                   THC of 96 percent     to Sec.
                               or more over each 4-  63.9306(a),
                               hour rolling          reducing the
                               averaging period.     measurements to 1-
                                                     hour averages; or
                                                    ii. Collecting the
                                                     CEMS data according
                                                     to Sec.
                                                     63.9307(b),
                                                     reducing the
                                                     measurements to 1-
                                                     hour averages,
                                                     correcting them to
                                                     15 percent O2
                                                     content, dry basis,
                                                     calculating the CO
                                                     or THC percent
                                                     reduction according
                                                     to Sec. 63.9320.
------------------------------------------------------------------------

      Table 6 to Subpart PPPPP of Part 63--Requirements for Reports

    As stated in Sec. 63.9350, you must submit each report that applies 
to you according to the following table:

------------------------------------------------------------------------
 
 
 
 
 
 
------------------------------------------------------------------------
1. Compliance report........  a. If there are no    Semiannually,
                               deviations from the   according to the
                               emission              requirements in
                               limitations that      Sec. 63.9350.
                               apply to you, a
                               statement that
                               there were no
                               deviations from the
                               emission
                               limitations during
                               the reporting
                               period.
                              b. If there were no   Semiannually,
                               periods during        according to the
                               which the CEMS or     requirements in
                               CPMS were out of      Sec. 63.9350.
                               control as
                               specified in Sec.
                               63.8(c)(7), a
                               statement that
                               there were no
                               periods during
                               which the CEMS or
                               CPMS was out of
                               control during the
                               reporting period.
                              c. If you have a      Semiannually,
                               deviation from any    according to the
                               emission limitation   requirements in
                               during the            Sec. 63.9350.
                               reporting period,
                               the report must
                               contain the
                               information in Sec.
                                 63.9350(c).
                              d. If there were      Semiannually,
                               periods during        according to the
                               which the CEMS or     requirements in
                               CPMS were out of      Sec. 63.9350.
                               control, as
                               specified in Sec.
                               63.8(c)(7), that
                               report must contain
                               the information in
                               Sec. 63.9350(d).
                              e. If you had an SSM  Semiannually,
                               of a control device   according to the
                               or associated         requirements in
                               monitoring            Sec. 63.9350.
                               equipment during
                               the reporting
                               period, the report
                               must include the
                               information in Sec.
                                 63.10(d)(5)(i).
------------------------------------------------------------------------

Table 7 to Subpart PPPPP of Part 63--Applicability of General Provisions 
                            to Subpart PPPPP

    As stated in 63.9365, you must comply with the General Provisions in 
Sec. Sec. 63.1 through 63.15 that apply to you according to the 
following table:

[[Page 46]]



----------------------------------------------------------------------------------------------------------------
                                                                                            Applies to subpart
               Citation                        Subject             Brief description              PPPPP
----------------------------------------------------------------------------------------------------------------
Sec. 63.1(a)(1)....................  Applicability..........  General applicability    Yes. Additional terms
                                                                 of the General           defined in Sec.
                                                                 Provisions.              63.9375.
--------------------------------------
Sec. 63.1(a)(2)-(4)................  Applicability..........  Applicability of source  Yes.
                                                                 categories.
--------------------------------------
Sec. 63.1(a)(5)....................  [Reserved].............
--------------------------------------
Sec. 63.1(a)(6)-(7)................  Applicability..........  Contact for source       Yes.
                                                                 category information;
                                                                 extension of
                                                                 compliance through
                                                                 early reduction.
--------------------------------------
Sec. 63.1(a)(8)....................  Applicability..........  Establishment of State   No. Refers to State
                                                                 rules or programs.       programs.
--------------------------------------
Sec. 63.1(a)(9)....................  [Reserved].............
--------------------------------------
Sec. 63.1(a)(10)-(14)..............  Applicability..........  Explanation of time      Yes.
                                                                 periods, postmark
                                                                 deadlines.
--------------------------------------
Sec. 63.1(b)(1)....................  Applicability..........  Initial applicability..  Yes. Subpart PPPPP
                                                                                          clarifies
                                                                                          applicability at Sec.
                                                                                           63.9285.
--------------------------------------
Sec. 63.1(b)(2)....................  Applicability..........  Title V operating        Yes. All major affected
                                                                 permit-reference to      sources are required
                                                                 part 70.                 to obtain a Title V
                                                                                          permit.
--------------------------------------
Sec. 63.1(b)(3)....................  Applicability..........  Record of applicability  Yes.
                                                                 determination.
--------------------------------------
Sec. 63.1(c)(1)....................  Applicability..........  Applicability after      Yes. Subpart PPPPP
                                                                 standards are set.       clarifies the
                                                                                          applicability of each
                                                                                          paragraph of subpart A
                                                                                          to sources subject to
                                                                                          subpart PPPPP.
--------------------------------------
Sec. 63.1(c)(2)....................  Applicability..........  Title V permit           No. Area sources are
                                                                 requirement for area     not subject to subpart
                                                                 sources.                 PPPPP.
--------------------------------------
Sec. 63.1(c)(3)....................  [Reserved].............
--------------------------------------
Sec. 63.1(c)(4)....................  Applicability..........  Extension of compliance  No. Existing sources
                                                                 for existing sources.    are not covered by the
                                                                                          substantive control
                                                                                          requirements of
                                                                                          subpart PPPPP.
--------------------------------------
Sec. 63.1(c)(5)....................  Applicability..........  Notification             Yes.
                                                                 requirements for an
                                                                 area source becoming a
                                                                 major source.
--------------------------------------
Sec. 63.1(d).......................  [Reserved].............
--------------------------------------
Sec. 63.1(e).......................  Applicability..........  Applicability of permit  Yes.
                                                                 program before a
                                                                 relevant standard has
                                                                 been set.
--------------------------------------
Sec. 63.2..........................  Definitions............  Definitions for Part 63  Yes. Additional
                                                                 standards.               definitions are
                                                                                          specified in Sec.
                                                                                          63.9375.
--------------------------------------
Sec. 63.3..........................  Units and Abbreviations  Units and abbreviations  Yes.
                                                                 for Part 63 standards.
--------------------------------------
Sec. 63.4..........................  Prohibited Activities..  Prohibited activities;   Yes.
                                                                 compliance date;
                                                                 circumvention,
                                                                 severability.
--------------------------------------
Sec. 63.5(a).......................  Construction/            Construction and         Yes.
                                        Reconstruction.          reconstruction--applic
                                                                 ability.
--------------------------------------
Sec. 63.5(b)(1)....................  Construction/            Requirements upon        Yes.
                                        Reconstruction.          construction or
                                                                 reconstruction.
--------------------------------------
Sec. 63.5(b)(2)....................  [Reserved].
--------------------------------------

[[Page 47]]

 
Sec. 63.5(b)(3)....................  Construction/            Approval of              Yes.
                                        Reconstruction.          construction.
--------------------------------------
Sec. 63.5(b)(4)....................  Construction/            Notification of          Yes.
                                        Reconstruction.          construction.
--------------------------------------
Sec. 63.5(b)(5)....................  Construction/            Compliance.............  Yes.
                                        Reconstruction.
--------------------------------------
Sec. 63.5(b)(6)....................  Construction/            Addition of equipment..  Yes.
                                        Reconstruction.
--------------------------------------
Sec. 63.5(c).......................  [Reserved]
--------------------------------------
Sec. 63.5(d).......................  Construction/            Application for          Yes.
                                        Reconstruction.          construction
                                                                 reconstruction.
--------------------------------------
Sec. 63.5(e).......................  Construction/            Approval of              Yes.
                                        Reconstruction.          construction or
                                                                 reconstruction.
--------------------------------------
Sec. 63.5(f).......................  Construction/            Approval of              Yes.
                                        Reconstruction.          construction or
                                                                 reconstruction based
                                                                 on prior State review.
--------------------------------------
Sec. 63.6(a).......................  Applicability..........  Applicability of         Yes.
                                                                 standards and
                                                                 monitoring
                                                                 requirements.
--------------------------------------
Sec. 63.6(b)(1)-(2)................  Compliance Dates for     Standards apply at       Yes.
                                        New and Reconstructed    effective date; 3
                                        Sources.                 years after effective
                                                                 date; upon startup; 10
                                                                 years after
                                                                 construction or
                                                                 reconstruction
                                                                 commences for 112(f).
--------------------------------------
Sec. 63.6(b)(3)....................  Compliance Dates for     Compliance dates for     No. Compliance is
                                        New and Reconstructed    sources constructed or   required by startup or
                                        Sources.                 reconstructed before     effective date.
                                                                 effective date.
--------------------------------------
Sec. 63.6(b)(4)....................  Compliance Dates for     Compliance dates for     Yes.
                                        New and Reconstructed    sources also subject
                                        Sources.                 to Sec. 112(f)
                                                                 standards.
--------------------------------------
Sec. 63.6(b)(5)....................  Compliance Dates for     Notification...........  Yes.
                                        New and Reconstructed
                                        Sources.
--------------------------------------
Sec. 63.6(b)(6)....................  [Reserved].
--------------------------------------
Sec. 63.6(b)(7)....................  Compliance Dates for     Compliance dates for     Yes.
                                        New and Reconstructed    new and reconstructed
                                        Sources.                 area sources that
                                                                 become major.
--------------------------------------
Sec. 63.6(c)(1)-(2)................  Compliance Dates for     Effective date           No. Existing sources
                                        Existing Sources.        establishes compliance   are not covered by the
                                                                 date.                    substantive control
                                                                                          requirements of
                                                                                          subpart PPPPP.
--------------------------------------
Sec. 63.6(c)(3)-(4)................  [Reserved].
--------------------------------------
Sec. 63.6(c)(5)....................  Compliance Dates for     Compliance dates for     Yes. If the area source
                                        Existing Sources.        existing area sources    become a major source
                                                                 that becomes major.      by addition or
                                                                                          reconstruction, the
                                                                                          added or reconstructed
                                                                                          portion will be
                                                                                          subject to subpart
                                                                                          PPPPP.
--------------------------------------
Sec. 63.6(d).......................  [Reserved].
--------------------------------------
Sec. 63.6(e)(1)-(2)................  Operation and            Operation and            Yes. Except that you
                                        Maintenance              maintenance.             are not required to
                                        Requirements.                                     have an SSMP for
                                                                                          control devices and
                                                                                          associated monitoring
                                                                                          equipment.
--------------------------------------
Sec. 63.6(e)(3)....................  SSMP...................  1. Requirement for SSM   Yes.You must develop an
                                                                 and SSMP.                SSMP for each control
                                                                2. Content of SSMP.....   device and associated
                                                                                          monitoring equipment.
--------------------------------------

[[Page 48]]

 
Sec. 63.6(f)(1)....................  Compliance Except        You must comply with     Yes, but you must
                                        During SSM.              emission standards at    comply with emission
                                                                 all times except         standards at all times
                                                                 during SSM of control    except during SSM of
                                                                 devices or associated    control devices and
                                                                 monitoring equipment.    associated monitoring
                                                                                          equipment only.
--------------------------------------
Sec. 63.6(f)(2)-(3)................  Methods for Determining  Compliance based on      Yes.
                                        Compliance.              performance test,
                                                                 operation and
                                                                 maintenance plans,
                                                                 records, inspection.
--------------------------------------
Sec. 63.6(g)(1)-(3)................  Alternative Standard...  Procedures for getting   Yes.
                                                                 an alternative
                                                                 standard.
--------------------------------------
Sec. 63.6(h).......................  Opacity/Visible          Requirements for         No. Subpart PPPPP does
                                        Emission (VE)            opacity/VE standards.    not establish opacity/
                                        Standards.                                        VE standards and does
                                                                                          not require continuous
                                                                                          opacity monitoring
                                                                                          systems (COMS).
--------------------------------------
Sec. 63.6(i)(1)-(14)...............  Compliance Extension...  Procedures and criteria  No. Compliance
                                                                 for Administrator to     extension provisions
                                                                 grant compliance         apply to existing
                                                                 extension.               sources, which do not
                                                                                          have emission
                                                                                          limitations in subpart
                                                                                          PPPPP.
--------------------------------------
Sec. 63.6(j).......................  Presidential Compliance  President may exempt     Yes.
                                        Exemption.               source category from
                                                                 requirement to comply
                                                                 with rule.
--------------------------------------
Sec. 63.7(a)(1)-(2)................  Performance Test Dates.  Dates for conducting     Yes.
                                                                 initial performance
                                                                 testing and other
                                                                 compliance
                                                                 demonstrations: Must
                                                                 conduct within 180
                                                                 days after first
                                                                 subject to rule.
--------------------------------------
Sec. 63.7(a)(3)....................  Section 114 Authority..  Administrator may        Yes.
                                                                 require a performance
                                                                 test under CAA Section
                                                                 114 at any time.
--------------------------------------
Sec. 63.7(b)(1)....................  Notification             Must notify              Yes.
                                        Performance Test.        Administrator 60 days
                                                                 before the test.
--------------------------------------
Sec. 63.7(b)(2)....................  Notification of          If have to reschedule    Yes.
                                        Rescheduling.            performance test, must
                                                                 notify Administrator 5
                                                                 days before schedule
                                                                 date of rescheduled
                                                                 date.
--------------------------------------
Sec. 63.7(c).......................  Quality Assurance/Test   1. Requirement to        Yes.
                                        Plan.                    submit site-specific
                                                                 test plan 60 days
                                                                 before the test or on
                                                                 date Administrator
                                                                 agrees with.
                                                                2. Test plan approval    Yes.
                                                                 procedures.
                                                                3. Performance audit     Yes.
                                                                 requirements.
                                                                4. Internal and          Yes.
                                                                 external QA procedures
                                                                 for testing.
--------------------------------------
Sec. 63.7(d).......................  Testing Facilities.....  Requirements for         Yes.
                                                                 testing facilities.
--------------------------------------

[[Page 49]]

 
Sec. 63.7(e)(1)....................  Conditions for           Performance tests must   Yes.
                                        Conducting Performance   be conducted under
                                        Tests.                   representative
                                                                 conditions; cannot
                                                                 conduct performance
                                                                 tests during SSM; not
                                                                 a violation to exceed
                                                                 standard during SSM.
--------------------------------------
Sec. 63.7(e)(2)....................  Conditions for           Must conduct according   Yes.
                                        Conducting Performance   to rule and EPA test
                                        Tests.                   methods unless
                                                                 Administrator approves
                                                                 alternative.
--------------------------------------
Sec. 63.7(e)(3)....................  Test Run Duration......  1. Must have three test  Yes.
                                                                 runs of at least 1
                                                                 hour each.
                                                                2. Compliance is based   Yes.
                                                                 on arithmetic mean of
                                                                 three runs.
                                                                3. Conditions when data  Yes.
                                                                 from an additional
                                                                 test run can be used.
--------------------------------------
Sec. 63.7(e)(4)....................  Other Performance        Administrator may        Yes.
                                        Testing.                 require other testing
                                                                 under section 114 of
                                                                 the CAA.
--------------------------------------
Sec. 63.7(f).......................  Alternative Test Method  Procedures by which      Yes.
                                                                 Administrator can
                                                                 grant approval to use
                                                                 an alternative test
                                                                 method.
--------------------------------------
Sec. 63.7(g).......................  Performance Test Data    1. Must include raw      Yes.
                                        Analysis.                data in performance
                                                                 test report.
                                                                2. Must submit           Yes.
                                                                 performance test data
                                                                 60 days after end of
                                                                 test with the
                                                                 Notification of
                                                                 Compliance Status.
                                                                3. Keep data for 5       Yes.
                                                                 years.
--------------------------------------
Sec. 63.7(h).......................  Waiver of Tests........  Procedures for           Yes.
                                                                 Administrator to waive
                                                                 performance test.
Sec. 63.8(a)(1)....................  Applicability of         Subject to all           Yes. Subpart PPPPP
                                        Monitoring               monitoring               contains specific
                                        Requirements.            requirements in          requirements for
                                                                 standard.                monitoring at Sec.
                                                                                          63.9325.
--------------------------------------
Sec. 63.8(a)(2)....................  Performance              Performance              Yes.
                                        Specifications.          Specifications in
                                                                 appendix B of part 60
                                                                 apply.
--------------------------------------
Sec. 63.8(a)(3)....................  [Reserved]
--------------------------------------
Sec. 63.8(a)(4)....................  Monitoring with Flares.  Unless your rule says    No. Subpart PPPPP does
                                                                 otherwise, the           not have monitoring
                                                                 requirements for         requirements for
                                                                 flares in 63.11 apply.   flares.
--------------------------------------
Sec. 63.8(b)(1)....................  Monitoring.............  Must conduct monitoring  Yes.
                                                                 according to standard
                                                                 unless Administrator
                                                                 approves alternative.
--------------------------------------
Sec. 63.8(b)(2)-(3)................  Multiple Effluents and   1. Specific              Yes.
                                        Multiple Monitoring      requirements for
                                        Systems.                 installing monitoring
                                                                 systems.
                                                                2. Must install on each  Yes.
                                                                 effluent before it is
                                                                 combined and before it
                                                                 is released to the
                                                                 atmosphere unless
                                                                 Administrator approves
                                                                 otherwise.

[[Page 50]]

 
                                                                3. If more than one      Yes.
                                                                 monitoring system on
                                                                 an emission point,
                                                                 must report all
                                                                 monitoring system
                                                                 results, unless one
                                                                 monitoring system is a
                                                                 backup.
--------------------------------------
Sec. 63.8(c)(1)....................  Monitoring System        Maintain monitoring      Yes.
                                        Operation and            system in a manner
                                        Maintenance.             consistent with good
                                                                 air pollution control
                                                                 practices.
--------------------------------------
Sec. 63.8(c)(1)(i).................  Routine and Predictable  1. Follow the SSMP for   Yes.
                                        CMS Malfunctions.        routine repairs of CMS.
                                                                2. Keep parts for        Yes.
                                                                 routine repairs of CMS
                                                                 readily available.
                                                                3. Reporting             Yes.
                                                                 requirements for SSM
                                                                 when action is
                                                                 described in SSMP.
--------------------------------------
Sec. 63.8(c)(1)(ii)................  SSM of CMS Not in SSMP.  Reporting requirements   Yes.
                                                                 for SSM of CMS when
                                                                 action is not
                                                                 described in SSMP.
--------------------------------------
Sec. 63.8(c)(1)(iii)...............  Compliance with          1. How Administrator     Yes.
                                        Operation and            determines if source
                                        Maintenance              complying with
                                        Requirements.            operation and
                                                                 maintenance
                                                                 requirements.
                                                                2. Review of source O&M
                                                                 procedures, records,
                                                                 manufacturer's
                                                                 instructions and
                                                                 recommendations, and
                                                                 inspection.
--------------------------------------
Sec. 63.8(c)(2)-(3)................  Monitoring System        1. Must install to get   Yes.
                                        Installation.            representative
                                                                 emission of parameter
                                                                 measurements.
                                                                2. Must verify           Yes.
                                                                 operational status
                                                                 before or at
                                                                 performance test.
--------------------------------------
Sec. 63.8(c)(4)....................  Continuous Monitoring    1. CMS must be           No. Follow specific
                                        System (CMS)             operating except         requirements in Sec.
                                        Requirements.            during breakdown, out    63.9335(a) and (b) of
                                                                 of control, repair,      subpart PPPPP.
                                                                 maintenance, and high-
                                                                 level calibration
                                                                 drifts.
                                                                2. COMS must have a      No. Follow specific
                                                                 minimum of one cycle     requirements in Sec.
                                                                 of sampling and          63.9335(a) and (b) of
                                                                 analysis for each        subpart PPPP.
                                                                 successive 10-second
                                                                 period and one cycle
                                                                 of data recording for
                                                                 each successive 6-
                                                                 minute period.
                                                                3. CEMS must have a      No. Follow specific
                                                                 minimum of one cycle     requirements in Sec.
                                                                 of operation for each    63.9335(a) and (b) of
                                                                 successive 15-minute     subpart PPPPP.
                                                                 period.
--------------------------------------
Sec. 63.8(c)(5)....................  COMS Minimum Procedures  COMS minimum procedures  No. Subpart PPPPP does
                                                                                          not have opacity/VE
                                                                                          standards.
--------------------------------------
Sec. 63.8(c)(6)-(8)................  CMS Requirements.......  Zero and high-level      Yes. Except that PPPP
                                                                 calibration check        does not require COMS.
                                                                 requirements, out-of-
                                                                 control periods.
--------------------------------------
Sec. 63.8(d).......................  CMS Quality Control....  1. Requirements for CMS  Yes.
                                                                 quality control,
                                                                 including calibration,
                                                                 etc.
                                                                2. Must keep quality     Yes.
                                                                 control plan on record
                                                                 for 5 years. Keep old
                                                                 versions for 5 years
                                                                 after revisions.
--------------------------------------

[[Page 51]]

 
Sec. 63.8(e).......................  CMS Performance          Notification,            Yes. Except for Sec.
                                        Evaluation.              performance evaluation   63.8(e)(5)(ii), which
                                                                 test plan, reports.      applies to COMS.
--------------------------------------
Sec. 63.8(f)(1)-(5)................  Alternative Monitoring   Procedures for           Yes.
                                        Method.                  Administrator to
                                                                 approve alternative
                                                                 monitoring.
--------------------------------------
Sec. 63.8(f)(6)....................  Alternative to Relative  Procedures for           Yes.
                                        Accuracy Test.           Administrator to
                                                                 approve alternative
                                                                 relative accuracy
                                                                 tests for CEMS.
--------------------------------------
Sec. 63.8(g).......................  Data Reduction.........  1. COMS 6-minute         Yes. Except that
                                                                 averages calculated      provisions for COMS
                                                                 over at least 36         are not applicable.
                                                                 evenly spaced data       Averaging periods for
                                                                 points.                  demonstrating
                                                                2. CEMS 1-hour averages   compliance are
                                                                 computed over at least   specified at Sec.
                                                                 4 equally spaced data    63.9340.
                                                                 points.
--------------------------------------
Sec. 63.8(g)(5)....................  Data Reduction.........  Data that cannot be      No. Specific language
                                                                 used in computing        is located at Sec.
                                                                 averages for CEMS and    63.9335(a).
                                                                 COMS.
--------------------------------------
Sec. 63.9(a).......................  Notification             Applicability and State  Yes.
                                        Requirements.            delegation.
--------------------------------------
Sec. 63.9(b)(1)-(5)................  Initial Notifications..  1. Submit notification   Yes.
                                                                 subject 120 days after
                                                                 effective date.
                                                                2. Notification of       Yes.
                                                                 intent to construct/
                                                                 reconstruct;
                                                                 notification of
                                                                 commencement of
                                                                 construct/
                                                                 reconstruct;
                                                                 notification of
                                                                 startup.
                                                                3. Contents of each....  Yes.
--------------------------------------
Sec. 63.9(c).......................  Request for Compliance   Can request if cannot    No. Compliance
                                        Extension.               comply by date or if     extensions do not
                                                                 installed BACT/LAER.     apply to new or
                                                                                          reconstructed sources.
--------------------------------------
Sec. 63.9(d).......................  Notification of Special  For sources that         Yes.
                                        Compliance               commence construction
                                        Requirements for New     between proposal and
                                        Source.                  promulgation and want
                                                                 to comply 3 years
                                                                 after effective date.
--------------------------------------
Sec. 63.9(e).......................  Notification of          Notify Administrator 60  No. Subpart PPPPP does
                                        Performance Test.        days prior.              not require
                                                                                          performance testing.
--------------------------------------
Sec. 63.9(f).......................  Notification of Opacity/ Notify Administrator 30  No. Subpart PPPPP does
                                        VE Test.                 days prior.              not have opacity/VE
                                                                                          standards.
--------------------------------------
Sec. 63.9(g)(1)....................  Additional               Notification of          Yes.
                                        Notifications when       performance evaluation.
                                        Using CMS.
--------------------------------------
Sec. 63.9(g)(2)....................  Additional               Notification of use of   No. Subpart PPPPP does
                                        Notifications when       COMS data.               not contain opacity or
                                        Using CMS.                                        VE standards.
--------------------------------------
Sec. 63.9(g)(3)....................  Additional               Notification that        Yes. If alternative is
                                        Notifications when       exceeded criterion for   in use.
                                        Using CMS.               relative accuracy.
--------------------------------------
Sec. 63.9(h)(1)-(6)................  Notification of          1. Contents............  Yes.
                                        Compliance Status.
                                                                2. Due 60 days after     Yes.
                                                                 end of performance
                                                                 test or other
                                                                 compliance
                                                                 demonstration, except
                                                                 for opacity/VE, which
                                                                 are due 30 days after.
                                                                3. When to submit to     Yes.
                                                                 Federal vs. State
                                                                 authority.
--------------------------------------

[[Page 52]]

 
Sec. 63.9(i).......................  Adjustment of Submittal  Procedures for           Yes.
                                        Deadlines.               Administrator to
                                                                 approve change in when
                                                                 notifications must be
                                                                 submitted.
--------------------------------------
Sec. 63.9(j).......................  Change in Previous       Must submit within 15    Yes.
                                        Information.             days after the change.
--------------------------------------
Sec. 63.10(a)......................  Recordkeeping/Reporting  1. Applies to all,       Yes.
                                                                 unless compliance
                                                                 extension.
                                                                2. When to submit to     Yes.
                                                                 Federal vs. State
                                                                 authority.
                                                                3. Procedures for        Yes.
                                                                 owners of more than
                                                                 one source.
--------------------------------------
Sec. 63.10(b)(1)...................  Recordkeeping/Reporting  1. General requirements  Yes.
                                                                2. Keep all records      Yes.
                                                                 readily available.
                                                                3. Keep for 5 years....  Yes.
--------------------------------------
Sec. 63.10(b)(2)(i)-(v)............  Records Related to SSM.  1. Occurrence of each    Yes.
                                                                 of operation (process
                                                                 equipment).
                                                                2. Occurrence of each    Yes.
                                                                 malfunction of air
                                                                 pollution equipment.
                                                                3. Maintenance on air    Yes.
                                                                 pollution control
                                                                 equipment.
                                                                4. Actions during SSM..  Yes.
                                                                5. All information       Yes.
                                                                 necessary to
                                                                 demonstrate
                                                                 conformance with the
                                                                 SSMP.
--------------------------------------
Sec. 63.10(b)(2)(vi)-(xi)..........  CMS Records............  Malfunctions,            Yes.
                                                                 inoperative, out of
                                                                 control.
--------------------------------------
Sec. 63.10(b)(2)(xii)..............  Records................  Records when under       Yes.
                                                                 waiver.
--------------------------------------
Sec. 63.10(b)(2)(xiii).............  Records................  Records when using       Yes.
                                                                 alternative to
                                                                 relative accuracy test.
--------------------------------------
Sec. 63.10(b)(2)(xiv)..............  Records................  All documentation        Yes.
                                                                 supporting initial
                                                                 notification and
                                                                 notification of
                                                                 compliance status.
--------------------------------------
Sec. 63.10(b)(3)...................  Records................  Applicability            Yes.
                                                                 determinations.
--------------------------------------
Sec. 63.10(c)(1)-(6), (9)-(15).....  Records................  Additional records for   Yes.
                                                                 CEMS.
--------------------------------------
Sec. 63.10(c)(7)-(8)...............  Records................  Records of excess        No. Specific language
                                                                 emissions and            is located at Sec.
                                                                 parameter monitoring     63.9355 of subpart
                                                                 exceedances for CMS.     PPPPP.
--------------------------------------
Sec. 63.10(d)(1)...................  General Reporting        Requirement to report..  Yes.
                                        Requirements.
--------------------------------------
Sec. 63.10(d)(2)...................  Report of Performance    When to submit to        Yes.
                                        Test Results.            Federal or State
                                                                 authority.
--------------------------------------
Sec. 63.10(d)(3)...................  Reporting Opacity or VE  What to report and when  No. Subpart PPPPP does
                                        Observations.                                     not have opacity/VE
                                                                                          standards.
--------------------------------------
Sec. 63.10(d)(4)...................  Progress Reports.......  Must submit progress     No. Compliance
                                                                 reports on schedule if   extensions do not
                                                                 under compliance         apply to new or
                                                                 extension.               reconstructed sources.
--------------------------------------
Sec. 63.10(d)(5)...................  SSM Reports............  Contents and submission  Yes.
--------------------------------------
Sec. 63.10(e)(1) and (2)(i)........  Additional CMS Reports.  Additional CMS reports.  Yes.
--------------------------------------
Sec. 63.10(e)(2)(ii)...............  Additional CMS Reports.  COMS-related report....  No. Subpart PPPPP does
                                                                                          not require COMS.
--------------------------------------

[[Page 53]]

 
Sec. 63.10(e)(3)...................  Additional CMS Reports.  Excess emissions and     No. Specific language
                                                                 parameter exceedances    is located in Sec.
                                                                 reports.                 63.9350 of subpart
                                                                                          PPPPP.
--------------------------------------
Sec. 63.10(e)(4)...................  Additional CMS Reports.  Reporting COMS data....  No. Subpart PPPPP does
                                                                                          not require COMS.
--------------------------------------
Sec. 63.10(f)......................  Waiver for               Procedures for           Yes.
                                        Recordkeeping/           Administrator to waive.
                                        Reporting.
--------------------------------------
Sec. 63.11.........................  Control Device           Requirements for flares  No. Subpart PPPPP does
                                        Requirements.                                     not specify use of
                                                                                          flares for compliance.
--------------------------------------
Sec. 63.12.........................  State Authority and      State authority to       Yes.
                                        Delegations.             enforce standards.
--------------------------------------
Sec. 63.13.........................  Addresses of State Air   Addresses where          Yes.
                                        Pollution Control        reports,
                                        Offices and EPA          notifications, and
                                        Regional Offices.        requests are sent.
--------------------------------------
Sec. 63.14.........................  Incorporations by        Test methods             Yes. ASTM D 6522-00 and
                                        Reference.               incorporated by          ANSI/ASME PTC 19.10-
                                                                 reference.               1981 (incorporated by
                                                                                          reference-See Sec.
                                                                                          63.14).
--------------------------------------
Sec. 63.15.........................  Availability of          Public and confidential  Yes.
                                        Information and          information.
                                        Confidentiality.
----------------------------------------------------------------------------------------------------------------



 Subpart QQQQQ_National Emission Standards for Hazardous Air Pollutants 
---------------------------------------------------------------------------
             for Friction Materials Manufacturing Facilities

    Source: 67 FR 64506, Oct. 18, 2002, unless otherwise noted.

                        What This Subpart Covers



Sec. 63.9480  What is the purpose of this subpart?

    This subpart establishes national emission standards for hazardous 
air pollutants (NESHAP) for friction materials manufacturing facilities 
that use a solvent-based process. This subpart also establishes 
requirements to demonstrate initial and continuous compliance with all 
applicable emission limitations in this subpart.



Sec. 63.9485  Am I subject to this subpart?

    (a) You are subject to this subpart if you own or operate a friction 
materials manufacturing facility (as defined in Sec. 63.9565) that is 
(or is part of) a major source of hazardous air pollutants (HAP) 
emissions on the first compliance date that applies to you, as specified 
in Sec. 63.9495. Your friction materials manufacturing facility is a 
major source of HAP if it emits or has the potential to emit any single 
HAP at a rate of 9.07 megagrams (10 tons) or more per year or any 
combination of HAP at a rate of 22.68 megagrams (25 tons) or more per 
year.
    (b) The requirements in this subpart do not apply to research and 
development facilities, as defined in section 112(c)(7) of the Clean Air 
Act.



Sec. 63.9490  What parts of my plant does this subpart cover?

    (a) This subpart applies to each new, reconstructed, or existing 
affected source at your friction materials manufacturing facility.
    (b) The affected source covered by this subpart is each new, 
reconstructed, or existing solvent mixer (as defined in Sec. 63.9565) 
at your friction materials manufacturing facility.
    (c) A solvent mixer at your friction materials manufacturing 
facility is new if you commence construction of the solvent mixer after 
October 18, 2002. An affected source is reconstructed if it meets the 
definition of ``reconstruction'' in Sec. 63.2, and reconstruction is 
commenced after October 18, 2002.

[[Page 54]]

    (d) A solvent mixer at your friction materials manufacturing 
facility is existing if it is not new or reconstructed.



Sec. 63.9495  When do I have to comply with this subpart?

    (a) If you have an existing solvent mixer, you must comply with each 
of the requirements for existing sources no later than October 18, 2005.
    (b) If you have a new or reconstructed solvent mixer and its initial 
startup date is after October 18, 2002, you must comply with the 
requirements for new and reconstructed sources upon initial startup.
    (c) If your friction materials manufacturing facility is an area 
source that increases its emissions or its potential to emit such that 
it becomes a (or part of a) major source of HAP emissions, then 
paragraphs (c)(1) and (2) of this section apply.
    (1) For any portion of the area source that becomes a new or 
reconstructed affected source, you must comply with the requirements for 
new and reconstructed sources upon startup or no later than October 18, 
2002, whichever is later.
    (2) For any portion of the area source that becomes an existing 
affected source, you must comply with the requirements for existing 
sources no later than 1 year after the area source becomes a major 
source or no later than October 18, 2005, whichever is later.
    (d) You must meet the notification and schedule requirements in 
Sec. 63.9535. Several of the notifications must be submitted before the 
compliance date for your affected source.

                          Emission Limitations



Sec. 63.9500  What emission limitations must I meet?

    (a) For each new, reconstructed, or existing large solvent mixer at 
your friction materials manufacturing facility, you must limit HAP 
solvent emissions to the atmosphere to no more than 30 percent of that 
which would otherwise be emitted in the absence of solvent recovery and/
or solvent substitution, based on a 7-day block average.
    (b) For each new, reconstructed, or existing small solvent mixer at 
your friction materials manufacturing facility, you must limit HAP 
solvent emissions to the atmosphere to no more than 15 percent of that 
which would otherwise be emitted in the absence of solvent recovery and/
or solvent substitution, based on a 7-day block average.

                     General Compliance Requirements



Sec. 63.9505  What are my general requirements for complying with this 
subpart?

    (a) You must be in compliance with the emission limitation in this 
subpart at all times, except during periods of startup, shutdown, or 
malfunction.
    (b) You must always operate and maintain your affected source, 
including air pollution control and monitoring equipment, according to 
the provisions in Sec. 63.6(e)(1)(i).
    (c) You must develop and implement a written startup, shutdown, and 
malfunction plan according to the provisions in Sec. 63.6(e)(3).

              Initial Compliance Demonstration Requirements



Sec. 63.9510  By what date must I conduct my initial compliance 
demonstration?

    (a) If you use a solvent recovery system and/or solvent 
substitution, you must conduct your initial compliance demonstration 
within 7 calendar days after the compliance date that is specified for 
your source in Sec. 63.9495.
    (b) If you use a control technique other than a solvent recovery 
system and/or solvent substitution, you must comply with the provisions 
in Sec. 63.9570.



Sec. 63.9515  How do I demonstrate initial compliance with the emission 
limitation that applies to me?

    (a) You have demonstrated initial compliance for each new, 
reconstructed, or existing large solvent mixer subject to the emission 
limitation in Sec. 63.9500(a) if the HAP solvent discharged to the 
atmosphere during the first 7 days after the compliance date, determined 
according to the provisions in Sec. 63.9520, does not exceed a 7-day 
block average of 30 percent of that which would otherwise be emitted in 
the absence of solvent recovery and/or solvent substitution.

[[Page 55]]

    (b) You have demonstrated initial compliance for each new, 
reconstructed, or existing small solvent mixer subject to the emission 
limitation in Sec. 63.9500(b) if the HAP solvent discharged to the 
atmosphere during the first 7 days after the compliance date, determined 
according to the provisions in Sec. 63.9520, does not exceed a 7-day 
block average of 15 percent of that which would otherwise be emitted in 
the absence of solvent recovery and/or solvent substitution.
    (c) You must submit a notification of compliance status containing 
the results of the initial compliance demonstration according to Sec. 
63.9535(e).



Sec. 63.9520  What procedures must I use to demonstrate initial compliance?

    (a) If you use a solvent recovery system, you must use the 
procedures in paragraphs (a)(1) through (8) of this section to 
demonstrate initial compliance with the emission limitations in Sec. 
63.9500(a) and (b).
    (1) Record the date and time of each mix batch.
    (2) Record the identity of each mix batch using a unique batch ID, 
as defined in Sec. 63.9565.
    (3) Measure and record the weight of HAP solvent loaded into the 
solvent mixer for each mix batch.
    (4) Measure and record the weight of HAP solvent recovered for each 
mix batch.
    (5) If you use a solvent recovery system, you must determine the 
percent of HAP solvent discharged to the atmosphere for each mix batch 
according to Equation 1 of this section as follows:

(Eq. 1)
[GRAPHIC] [TIFF OMITTED] TR18OC02.002

Where:

Pb = Percent of HAP solvent discharged to the atmosphere for 
each mix batch, percent;
Srec = Weight of HAP solvent recovered for each mix batch, 
lb;
Smix = Weight of HAP solvent loaded into the solvent mixer 
for each mix batch, lb.

    (6) If you use solvent substitution for a mix batch, you must record 
the use of a non-HAP material as a substitute for a HAP solvent for that 
mix batch and assign a value of 0 percent to the percent of HAP solvent 
discharged to the atmosphere for that mix batch (Pb).
    (7) Determine the 7-day block average percent of HAP solvent 
discharged to the atmosphere according to Equation 2 of this section as 
follows:
[GRAPHIC] [TIFF OMITTED] TR18OC02.003

Where:

%P7 = 7-day block average percent of HAP solvent discharged 
to the atmosphere, percent;
i = mix batch;
n = number of mix batches in 7-day block average.

    (8) Have valid data for at least 90 percent of the mix batches over 
the 7-day averaging period.
    (b) If you use a control technique other than a solvent recovery 
system and/or solvent substitution, you may apply to EPA for approval to 
use an alternative method of demonstrating compliance with the emission 
limitations for solvent mixers in Sec. 63.9500(a) and (b), as provided 
in Sec. 63.9570.



Sec. 63.9525  What are the installation, operation, and maintenance 
requirements for my weight measurement device?

    (a) If you use a solvent recovery system, you must install, operate, 
and maintain a weight measurement device to measure the weight of HAP 
solvent loaded into the solvent mixer and the weight of HAP solvent 
recovered for each mix batch.
    (b) For each weight measurement device required by this section, you 
must develop and submit for approval a site-specific monitoring plan 
that addresses the requirements of paragraphs (b)(1) through (6) of this 
section:
    (1) Procedures for installing the weight measurement device;
    (2) The minimum accuracy of the weight measurement device in pounds 
and as a percent of the average weight of solvent to be loaded into the 
solvent mixer;
    (3) Site-specific procedures for how the measurements will be made;
    (4) How the measurement data will be recorded, reduced, and stored;

[[Page 56]]

    (5) Procedures and acceptance criteria for calibration of the weight 
measurement device; and
    (6) How the measurement device will be maintained, including a 
routine maintenance schedule and spare parts inventory list.
    (c) The site-specific monitoring plan required in paragraph (b) of 
this section must include, at a minimum, the requirements of paragraphs 
(c)(1) through (3) of this section:
    (1) The weight measurement device must have a minimum accuracy of 
0.05 kilograms (0.1 pounds) 
or 1 percent of the average weight of solvent to 
be loaded into the solvent mixer, whichever is greater.
    (2) An initial multi-point calibration of the weight measurement 
device must be made using 5 points spanning the expected range of weight 
measurements before the weight measurement device can be used. The 
manufacturer's calibration results can be used to meet this requirement.
    (3) Once per day, an accuracy audit must be made using a single 
Class F calibration weight that corresponds to 20 to 80 percent of the 
average weight of solvent to be loaded into the solvent mixer. If the 
weight measurement device cannot reproduce the value of the calibration 
weight within 0.05 kilograms (0.1 pounds) or 
1 percent of the average weight of solvent to be 
loaded into the solvent mixer, whichever is greater, the scale must be 
recalibrated before being used again. The recalibration must be 
performed with at least five Class F calibration weights spanning the 
expected range of weight measurements.
    (d) You must operate and maintain the weight measurement device 
according to the site-specific monitoring plan.
    (e) You must maintain records of all maintenance activities, 
calibrations, and calibration audits.

                   Continuous Compliance Requirements



Sec. 63.9530  How do I demonstrate continuous compliance with the 
emission limitation that applies to me?

    (a) If you use a solvent recovery system and/or solvent 
substitution, you must demonstrate continuous compliance with the 
emission limitations for solvent mixers in Sec. 63.9500(a) and (b) 
according to the provisions in paragraphs (a)(1) through (3) of this 
section.
    (1) Except for during malfunctions of your weight measurement device 
and associated repairs, you must collect and record the information 
required in Sec. 63.9520(a)(1) through (8) at all times that the 
affected source is operating and record all information needed to 
document conformance with these requirements.
    (2) For new, reconstructed, or existing large solvent mixers, 
maintain the 7-day block average percent of HAP solvent discharged to 
the atmosphere at or below 30 percent of that which would otherwise be 
emitted in the absence of solvent recovery and/or solvent substitution.
    (3) For new, reconstructed, or existing small solvent mixers, 
maintain the 7-day block average percent of HAP solvent discharged to 
the atmosphere at or below 15 percent of that which would otherwise be 
emitted in the absence of solvent recovery and/or solvent substitution.
    (b) If you use a control technique other than a solvent recovery 
system and/or solvent substitution, you must demonstrate continuous 
compliance with the emission limitations for solvent mixers in Sec. 
63.9500(a) and (b) according to the provisions in Sec. 63.9570.
    (c) You must report each instance in which you did not meet the 
emission limitations for solvent mixers in Sec. 63.9500(a) and (b). 
This includes periods of startup, shutdown, or malfunction. These 
instances are deviations from the emission limitations in this subpart. 
These deviations must be reported according to the requirements in Sec. 
63.9540.
    (d) During periods of startup, shutdown, or malfunction, you must 
operate in accordance with your startup, shutdown, and malfunction plan.
    (e) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations 
that occur during a period of startup, shutdown, or malfunction are not 
violations if you demonstrate to the Administrator's satisfaction that 
you were operating in accordance with the startup, shutdown, and 
malfunction plan. The Administrator will determine whether deviations 
that occur during a period of

[[Page 57]]

startup, shutdown, or malfunction are violations, according to the 
provisions in Sec. 63.6(e).

                   Notifications, Reports, and Records



Sec. 63.9535  What notifications must I submit and when?

    (a) You must submit all of the notifications in Sec. Sec. 
63.8(f)(4) and 63.9(b), (c), (d), and (h) that apply to you by the 
specified dates.
    (b) If you use a control technique other than a solvent recovery 
system and/or solvent substitution, you must comply with the provisions 
in Sec. 63.9570.
    (c) As specified in Sec. 63.9(b)(2), if you start up your affected 
source before October 18, 2002, you must submit your initial 
notification no later than 120 calendar days after October 18, 2002.
    (d) As specified in Sec. 63.9(b)(3), if you start up your new 
affected source on or after October 18, 2002, you must submit your 
initial notification no later than 120 calendar days after you become 
subject to this subpart.
    (e) You must submit a notification of compliance status according to 
Sec. 63.9(h)(2)(ii). You must submit the notification of compliance 
status before the close of business on the 30th calendar day following 
the completion of the initial compliance demonstration.



Sec. 63.9540  What reports must I submit and when?

    (a) Unless the Administrator has approved a different schedule, you 
must submit each semiannual compliance report according to the 
requirements in paragraphs (a)(1) through (5) of this section.
    (1) The first compliance report must cover the period beginning on 
the compliance date that is specified for your affected source in Sec. 
63.9495 and ending on June 30 or December 31, whichever date comes first 
after the compliance date that is specified for your source in Sec. 
63.9495.
    (2) The first compliance report must be postmarked or delivered no 
later than July 31 or January 31, whichever date comes first after your 
first compliance report is due.
    (3) Each subsequent compliance report must cover the semiannual 
reporting period from January 1 through June 30 or the semiannual 
reporting period from July 1 through December 31.
    (4) Each subsequent compliance report must be postmarked or 
delivered no later than July 31 or January 31, whichever date comes 
first after the end of the semiannual reporting period.
    (5) For each affected source that is subject to permitting 
regulations pursuant to 40 CFR part 70 or 71 of this chapter, and if the 
permitting authority has established dates for submitting semiannual 
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A) of this chapter, you may submit the first and 
subsequent compliance reports according to the dates the permitting 
authority has established instead of according to the dates in 
paragraphs (a)(1) through (4) of this section.
    (b) Each compliance report must include the information in 
paragraphs (b)(1) through (3) of this section, and if applicable, 
paragraphs (b)(4) through (6) of this section.
    (1) Company name and address.
    (2) Statement by a responsible official, with the official's name, 
title, and signature, certifying that, based on information and belief 
formed after reasonable inquiry, the statements and information in the 
report are true, accurate, and complete.
    (3) Date of report and beginning and ending dates of the reporting 
period.
    (4) If you had a startup, shutdown, or malfunction during the 
reporting period and you took actions consistent with your startup, 
shutdown, and malfunction plan, the compliance report must include the 
information in Sec. 63.10(d)(5)(i).
    (5) If there were no deviations from the emission limitations for 
solvent mixers in Sec. 63.9500(a) and (b), a statement that there were 
no deviations from the emission limitations during the reporting period.
    (6) If there were no periods during which a monitoring system was 
out-of-control as specified in Sec. 63.8(c)(7), a statement that there 
were no periods during which a monitoring system was out-of-control 
during the reporting period.

[[Page 58]]

    (c) For each deviation from an emission limitation occurring at an 
affected source, you must include the information in paragraphs (b)(1) 
through (4) and (c)(1) and (2) of this section. This includes periods of 
startup, shutdown, or malfunction.
    (1) The total operating time of each affected source during the 
reporting period.
    (2) Information on the number, duration, and cause of deviations 
(including unknown cause, if applicable), as applicable, and the 
corrective action taken.
    (d) If you had a startup, shutdown, or malfunction during the 
semiannual reporting period that was not consistent with your startup, 
shutdown, and malfunction plan, you must submit an immediate startup, 
shutdown, and malfunction report according to the requirements in Sec. 
63.10(d)(5)(ii).
    (e) If you have obtained a title V operating permit for an affected 
source pursuant to 40 CFR part 70 or 71 of this chapter, you must report 
all deviations as defined in this subpart in the semiannual monitoring 
report required by 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A) of this chapter. If you submit a compliance report 
for an affected source along with, or as part of, the semiannual 
monitoring report required by 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A) of this chapter, and the compliance report includes 
all the required information concerning deviations from any emission 
limitation in this subpart, then submission of the compliance report 
satisfies any obligation to report the same deviations in the semiannual 
monitoring report. However, submission of a compliance report does not 
otherwise affect any obligation you may have to report deviations from 
permit requirements to your permitting authority.



Sec. 63.9545  What records must I keep?

    (a) You must keep the records in paragraphs (a)(1) and (2) of this 
section that apply to you.
    (1) A copy of each notification and report that you submitted to 
comply with this subpart, including all documentation supporting any 
initial notification or notification of compliance status that you 
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
    (2) The records in Sec. 63.6(e)(3)(iii) through (v) related to 
startup, shutdown, or malfunction.
    (b) You must keep the records required in Sec. 63.9525 to show 
proper operation and maintenance of the weight measurement device.
    (c) You must keep the records required in Sec. 63.9530 to show 
continuous compliance with the emission limitations for solvent mixers 
in Sec. 63.9500(a) and (b).



Sec. 63.9550  In what form and how long must I keep my records?

    (a) You must keep your records in a form suitable and readily 
available for expeditious review, according to Sec. 63.10(b)(1).
    (b) As specified in Sec. 63.10(b)(1), you must keep each record for 
5 years following the date of each occurrence, measurement, maintenance, 
corrective action, report, or record.
    (c) You must keep each record on site for at least 2 years after the 
date of each occurrence, measurement, maintenance, corrective action, 
report, or record, according to Sec. 63.10(b)(1). You can keep the 
records offsite for the remaining 3 years.

                   Other Requirements and Information



Sec. 63.9555  What parts of the General Provisions apply to me?

    Table 1 to this subpart shows which parts of the General Provisions 
in Sec. Sec. 63.1 through 63.15 apply to you.



Sec. 63.9560  Who implements and enforces this subpart?

    (a) This subpart can be implemented and enforced by the U.S. EPA, or 
a delegated authority such as your State, local, or tribal agency. If 
the U.S. EPA Administrator has delegated authority to your State, local, 
or tribal agency, then that agency, in addition to the U.S. EPA, has the 
authority to implement and enforce this subpart. You should contact your 
U.S. EPA Regional Office to find out if this subpart is delegated to 
your State, local, or tribal agency.
    (b) In delegating implementation and enforcement authority of this 
subpart to a State, local, or tribal agency under 40 CFR part 63, 
subpart E, the

[[Page 59]]

authorities contained in paragraphs (c)(1) through (4) of this section 
are retained by the Administrator of the U.S. EPA and are not 
transferred to the State, local, or tribal agency.
    (c) The authorities that cannot be delegated to State, local or 
tribal agencies are as follows:
    (1) Approval of alternatives to the emission limitations in Sec. 
63.9500(a) and (b) under Sec. 63.6(g).
    (2) Approval of major alternatives to test methods under Sec. 
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
    (3) Approval of major alternatives to monitoring under Sec. 63.8(f) 
and as defined in Sec. 63.90.
    (4) Approval of major alternatives to recordkeeping and reporting 
under Sec. 63.10(f) and as defined in Sec. 63.90.



Sec. 63.9565  What definitions apply to this subpart?

    Terms used in this subpart are defined in the Clean Air Act, in 
Sec. 63.2, and in this section as follows:
    Batch ID means a unique identifier used to differentiate each 
individual mix batch.
    Deviation means any instance in which an affected source subject to 
this subpart, or an owner or operator of such a source:
    (1) Fails to meet any requirement or obligation established by this 
subpart, including, but not limited to, any emission limitation 
(including any operating limit);
    (2) Fails to meet any term or condition that is adopted to implement 
an applicable requirement in this subpart and that is included in the 
operating permit for any affected source required to obtain such a 
permit; or
    (3) Fails to meet any emission limitation (including any operating 
limit) in this subpart during startup, shutdown, or malfunction, 
regardless of whether or not such failure is permitted by this subpart.
    Friction ingredients means any of the components used in the 
manufacture of friction materials, excluding the HAP solvent. Friction 
ingredients include, but are not limited to, reinforcement materials, 
property modifiers, resins, and other additives.
    Friction materials manufacturing facility means a facility that 
manufactures friction materials using a solvent-based process. Friction 
materials are used in the manufacture of products used to accelerate or 
decelerate objects. Products that use friction materials include, but 
are not limited to, disc brake pucks, disc brake pads, brake linings, 
brake shoes, brake segments, brake blocks, brake discs, clutch facings, 
and clutches.
    HAP solvent means a solvent that contains 10 percent or more of any 
one HAP, as listed in section 112(b) of the Clean Air Act, or any 
combination of HAP that is added to a solvent mixer. Examples include 
hexane, toluene, and trichloroethylene.
    Initial startup means the first time that equipment is put into 
operation. Initial startup does not include operation solely for testing 
equipment. Initial startup does not include subsequent startups (as 
defined in this section) following malfunction or shutdowns or following 
changes in product or between batch operations.
    Large solvent mixer means a solvent mixer with a design capacity 
greater than or equal to 2,000 pounds, including friction ingredients 
and HAP solvent.
    Mix batch means each batch of friction materials manufactured in a 
solvent mixer.
    Responsible official means responsible official as defined in Sec. 
63.2.
    7-day block average means an averaging technique for a weekly 
compliance determination where the calculated values for percent HAP 
solvent discharged to the atmosphere are averaged together for all mix 
batches (for which there are valid data) in a 7-day block period 
according to the equation provided in Sec. 63.9520(a)(6).
    Small solvent mixer means a solvent mixer with a design capacity 
less than 2,000 pounds, including friction ingredients and HAP solvent.
    Solvent mixer means a mixer used in the friction materials 
manufacturing process in which HAP solvent is used as one of the 
ingredients in at least one batch during a semiannual reporting period. 
Trace amounts of HAP solvents in resins or other friction ingredients do 
not qualify mixers as solvent mixers.
    Solvent recovery system means equipment used for the purpose of 
recovering

[[Page 60]]

the HAP solvent from the exhaust stream. An example of a solvent 
recovery system is a condenser.
    Solvent substitution means substitution of a non-HAP material for a 
HAP solvent.
    Startup means bringing equipment online and starting the production 
process.
    Startup, shutdown, and malfunction plan means a plan developed 
according to the provisions of Sec. 63.6(e)(3).



Sec. 63.9570  How do I apply for alternative compliance requirements?

    (a) If you use a control technique other than a solvent recovery 
system and/or solvent substitution, you may request approval to use an 
alternative method of demonstrating compliance with the emission 
limitations in Sec. 63.9500(a) and (b) according to the procedures in 
this section.
    (b) You can request approval to use an alternative method of 
demonstrating compliance in the initial notification for existing 
sources, the notification of construction or reconstruction for new 
sources, or at any time.
    (c) You must submit a description of the proposed testing, 
monitoring, recordkeeping, and reporting that will be used and the 
proposed basis for demonstrating compliance.
    (1) If you have not previously performed testing, you must submit a 
proposed test plan. If you are seeking permission to use an alternative 
method of compliance based on previously performed testing, you must 
submit the results of testing, a description of the procedures followed 
in testing, and a description of pertinent conditions during testing.
    (2) You must submit a monitoring plan that includes a description of 
the control technique, test results verifying the performance of the 
control technique, the appropriate operating parameters that will be 
monitored, and the frequency of measuring and recording to establish 
continuous compliance with the emission limitations in Sec. 63.9500(a) 
and (b). You must also include the proposed performance specifications 
and quality assurance procedures for the monitors. The monitoring plan 
is subject to the Administrator's approval. You must install, calibrate, 
operate, and maintain the monitors in accordance with the monitoring 
plan approved by the Administrator.
    (d) Use of the alternative method of demonstrating compliance must 
not begin until approval is granted by the Administrator.



Sec. Sec. 63.9571-63.9579  [Reserved]

Table 1 to Subpart QQQQQ of Part 63--Applicability of General Provisions 
                            to Subpart QQQQQ

    As required in Sec. 63.9505, you must comply with each applicable 
General Provisions requirement according to the following table:

----------------------------------------------------------------------------------------------------------------
                                                                  Applies to subpart
             Citation                        Subject                    QQQQQ?                 Explanation
----------------------------------------------------------------------------------------------------------------
Sec. 63.1.......................  Applicability...........  Yes......................
Sec. 63.2.......................  Definitions.............  Yes......................
Sec. 63.3.......................  Units and Abbreviations.  Yes......................
Sec. 63.4.......................  Prohibited Activities...  Yes......................
Sec. 63.5.......................  Construction/             Yes......................
                                     Reconstruction.
Sec. 63.6(a)-(c), (e)-(f), (i)-   Compliance with           Yes......................
 (j).                                Standards and
                                     Maintenance
                                     Requirements.
Sec. 63.6(d)....................  [Reserved]..............
Sec. 63.6(g)....................  Use of an Alternative     No.......................  Subpart QQQQQ contains
                                     Nonopacity Emission                                  no work practice
                                     Standard.                                            standards.
Sec. 63.6(h)....................  Compliance with Opacity   No.......................  Subpart QQQQQ contains
                                     and Visible Emission                                 no opacity or VE
                                     Standards.                                           limits.
Sec. 63.7(a)(1)-(2).............  Applicability and         No.......................  Subpart QQQQQ includes
                                     Performance Test Dates.                              dates for initial
                                                                                          compliance
                                                                                          demonstrations.
Sec. 63.7(a)(3), (b)-(h)........  Performance Testing       No.......................  Subpart QQQQQ does not
                                     Requirements.                                        require performance
                                                                                          tests.
Sec. 63.8(a)(1)-(2), (b), (c)(1)- Monitoring Requirements.  Yes......................
 (3), (f)(1)-(5).
Sec. 63.8(a)(3).................  [Reserved]..............

[[Page 61]]

 
Sec. 63.8(a)(4).................  Additional Monitoring     No.......................  Subpart QQQQQ does not
                                     Requirements for                                     require flares.
                                     Control Devices in Sec.
                                       63.11.
Sec. 63.8(c)(4).................  Continuous Monitoring     No.......................  Subpart QQQQQ does not
                                     System (CMS)                                         require CMS.
                                     Requirements.
Sec. 63.8(c)(5).................  Continuous Opacity        No.......................  Subpart QQQQQ does not
                                     Monitoring System                                    require COMS.
                                     (COMS) Minimum
                                     Procedures.
Sec. 63.8(c)(6).................  Zero and High Level       No.......................  Subpart QQQQQ specifies
                                     Calibration Check                                    calibration
                                     Requirements.                                        requirements.
Sec. 63.8(c)(7)-(8).............  Out-of-Control Periods..  No.......................  Subpart QQQQQ specifies
                                                                                          out-of-control periods
                                                                                          and reporting
                                                                                          requirements.
Sec. 63.8(d)....................  CMS Quality Control.....  No.......................  Subpart QQQQQ requires
                                                                                          a monitoring plan that
                                                                                          specifies CMS quality
                                                                                          control procedures.
Sec. 63.8(e)....................  CMS Performance           No.......................  Subpart QQQQQ does not
                                     Evaluation.                                          require CMS
                                                                                          performance
                                                                                          evaluations.
Sec. 63.8(f)(6).................  Relative Accuracy Test    No.......................  Subpart QQQQQ does not
                                     Audit (RATA)                                         require continuous
                                     Alternative.                                         emissions monitoring
                                                                                          systems (CEMS).
Sec. 63.8(g)(1)-(5).............  Data Reduction..........  No.......................  Subpart QQQQQ specifies
                                                                                          data reduction
                                                                                          requirements.
Sec. 63.9(a)-(d), (h)-(j).......  Notification              Yes......................  Except that subpart
                                     Requirements.                                        QQQQQ does not require
                                                                                          performance tests or
                                                                                          CMS performance
                                                                                          evaluations.
Sec. 63.9(e)....................  Notification of           No.......................  Subpart QQQQQ does not
                                     Performance Test.                                    require performance
                                                                                          tests.
Sec. 63.9(f)....................  Notification of VE/       No.......................  Subpart QQQQQ contains
                                     Opacity Test.                                        no opacity or VE
                                                                                          limits.
Sec. 63.9(g)....................  Additional Notifications  No.......................  Subpart QQQQQ does not
                                     When Using CMS.                                      require CMS
                                                                                          performance
                                                                                          evaluations.
Sec. 63.10(a), (b), (d)(1),       Recordkeeping and         Yes......................
 (d)(4)-(5), (e)(3), (f).            Reporting Requirements.
Sec. 63.10(c)(1)-(6), (9)-(15)..  Additional Records for    No.......................  Subpart QQQQQ specifies
                                     CMS.                                                 record requirements.
Sec. 63.10(c)(7)-(8)............  Records of Excess         No.......................  Subpart QQQQQ specifies
                                     Emissions and Parameter                              record requirements.
                                     Monitoring Exceedances
                                     for CMS.
Sec. 63.10(d)(2)................  Reporting Results of      No.......................  Subpart QQQQQ does not
                                     Performance Tests.                                   require performance
                                                                                          tests.
Sec. 63.10(d)(3)................  Reporting Opacity or VE   No.......................  Subpart QQQQQ contains
                                     Observations.                                        no opacity or VE
                                                                                          limits.
Sec. 63.10(e)(1)-(2)............  Additional CMS Reports..  No.......................  Subpart QQQQQ does not
                                                                                          require CMS.
Sec. 63.10(e)(4)................  Reporting COMS Data.....  No.......................  Subpart QQQQQ does not
                                                                                          require COMS.
Sec. 63.11......................  Control Device            No.......................  Subpart QQQQQ does not
                                     Requirements.                                        require flares.
Sec. Sec. 63.12-63.15..........  Delegation, Addresses,    Yes......................
                                     Incorporation by
                                     Reference Availability
                                     of Information.
----------------------------------------------------------------------------------------------------------------

Subpart RRRRR_National Emission Standards for Hazardous Air Pollutants: 
                      Taconite Iron Ore Processing

    Source: 68 FR 61888, Oct. 30, 2003, unless otherwise noted.

                        What This Subpart Covers



Sec. 63.9580  What is the purpose of this subpart?

    This subpart establishes national emission standards for hazardous 
air pollutants (NESHAP) for taconite iron ore processing. This subpart 
also establishes requirements to demonstrate initial and continuous 
compliance with all applicable emission limitations (emission limits and 
operating limits), work practice standards, and operation and 
maintenance requirements in this subpart.



Sec. 63.9581  Am I subject to this subpart?

    You are subject to this subpart if you own or operate a taconite 
iron ore processing plant that is (or is part of)

[[Page 62]]

a major source of hazardous air pollutant (HAP) emissions on the first 
compliance date that applies to you. Your taconite iron ore processing 
plant is a major source of HAP if it emits or has the potential to emit 
any single HAP at a rate of 10 tons or more per year or any combination 
of HAP at a rate of 25 tons or more per year.



Sec. 63.9582  What parts of my plant does this subpart cover?

    (a) This subpart applies to each new and existing affected source at 
your taconite iron ore processing plant.
    (b) The affected sources are each new or existing ore crushing and 
handling operation, ore dryer, indurating furnace, and finished pellet 
handling operation at your taconite iron ore processing plant, as 
defined in Sec. 63.9652.
    (c) This subpart covers emissions from ore crushing and handling 
emission units, ore dryer stacks, indurating furnace stacks, finished 
pellet handling emission units, and fugitive dust emissions.
    (d) An ore crushing and handling operation, ore dryer, indurating 
furnace, or finished pellet handling operation at your taconite iron ore 
processing plant is existing if you commenced construction or 
reconstruction of the affected source before December 18, 2002.
    (e) An ore crushing and handling operation, ore dryer, indurating 
furnace, or finished pellet handling operation at your taconite iron ore 
processing plant is new if you commence construction or reconstruction 
of the affected source on or after December 18, 2002. An affected source 
is reconstructed if it meets the definition of reconstruction in Sec. 
63.2.



Sec. 63.9583  When do I have to comply with this subpart?

    (a) If you have an existing affected source, you must comply with 
each emission limitation, work practice standard, and operation and 
maintenance requirement in this subpart that applies to you no later 
than October 30, 2006.
    (b) If you have a new affected source and its initial startup date 
is on or before October 30, 2003, you must comply with each emission 
limitation, work practice standard, and operation and maintenance 
requirement in this subpart that applies to you by October 30, 2003.
    (c) If you have a new affected source and its initial startup date 
is after October 30, 2003, you must comply with each emission 
limitation, work practice standard, and operation and maintenance 
requirement in this subpart that applies to you upon initial startup.
    (d) If your taconite iron ore processing plant is an area source 
that becomes a major source of HAP, the compliance dates in paragraphs 
(d)(1) and (2) of this section apply to you.
    (1) Any portion of the taconite iron ore processing plant that is a 
new affected source or a new reconstructed source must be in compliance 
with this subpart upon startup.
    (2) All other parts of the taconite iron ore processing plant must 
be in compliance with this subpart no later than 3 years after the plant 
becomes a major source.
    (e) You must meet the notification and schedule requirements in 
Sec. 63.9640. Several of these notifications must be submitted before 
the compliance date for your affected source.

            Emission Limitations and Work Practice Standards



Sec. 63.9590  What emission limitations must I meet?

    (a) You must meet each emission limit in Table 1 to this subpart 
that applies to you.
    (b) You must meet each operating limit for control devices in 
paragraphs (b)(1) through (5) of this section that applies to you.
    (1) Except as provided in paragraph (b)(2) of this section, for each 
wet scrubber applied to meet any particulate matter emission limit in 
Table 1 to this subpart, you must maintain the daily average pressure 
drop and daily average scrubber water flow rate at or above the minimum 
levels established during the initial performance test.
    (2) For each dynamic wet scrubber applied to meet any particulate 
matter emission limit in Table 1 to this subpart, you must maintain the 
daily average scrubber water flow rate and either the daily average fan 
amperage (a

[[Page 63]]

surrogate for fan speed as revolutions per minute) or the daily average 
pressure drop at or above the minimum levels established during the 
initial performance test.
    (3) For each dry electrostatic precipitator applied to meet any 
particulate matter emission limit in Table 1 to this subpart, you must 
meet the operating limits in paragraph (b)(3)(i) or (ii) of this 
section.
    (i) Maintain the 6-minute average opacity of emissions exiting the 
control device stack at or below the level established during the 
initial performance test.
    (ii) Maintain the daily average secondary voltage and daily average 
secondary current for each field at or above the minimum levels 
established during the initial performance test.
    (4) For each wet electrostatic precipitator applied to meet any 
particulate matter emission limit in Table 1 to this subpart, you must 
meet the operating limits in paragraphs (b)(4)(i) through (iii) of this 
section.
    (i) Maintain the daily average secondary voltage for each field at 
or above the minimum levels established during the initial performance 
test.
    (ii) Maintain the daily average stack outlet temperature at or below 
the maximum levels established during the initial performance test.
    (iii) Maintain the daily average water flow rate at or above the 
minimum levels established during the initial performance test.
    (5) If you use any air pollution control device other than a 
baghouse, wet scrubber, dynamic scrubber, dry electrostatic 
precipitator, or wet electrostatic precipitator, you must submit a site-
specific monitoring plan in accordance with Sec. 63.9631(f).
    (c) You may petition the Administrator for approval of alternatives 
to the monitoring requirements in paragraphs (b)(1) through (4) of this 
section as allowed under Sec. 63.8(f) and as defined in Sec. 63.90.



Sec. 63.9591  What work practice standards must I meet?

    (a) You must prepare, and at all times operate according to, a 
fugitive dust emissions control plan that describes in detail the 
measures that will be put in place to control fugitive dust emissions 
from the locations listed in paragraphs (a)(1) through (6) of this 
section.
    (1) Stockpiles (includes, but is not limited to, stockpiles of 
uncrushed ore, crushed ore, or finished pellets);
    (2) Material transfer points;
    (3) Plant roadways;
    (4) Tailings basin;
    (5) Pellet loading areas; and
    (6) Yard areas.
    (b) A copy of your fugitive dust emissions control plan must be 
submitted for approval to the Administrator on or before the applicable 
compliance date for the affected source as specified in Sec. 63.9583. 
The requirement for the plant to operate according to the fugitive dust 
emissions control plan must be incorporated by reference in the 
operating permit for the plant that is issued by the designated 
permitting authority under 40 CFR part 70 or 40 CFR part 71.
    (c) You can use an existing fugitive dust emissions control plan 
provided it meets the requirements in paragraphs (c)(1) through (3) of 
this section.
    (1) The plan satisfies the requirements of paragraph (a) of this 
section.
    (2) The plan describes the current measures to control fugitive dust 
emission sources.
    (3) The plan has been approved as part of a State implementation 
plan or title V permit.
    (d) You must maintain a current copy of the fugitive dust emissions 
control plan onsite, and it must be available for inspection upon 
request. You must keep the plan for the life of the affected source or 
until the affected source is no longer subject to the requirements of 
this subpart.

                 Operation and Maintenance Requirements



Sec. 63.9600  What are my operation and maintenance requirements?

    (a) As required by Sec. 63.6(e)(1)(i), you must always operate and 
maintain your affected source, including air pollution control and 
monitoring equipment, in a manner consistent with good air pollution 
control practices for minimizing emissions at least to the levels 
required by this subpart.

[[Page 64]]

    (b) You must prepare, and at all times operate according to, a 
written operation and maintenance plan for each control device applied 
to meet any particulate matter emission limit in Table 1 to this subpart 
and to meet the requirement of each indurating furnace subject to good 
combustion practices (GCP). Each site-specific operation and maintenance 
plan must be submitted to the Administrator on or before the compliance 
date that is specified in Sec. 63.9583 for your affected source. The 
plan you submit must explain why the chosen practices (i.e., quantified 
objectives) are effective in performing corrective actions or GCP in 
minimizing the formation of formaldehyde (and other products of 
incomplete combustion). The Administrator will review the adequacy of 
the site-specific practices and objectives you will follow and the 
records you will keep to demonstrate compliance with your Plan. If the 
Administrator determines that any portion of your operation and 
maintenance plan is not adequate, we can reject those portions of the 
plan, and request that you provide additional information addressing the 
relevant issues. In the interim of this process, you will continue to 
follow your current site-specific practices and objectives, as 
submitted, until your revisions are accepted as adequate by the 
Administrator. You must maintain a current copy of the operation and 
maintenance plan onsite, and it must be available for inspection upon 
request. You must keep the plan for the life of the affected source or 
until the affected source is no longer subject to the requirements of 
this subpart. Each operation and maintenance plan must address the 
elements in paragraphs (b)(1) through (4) of this section.
    (1) Preventative maintenance for each control device, including a 
preventative maintenance schedule that is consistent with the 
manufacturer's instructions for routine and long-term maintenance.
    (2) Corrective action procedures for bag leak detection systems. In 
the event a bag leak detection system alarm is triggered, you must 
initiate corrective action to determine the cause of the alarm within 1 
hour of the alarm, initiate corrective action to correct the cause of 
the problem within 24 hours of the alarm, and complete the corrective 
action as soon as practicable. Corrective actions may include, but are 
not limited to, the actions listed in paragraphs (b)(2)(i) through (vi) 
of this section.
    (i) Inspecting the baghouse for air leaks, torn or broken bags or 
filter media, or any other condition that may cause an increase in 
emissions.
    (ii) Sealing off defective bags or filter media.
    (iii) Replacing defective bags or filter media or otherwise 
repairing the control device.
    (iv) Sealing off a defective baghouse compartment.
    (v) Cleaning the bag leak detection system probe, or otherwise 
repairing the bag leak detection system.
    (vi) Adjusting the process operation producing the particulate 
emissions.
    (3) Corrective action procedures for continuous parameter monitoring 
systems (CPMS) for all air pollution control devices except for 
baghouses. In the event you exceed an established operating limit for an 
air pollution control device except for a baghouse, you must initiate 
corrective action to determine the cause of the operating limit 
exceedance and complete the corrective action within 10 calendar days. 
The corrective action procedures you take must be consistent with the 
installation, operation, and maintenance procedures listed in your site-
specific CPMS monitoring plan in accordance with Sec. 63.9632(b).
    (4) Good combustion practices for indurating furnaces. You must 
identify and implement a set of site-specific GCP for each type of 
indurating furnace at your plant. These GCP should correspond to your 
standard operating procedures for maintaining the proper and efficient 
combustion within each indurating furnace. Good combustion practices 
include, but are not limited to, the elements listed in paragraphs 
(b)(4)(i) through (v) of this section.
    (i) Proper operating conditions for each indurating furnace (e.g., 
minimum combustion temperature, maximum carbon monoxide concentration in 
the furnace exhaust gases, burner alignment, or proper fuel-air 
distribution/mixing).

[[Page 65]]

    (ii) Routine inspection and preventative maintenance and 
corresponding schedules of each indurating furnace.
    (iii) Performance analyses of each indurating furnace.
    (iv) Keeping applicable operator logs.
    (v) Keeping applicable records to document compliance with each 
element.

                     General Compliance Requirements



Sec. 63.9610  What are my general requirements for complying with this 
subpart?

    (a) You must be in compliance with the requirements in paragraphs 
(a)(1) through (6) in this section at all times, except during periods 
of startup, shutdown, and malfunction. The terms startup, shutdown, and 
malfunction are defined in Sec. 63.2.
    (1) The emission limitations in Sec. 63.9590.
    (2) The work practice standards in Sec. 63.9591.
    (3) The operation and maintenance requirements in Sec. 63.9600.
    (4) The notification requirements in Sec. 63.9640.
    (5) The reporting requirements in Sec. 63.9641.
    (6) The recordkeeping requirements in Sec. 63.9642.
    (b) During the period between the compliance date specified for your 
affected source in Sec. 63.9583 and the date upon which continuous 
monitoring systems have been installed and certified and any applicable 
operating limits have been set, you must maintain a log detailing the 
operation and maintenance of the process and emissions control 
equipment. This includes the daily monitoring and recordkeeping of air 
pollution control device operating parameters as specified in Sec. 
63.9590(b).
    (c) You must develop and implement a written startup, shutdown, and 
malfunction plan according to the provisions in Sec. 63.6(e)(3).

                     Initial Compliance Requirements



Sec. 63.9620  On which units and by what date must I conduct performance 
tests or other initial compliance demonstrations?

    (a) For each ore crushing and handling affected source, you must 
demonstrate initial compliance with the emission limits in Table 1 to 
this subpart by conducting an initial performance test for particulate 
matter as specified in paragraphs (a)(1) and (2) of this section.
    (1) Except as provided in paragraph (e) of this section, an initial 
performance test must be performed on all stacks associated with ore 
crushing and handling.
    (2) Initial performance tests must be completed no later than 180 
calendar days after the compliance date specified in Sec. 63.9583. 
Performance tests conducted between October 30, 2003 and no later than 
180 days after the corresponding compliance date can be used for initial 
compliance demonstration, provided the tests meet the initial 
performance testing requirements of this subpart.
    (b) For each indurating furnace affected source, you must 
demonstrate initial compliance with the emission limits in Table 1 to 
this subpart by conducting an initial performance test for particulate 
matter as specified in paragraphs (b)(1) and (2) of this section.
    (1) An initial performance test must be performed on all stacks 
associated with each indurating furnace.
    (2) Initial performance tests must be completed no later than 180 
calendar days after the compliance date specified in Sec. 63.9583. 
Performance tests conducted between October 30, 2003 and no later than 
180 days after the corresponding compliance date can be used for initial 
compliance demonstration, provided the tests meet the initial 
performance testing requirements of this subpart. For indurating 
furnaces with multiple stacks, the performance tests for all stacks must 
be completed within a reasonable period of time, such that the 
indurating furnace operating characteristics remain representative for 
the duration of the stack tests.
    (c) For each finished pellet handling affected source, you must 
demonstrate initial compliance with the emission limits in Table 1 to 
this subpart by conducting an initial performance test for particulate 
matter as specified in paragraphs (c)(1) and (2) of this section.
    (1) Except as provided in paragraph (e) of this section, an initial 
performance test must be performed on all

[[Page 66]]

stacks associated with finished pellet handling.
    (2) Initial performance tests must be completed no later than 180 
calendar days after the compliance date specified in Sec. 63.9583. 
Performance tests conducted between October 30, 2003 and no later than 
180 days after the corresponding compliance date can be used for initial 
compliance demonstration, provided the tests meet the initial compliance 
testing requirements of this subpart.
    (d) For each ore dryer affected source, you must demonstrate initial 
compliance with the emission limits in Table 1 to this subpart by 
conducting an initial performance test for particulate matter as 
specified in paragraphs (d)(1) and (2) of this section.
    (1) An initial performance test must be performed on all stacks 
associated with each ore dryer.
    (2) Initial performance tests must be completed no later than 180 
calendar days after the compliance date specified in Sec. 63.9583. 
Performance tests conducted between October 30, 2003 and no later than 
180 days after the corresponding compliance date can be used for initial 
compliance demonstration, provided the tests meet the initial compliance 
testing requirements of this subpart. For ore dryers with multiple 
stacks, the performance tests for all stacks must be completed within a 
reasonable period of time, such that the ore dryer operating 
characteristics remain representative for the duration of the stack 
tests.
    (e) For ore crushing and handling affected sources and finished 
pellet handling affected sources, in lieu of conducting initial 
performance tests for particulate matter on all stacks, you may elect to 
group a maximum of six similar emission units together and conduct an 
initial compliance test on one representative emission unit within each 
group of similar emission units. The determination of whether emission 
units are similar must meet the criteria in paragraph (f) of this 
section. If you decide to test representative emission units, you must 
prepare and submit a testing plan as described in paragraph (g) of this 
section.
    (f) If you elect to test representative emission units as provided 
in paragraph (e) of this section, the units that are grouped together as 
similar units must meet the criteria in paragraphs (f)(1) through (3) of 
this section.
    (1) All emission units within a group must be of the same process 
type (e.g., primary crushers, secondary crushers, tertiary crushers, 
fine crushers, ore conveyors, ore bins, ore screens, grate feed, pellet 
loadout, hearth layer, cooling stacks, pellet conveyor, and pellet 
screens). You cannot group emission units from different process types 
together for the purposes of this section.
    (2) All emission units within a group must also have the same type 
of air pollution control device (e.g., wet scrubbers, dynamic wet 
scrubbers, rotoclones, multiclones, wet and dry electrostatic 
precipitators, and baghouses). You cannot group emission units with 
different air pollution control device types together for the purposes 
of this section.
    (3) The site-specific operating limits established for the emission 
unit selected as representative of a group of similar emission units 
will be used as the operating limit for each emission unit within the 
group. The operating limit established for the representative unit must 
be met by each emission unit within the group.
    (g) If you plan to conduct initial performance tests on 
representative emission units within an ore crushing and handling 
affected source or a finished pellet handling affected source, you must 
submit a testing plan for initial performance tests. This testing plan 
must be submitted to the Administrator or delegated authority no later 
than 90 days prior to the first scheduled initial performance test. The 
testing plan must contain the information specified in paragraphs (g)(1) 
through (3) of this section.
    (1) A list of all emission units. This list must clearly identify 
all emission units that have been grouped together as similar emission 
units. Within each group of emission units, you must identify the 
emission unit that will be the representative unit for that group and 
subject to initial performance testing.
    (2) A list of the process type and type of air pollution control 
device on each emission unit.

[[Page 67]]

    (3) A schedule indicating when you will conduct an initial 
performance test for particulate matter for each representative emission 
unit.
    (h) For each work practice standard and operation and maintenance 
requirement that applies to you where initial compliance is not 
demonstrated using a performance test, you must demonstrate initial 
compliance within 30 calendar days after the compliance date that is 
specified for your affected source in Sec. 63.9583.
    (i) If you commenced construction or reconstruction of an affected 
source between December 18, 2002 and October 30, 2003 , you must 
demonstrate initial compliance with either the proposed emission limit 
or the promulgated emission limit no later than 180 calendar days after 
October 30, 2003 or no later than 180 calendar days after startup of the 
source, whichever is later, according to Sec. 63.7(a)(2)(ix).
    (j) If you commenced construction or reconstruction of an affected 
source between December 18, 2002 and October 30, 2003, and you chose to 
comply with the proposed emission limit when demonstrating initial 
compliance, you must conduct a second performance test to demonstrate 
compliance with the promulgated emission limit by 3 years and 180 
calendar days after October 30, 2003, or after startup of the source, 
whichever is later, according to Sec. 63.7(a)(2)(ix).



Sec. 63.9621  What test methods and other procedures must I use to 

demonstrate initial compliance with the emission limits for 
particulate matter?

    (a) You must conduct each performance test that applies to your 
affected source according to the requirements in Sec. 63.7(e)(1) and 
paragraphs (b) and (c) of this section.
    (b) For each ore crushing and handling affected source and each 
finished pellet handling affected source, you must determine compliance 
with the applicable emission limit for particulate matter in Table 1 to 
this subpart by following the test methods and procedures in paragraphs 
(b)(1) through (3) of this section.
    (1) Except as provided in Sec. 63.9620(e), determine the 
concentration of particulate matter in the stack gas for each emission 
unit according to the test methods in appendix A to part 60 of this 
chapter. The applicable test methods are listed in paragraphs (b)(1)(i) 
through (v) of this section.
    (i) Method 1 or 1A to select sampling port locations and the number 
of traverse points. Sampling ports must be located at the outlet of the 
control device and prior to any releases to the atmosphere.
    (ii) Method 2, 2A, 2C, 2D, 2F, or 2G, as applicable, to determine 
the volumetric flow rate of the stack gas.
    (iii) Method 3, 3A, or 3B to determine the dry molecular weight of 
the stack gas.
    (iv) Method 4 to determine the moisture content of the stack gas.
    (v) Method 5, 5D, or 17 to determine the concentration of 
particulate matter.
    (2) Each Method 5, 5D, or 17 performance test must consist of three 
separate runs. Each run must be conducted for a minimum of 2 hours. The 
average particulate matter concentration from the three runs will be 
used to determine compliance, as shown in Equation 1 of this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.000

Where:

Ci = Average particulate matter concentration for emission 
unit, grains per dry standard cubic foot, (gr/dscf);
C1 = Particulate matter concentration for run 1 corresponding 
to emission unit, gr/dscf;
C2 = Particulate matter concentration for run 2 corresponding 
to emission unit, gr/dscf; and
C3 = Particulate matter concentration for run 3 corresponding 
to emission unit, gr/dscf.

    (3) For each ore crushing and handling affected source and each 
finished pellet handling affected source, you must determine the flow-
weighted mean concentration of particulate matter emissions from all 
emission units in each affected source following the procedure in 
paragraph (b)(3)(i) or (ii) of this section.
    (i) If an initial performance test is conducted on all emission 
units within an affected source, calculate the flow-

[[Page 68]]

weighted mean concentration of particulate matter emissions from the 
affected source using Equation 2 of this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.001

Where:

Ca = Flow-weighted mean concentration of particulate matter 
for all emission units within affected source, (gr/dscf);
Ci = Average particulate matter concentration measured during 
the performance test from emission unit ``i'' in affected source, as 
determined using Equation 1 of this section, gr/dscf;
Qi = Average volumetric flow rate of stack gas measured 
during the performance test from emission unit ``i'' in affected source, 
dscf/hr; and
n = Number of emission units in affected source.

    (ii) If you are grouping similar emission units together in 
accordance with Sec. 63.9620(e), you must follow the procedures in 
paragraphs (b)(3)(ii)(A) through (C) of this section.
    (A) Assign the average particulate matter concentration measured 
from the representative unit, as determined from Equation 1 of this 
section, to each emission unit within the corresponding group of similar 
units.
    (B) Establish the maximum operating volumetric flow rate of exhaust 
gas from each emission unit within each group of similar units.
    (C) Using the data from paragraphs (b)(3)(ii)(A) and (B) of this 
section, calculate the flow-weighted mean concentration of particulate 
matter emissions from the affected source using Equation 3 of this 
section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.002

Where:

Ca = Flow-weighted mean concentration of particulate matter 
for all emission units within affected source, gr/dscf;
Ck = Average particulate matter concentration measured during 
the performance test from the representative emission unit in group 
``k'' of affected source ``a,'' as determined using Equation 1 of this 
section, gr/dscf;
Qk = Sum of the maximum operating volumetric flow rates of 
stack gas from all similar emission units within group ``k'' of affected 
source, dscf/hr; and
m = Number of similar emission unit groups in affected source.

    (c) For each ore dryer affected source and each indurating furnace 
affected source, you must determine compliance with the applicable 
emission limit for particulate matter in Table 1 to this subpart by 
following the test methods and procedures in paragraphs (c)(1) through 
(3) of this section.
    (1) Determine the concentration of particulate matter for each stack 
according to the test methods in 40 CFR part 60, appendix A. The 
applicable test methods are listed in paragraphs (c)(1)(i) through (v) 
of this section.
    (i) Method 1 or 1A to select sampling port locations and the number 
of traverse points. Sampling ports must be located at the outlet of the 
control device and prior to any releases to the atmosphere.
    (ii) Method 2, 2A, 2C, 2D, 2F, or 2G, as applicable, to determine 
the volumetric flow rate of the stack gas.
    (iii) Method 3, 3A, or 3B to determine the dry molecular weight of 
the stack gas.
    (iv) Method 4 to determine the moisture content of the stack gas.
    (v) Method 5, 5D, or 17 to determine the concentration of 
particulate matter.
    (2) Each Method 5, 5D, or 17 performance test must consist of three 
separate runs. Each run must be conducted for a minimum of 2 hours. The 
average particulate matter concentration from the three runs will be 
used to determine compliance, as shown in Equation 1 of this section.
    (3) For each ore dryer and each indurating furnace with multiple 
stacks, calculate the flow-weighted mean concentration of particulate 
matter emissions using Equation 4 of this section.

[[Page 69]]

[GRAPHIC] [TIFF OMITTED] TR30OC03.003

Where:

Cb = Flow-weighted mean concentration of particulate matter 
for all stacks associated with affected source, gr/dscf;
Cj = Average particulate matter concentration measured during 
the performance test from stack ``j'' in affected source, as determined 
using Equation 1 of this section, gr/dscf;
Qj = Average volumetric flow rate of stack gas measured 
during the performance test from stack ``j'' in affected source, dscf/
hr;
n = Number of stacks associated with affected source.



Sec. 63.9622  What test methods and other procedures must I use to 
establish and demonstrate initial compliance with the operating limits?

    (a) For wet scrubbers subject to performance testing in Sec. 
63.9620 and operating limits for pressure drop and scrubber water flow 
rate in Sec. 63.9590(b)(1), you must establish site-specific operating 
limits according to the procedures in paragraphs (a)(1) through (3) of 
this section.
    (1) Using the CPMS required in Sec. 63.9631(b), measure and record 
the pressure drop and scrubber water flow rate every 15 minutes during 
each run of the particulate matter performance test.
    (2) Calculate and record the average pressure drop and scrubber 
water flow rate for each individual test run. Your operating limits are 
established as the lowest average pressure drop and the lowest average 
scrubber water flow rate corresponding to any of the three test runs.
    (3) If a rod-deck venturi scrubber is applied to an indurating 
furnace to meet any particulate matter emission limit in Table 1 to this 
subpart, you may establish a lower average pressure drop operating limit 
by using historical average pressure drop data from a certified 
performance test completed on or after December 18, 2002 instead of 
using the average pressure drop value determined during the initial 
performance test, as specified in paragraph (a)(2) of this section. If 
historical average pressure drop data are used to establish an operating 
limit (i.e., using data from a certified performance test conducted 
prior to the promulgation date of the final rule), then the average 
particulate matter concentration corresponding to the historical 
performance test must be at or below the applicable indurating furnace 
emission limit, as listed in Table 1 to this subpart.
    (b) For dynamic wet scrubbers subject to performance testing in 
Sec. 63.9620 and operating limits for scrubber water flow rate and 
either fan amperage or pressure drop in Sec. 63.9590(b)(2), you must 
establish site-specific operating limits according to the procedures in 
paragraphs (b)(1) and (2) of this section.
    (1) Using the CPMS required in Sec. 63.9631(b), measure and record 
the scrubber water flow rate and either the fan amperage or pressure 
drop every 15 minutes during each run of the particulate matter 
performance test.
    (2) Calculate and record the average scrubber water flow rate and 
either the average fan amperage or average pressure drop for each 
individual test run. Your operating limits are established as the lowest 
average scrubber water flow rate and either the lowest average fan 
amperage or pressure drop value corresponding to any of the three test 
runs.
    (c) For a dry electrostatic precipitator subject to performance 
testing in Sec. 63.9620 and operating limits in Sec. 63.9590(b)(3), 
you must establish a site-specific operating limit according to the 
procedures in paragraphs (c)(1) or (2) of this section.
    (1) If the operating limit for your dry electrostatic precipitator 
is a 6-minute average opacity of emissions value, then you must follow 
the requirements in paragraphs (c)(1)(i) through (iii) of this section.
    (i) Using the continuous opacity monitoring system (COMS) required 
in Sec. 63.9631(d)(1), measure and record the opacity of emissions from 
each control device stack during the particulate matter performance 
test.
    (ii) Compute and record the 6-minute opacity averages from 24 or 
more data points equally spaced over each 6-

[[Page 70]]

minute period (e.g., at 15-second intervals) during the test runs.
    (iii) Using the opacity measurements from a performance test that 
meets the emission limit, determine the opacity value corresponding to 
the 99 percent upper confidence level of a normal distribution of the 6-
minute opacity averages.
    (2) If the operating limit for your dry electrostatic precipitator 
is the daily average secondary voltage and daily average secondary 
current for each field, then you must follow the requirements in 
paragraphs (c)(2)(i) and (ii) of this section.
    (i) Using the CPMS required in Sec. 63.9631(d)(2), measure and 
record the secondary voltage and secondary current for each dry 
electrostatic precipitator field every 15 minutes during each run of the 
particulate matter performance test.
    (ii) Calculate and record the average secondary voltage and 
secondary current for each dry electrostatic precipitator field for each 
individual test run. Your operating limits are established as the lowest 
average secondary voltage and secondary current value for each dry 
electrostatic precipitator field corresponding to any of the three test 
runs.
    (d) For a wet electrostatic precipitator subject to performance 
testing in Sec. 63.9620 and operating limit in Sec. 63.9590(b)(4), you 
must establish a site-specific operating limit according to the 
procedures in paragraphs (d)(1) and (2) of this section.
    (1) Using the CPMS required in Sec. 63.9631(e), measure and record 
the parametric values in paragraphs (d)(1)(i) through (iii) of this 
section for each wet electrostatic precipitator field every 15 minutes 
during each run of the particulate matter performance test.
    (i) Secondary voltage;
    (ii) Water flow rate; and
    (iii) Stack outlet temperature.
    (2) For each individual test run, calculate and record the average 
value for each operating parameter in paragraphs (d)(1)(i) through (iii) 
of this section for each wet electrostatic precipitator field. Your 
operating limits are established as the lowest average value for each 
operating parameter corresponding to any of the three test runs.
    (e) If you use an air pollution control device other than a wet 
scrubber, dynamic wet scrubber, dry electrostatic precipitator, wet 
electrostatic precipitator, or baghouse, and it is subject to 
performance testing in Sec. 63.9620, you must submit a site-specific 
monitoring plan in accordance with Sec. 63.9631(f). The site-specific 
monitoring plan must include the site-specific procedures for 
demonstrating initial and continuous compliance with the corresponding 
operating limits.
    (f) You may change the operating limits for any air pollution 
control device as long as you meet the requirements in paragraphs (f)(1) 
through (3) of this section.
    (1) Submit a written notification to the Administrator of your 
request to conduct a new performance test to revise the operating limit.
    (2) Conduct a performance test to demonstrate compliance with the 
applicable emission limitation in Table 1 to this subpart.
    (3) Establish revised operating limits according to the applicable 
procedures in paragraphs (a) through (e) of this section.



Sec. 63.9623  How do I demonstrate initial compliance with the emission 
limitations that apply to me?

    (a) For each affected source subject to an emission limit in Table 1 
to this subpart, you must demonstrate initial compliance by meeting the 
emission limit requirements in paragraphs (a)(1) through (4) of this 
section.
    (1) For ore crushing and handling, the flow-weighted mean 
concentration of particulate matter, determined according to the 
procedures in Sec. Sec. 63.9620(a) and 63.9621(b), must not exceed the 
emission limits in Table 1 to this subpart.
    (2) For indurating furnaces, the flow-weighted mean concentration of 
particulate matter, determined according to the procedures in Sec. Sec. 
63.9620(b) and 63.9621(c), must not exceed the emission limits in Table 
1 to this subpart.
    (3) For finished pellet handling, the flow-weighted mean 
concentration of particulate matter, determined according to the 
procedures in Sec. Sec. 63.9620(c) and

[[Page 71]]

63.9621(b), must not exceed the emission limits in Table 1 to this 
subpart.
    (4) For ore dryers, the flow-weighted mean concentration of 
particulate matter, determined according to the procedures in Sec. Sec. 
63.9620(d) and 63.9621(c), must not exceed the emission limits in Table 
1 to this subpart.
    (b) For each affected source subject to an emission limit in Table 1 
to this subpart, you must demonstrate initial compliance by meeting the 
operating limit requirements in paragraphs (b)(1) through (5) of this 
section.
    (1) For each wet scrubber subject to performance testing in Sec. 
63.9620 and operating limits for pressure drop and scrubber water flow 
rate in Sec. 63.9590(b)(1), you have established appropriate site-
specific operating limits and have a record of the pressure drop and 
scrubber water flow rate measured during the performance test in 
accordance with Sec. 63.9622(a).
    (2) For each dynamic wet scrubber subject to performance testing in 
Sec. 63.9620 and operating limits for scrubber water flow rate and 
either fan amperage or pressure drop in Sec. 63.9590(b)(2), you have 
established appropriate site-specific operating limits and have a record 
of the scrubber water flow rate and either the fan amperage or pressure 
drop value, measured during the performance test in accordance with 
Sec. 63.9622(b).
    (3) For each dry electrostatic precipitator subject to performance 
testing in Sec. 63.9620 and one of the operating limits in Sec. 
63.9590(b)(3), you must meet the requirements in paragraph (b)(3)(i) or 
(ii) of this section.
    (i) If you are subject to the operating limit for opacity in Sec. 
63.9590(b)(3)(i), you have established appropriate site-specific 
operating limits and have a record of the opacity measured during the 
performance test in accordance with Sec. 63.9622(c)(1).
    (ii) If you are subject to the operating limit for secondary voltage 
and secondary current in Sec. 63.9590(b)(3)(ii), you have established 
appropriate site-specific operating limits and have a record of the 
secondary voltage and secondary current measured during the performance 
test in accordance with Sec. 63.9622(c)(2).
    (4) For each wet electrostatic precipitator subject to performance 
testing in Sec. 63.9620 and operating limits for secondary voltage, 
water flow rate, and stack outlet temperature in Sec. 63.9590(b)(4), 
you have established appropriate site-specific operating limits and have 
a record of the secondary voltage, water flow rate, and stack outlet 
temperature measured during the performance test in accordance with 
Sec. 63.9622(d).
    (5) For other air pollution control devices subject to performance 
testing in Sec. 63.9620 and operating limits in accordance with Sec. 
63.9590(b)(5), you have submitted a site-specific monitoring plan in 
accordance with Sec. 63.9631(f) and have a record of the site-specific 
operating limits as measured during the performance test in accordance 
with Sec. 63.9622(e).
    (c) For each emission limitation and operating limit that applies to 
you, you must submit a notification of compliance status according to 
Sec. 63.9640(e).



Sec. 63.9624  How do I demonstrate initial compliance with the work 
practice standards that apply to me?

    You must demonstrate initial compliance with the work practice 
standards by meeting the requirements in paragraphs (a) through (c) of 
this section.
    (a) You must prepare a fugitive dust emissions control plan in 
accordance with the requirements in Sec. 63.9591.
    (b) You must submit to the Administrator the fugitive dust emissions 
control plan in accordance with the requirements in Sec. 63.9591.
    (c) You must implement each control practice according to the 
procedures specified in your fugitive dust emissions control plan.



Sec. 63.9625  How do I demonstrate initial compliance with the operation 
and maintenance requirements that apply to me?

    For each air pollution control device subject to operating limits in 
Sec. 63.9590(b), you have demonstrated initial compliance if you meet 
all of the requirements in paragraphs (a) through (d) of this section.
    (a) You have prepared the operation and maintenance plan for air 
pollution

[[Page 72]]

control devices in accordance with Sec. 63.9600(b).
    (b) You have operated each air pollution control device according to 
the procedures in the operation and maintenance plan.
    (c) You have submitted a notification of compliance status according 
to the requirements in Sec. 63.9640(e).
    (d) You have prepared a site-specific monitoring plan in accordance 
with Sec. 63.9632(b).

                   Continuous Compliance Requirements



Sec. 63.9630  When must I conduct subsequent performance tests?

    (a) You must conduct subsequent performance tests to demonstrate 
continued compliance with the ore crushing and handling emission limits 
in Table 1 to this subpart according to the schedule developed by your 
permitting authority and shown in your title V permit. If a title V 
permit has not been issued, you must submit a testing plan and schedule, 
containing the information specified in paragraph (e) of this section, 
to the permitting authority for approval.
    (b) You must conduct subsequent performance tests on all stacks 
associated with indurating furnaces to demonstrate continued compliance 
with the indurating furnace emission limits in Table 1 to this subpart 
according to the schedule developed by your permitting authority and 
shown in your title V permit, but no less frequent than twice per 5-year 
permit term. If a title V permit has not been issued, you must submit a 
testing plan and schedule, containing the information specified in 
paragraph (e) of this section, to the permitting authority for approval. 
For indurating furnaces with multiple stacks, the performance tests for 
all stacks associated with that indurating furnace must be conducted 
within a reasonable period of time, such that the indurating furnace 
operating characteristics remain representative for the duration of the 
stack tests.
    (c) You must conduct subsequent performance tests to demonstrate 
continued compliance with the finished pellet handling emission limits 
in Table 1 to this subpart according to the schedule developed by your 
permitting authority and shown in your title V permit. If a title V 
permit has not been issued, you must submit a testing plan and schedule, 
containing the information specified in paragraph (e) of this section, 
to the permitting authority for approval.
    (d) You must conduct subsequent performance tests on all stacks 
associated with ore dryers to demonstrate continued compliance with the 
ore dryer emission limits in Table 1 to this subpart according to the 
schedule developed by your permitting authority and shown in your title 
V permit. If a title V permit has not been issued, you must submit a 
testing plan and schedule, containing the information specified in 
paragraph (e) of this section, to the permitting authority for approval. 
For ore dryers with multiple stacks, the performance tests for all 
stacks associated with an ore dryer must be conducted within a 
reasonable period of time, such that the ore dryer operating 
characteristics remain representative for the duration of the stack 
tests.
    (e) If your plant does not have a title V permit, you must submit a 
testing plan for subsequent performance tests as required in paragraphs 
(a) through (d) of this section. This testing plan must be submitted to 
the Administrator on or before the compliance date that is specified in 
Sec. 63.9583. The testing plan must contain the information specified 
in paragraphs (e)(1) and (2) of this section. You must maintain a 
current copy of the testing plan onsite, and it must be available for 
inspection upon request. You must keep the plan for the life of the 
affected source or until the affected source is no longer subject to the 
requirements of this subpart.
    (1) A list of all emission units.
    (2) A schedule indicating when you will conduct subsequent 
performance tests for particulate matter for each of the emission units.



Sec. 63.9631  What are my monitoring requirements?

    (a) For each baghouse applied to meet any particulate matter 
emission limit in Table 1 to this subpart, you must install, operate, 
and maintain a bag leak detection system to monitor

[[Page 73]]

the relative change in particulate matter loadings according to the 
requirements in Sec. 63.9632(a), and conduct inspections at their 
specified frequencies according to the requirements in paragraphs (a)(1) 
through (8) of this section.
    (1) Monitor the pressure drop across each baghouse cell each day to 
ensure pressure drop is within the normal operating range.
    (2) Confirm that dust is being removed from hoppers through weekly 
visual inspections or other means of ensuring the proper functioning of 
removal mechanisms.
    (3) Check the compressed air supply of pulse-jet baghouses each day.
    (4) Monitor cleaning cycles to ensure proper operation using an 
appropriate methodology.
    (5) Check bag cleaning mechanisms for proper functioning through 
monthly visual inspections or equivalent means.
    (6) Make monthly visual checks of bag tension on reverse air and 
shaker-type baghouses to ensure that bags are not kinked (kneed or bent) 
or lying on their sides. You do not have to make this check for shaker-
type baghouses that have self-tensioning (spring-loaded) devices.
    (7) Confirm the physical integrity of the baghouse through quarterly 
visual inspections of the baghouse interior for air leaks.
    (8) Inspect fans for wear, material buildup, and corrosion through 
quarterly visual inspections, vibration detectors, or equivalent means.
    (b) Except as provided in paragraph (c) of this section, for each 
wet scrubber subject to the operating limits for pressure drop and 
scrubber water flow rate in Sec. 63.9590(b)(1), you must install, 
operate, and maintain a CPMS according to the requirements in Sec. 
63.9632(b) through (e) and monitor the daily average pressure drop and 
daily average scrubber water flow rate according to the requirements in 
Sec. 63.9633.
    (c) For each dynamic wet scrubber subject to the scrubber water flow 
rate and either the fan amperage or pressure drop operating limits in 
Sec. 63.9590(b)(2), you must install, operate, and maintain a CPMS 
according to the requirements in Sec. 63.9632(b) through (e) and 
monitor the daily average scrubber water flow rate and either the daily 
average fan amperage or the daily average pressure drop according to the 
requirements in Sec. 63.9633.
    (d) For each dry electrostatic precipitator subject to the operating 
limits in Sec. 63.9590(b)(3), you must follow the monitoring 
requirements in paragraph (d)(1) or (2) of this section.
    (1) If the operating limit you choose to monitor is the 6-minute 
average opacity of emissions in accordance with Sec. 63.9590(b)(3)(i), 
you must install, operate, and maintain a COMS according to the 
requirements in Sec. 63.9632(f) and monitor the 6-minute average 
opacity of emissions exiting each control device stack according to the 
requirements in Sec. 63.9633.
    (2) If the operating limit you choose to monitor is average 
secondary voltage and average secondary current for each dry 
electrostatic precipitator field in accordance with Sec. 
63.9590(b)(3)(ii), you must install, operate, and maintain a CPMS 
according to the requirements in Sec. 63.9632(b) through (e) and 
monitor the daily average secondary voltage and daily average secondary 
current according to the requirements in Sec. 63.9633.
    (e) For each wet electrostatic precipitator subject to the operating 
limits in Sec. 63.9590(b)(4), you must install, operate, and maintain a 
CPMS according to the requirements in Sec. 63.9632(b) through (e) and 
monitor the daily average secondary voltage, daily average stack outlet 
temperature, and daily average water flow rate according to the 
requirements in Sec. 63.9633.
    (f) If you use any air pollution control device other than a 
baghouse, wet scrubber, dry electrostatic precipitator, or wet 
electrostatic precipitator, you must submit a site-specific monitoring 
plan that includes the information in paragraphs (f)(1) through (4) of 
this section. The monitoring plan is subject to approval by the 
Administrator. You must maintain a current copy of the monitoring plan 
onsite, and it must be available for inspection upon request. You must 
keep the plan for the life of the affected source or until the affected 
source is no longer subject to the requirements of this subpart.
    (1) A description of the device.

[[Page 74]]

    (2) Test results collected in accordance with Sec. 63.9621 
verifying the performance of the device for reducing emissions of 
particulate matter to the atmosphere to the levels required by this 
subpart.
    (3) A copy of the operation and maintenance plan required in Sec. 
63.9600(b).
    (4) Appropriate operating parameters that will be monitored to 
maintain continuous compliance with the applicable emission 
limitation(s).



Sec. 63.9632  What are the installation, operation, and maintenance 
requirements for my monitoring equipment?

    (a) For each negative pressure baghouse or positive pressure 
baghouse equipped with a stack, applied to meet any particulate emission 
limit in Table 1 to this subpart, you must install, operate, and 
maintain a bag leak detection system according to the requirements in 
paragraphs (a)(1) through (8) of this section.
    (1) The system must be certified by the manufacturer to be capable 
of detecting emissions of particulate matter at concentrations of 10 
milligrams per actual cubic meter (0.0044 grains per actual cubic foot) 
or less.
    (2) The system must provide output of relative changes in 
particulate matter loadings.
    (3) The system must be equipped with an alarm that will sound when 
an increase in relative particulate loadings is detected over the alarm 
level set point established according to paragraph (a)(4) of this 
section. The alarm must be located such that it can be heard by the 
appropriate plant personnel.
    (4) For each bag leak detection system, you must develop and submit 
to the Administrator for approval, a site-specific monitoring plan that 
addresses the items identified in paragraphs (a)(4)(i) through (v) of 
this section. For each bag leak detection system that operates based on 
the triboelectric effect, the monitoring plan shall be consistent with 
the recommendations contained in the U.S. Environmental Protection 
Agency (U.S. EPA) guidance document, ``Fabric Filter Bag Leak Detection 
Guidance'' (EPA-454/R-98-015). This document is available on the EPA's 
Technology Transfer Network at http://www.epa.gov/ttn/emc/cem/tribo.pdf 
(Adobe Acrobat version) or http://www.epa.gov/ttn/emc/cem/tribo.wpd 
(WordPerfect version). You must operate and maintain the bag leak 
detection system according to the site-specific monitoring plan at all 
times. The plan shall describe all of the items in paragraphs (a)(4)(i) 
through (v) of this section.
    (i) Installation of the bag leak detection system.
    (ii) Initial and periodic adjustment of the bag leak detection 
system including how the alarm set-point will be established.
    (iii) Operation of the bag leak detection system including quality 
assurance procedures.
    (iv) How the bag leak detection system will be maintained including 
a routine maintenance schedule and spare parts inventory list.
    (v) How the bag leak detection system output shall be recorded and 
stored.
    (5) To make the initial adjustment of the system, establish the 
baseline output by adjusting the sensitivity (range) and the averaging 
period of the device. Then, establish the alarm set points and the alarm 
delay time (if applicable).
    (6) Following initial adjustment, do not adjust averaging period, 
alarm set point, or alarm delay time, without approval from the 
Administrator except as provided for in paragraph (a)(6)(i) of this 
section.
    (i) Once per quarter, you may adjust the sensitivity of the bag leak 
detection system to account for seasonal effects, including temperature 
and humidity, according to the procedures identified in the site-
specific monitoring plan required under paragraph (a)(4) of this 
section.
    (ii) [Reserved]
    (7) Where multiple detectors are required, the system's 
instrumentation and alarm may be shared among detectors.
    (8) The bag leak detector sensor must be installed downstream of the 
baghouse and upstream of any wet scrubber.
    (b) For each CPMS required in Sec. 63.9631, you must develop and 
make

[[Page 75]]

available for inspection upon request by the permitting authority a 
site-specific monitoring plan that addresses the requirements in 
paragraphs (b)(1) through (7) of this section.
    (1) Installation of the CPMS sampling probe or other interface at a 
measurement location relative to each affected emission unit such that 
the measurement is representative of control of the exhaust emissions 
(e.g., on or downstream of the last control device).
    (2) Performance and equipment specifications for the sample 
interface, the parametric signal analyzer, and the data collection and 
reduction system.
    (3) Performance evaluation procedures and acceptance criteria (e.g., 
calibrations).
    (4) Ongoing operation and maintenance procedures in accordance with 
the general requirements of Sec. 63.8(c)(1), (3), (4)(ii), (7), and 
(8).
    (5) Ongoing data quality assurance procedures in accordance with the 
general requirements of Sec. 63.8(d).
    (6) Ongoing recordkeeping and reporting procedures in accordance 
with the general requirements of Sec. 63.10(c), (e)(1), and (e)(2)(i).
    (7) Corrective action procedures that you will follow in the event 
an air pollution control device, except for a baghouse, exceeds an 
established operating limit as required in Sec. 63.9600(b)(3).
    (c) Unless otherwise specified, each CPMS must meet the requirements 
in paragraphs (c)(1) and (2) of this section.
    (1) Each CPMS must complete a minimum of one cycle of operation for 
each successive 15-minute period and must have valid data for at least 
95 percent of every daily averaging period.
    (2) Each CPMS must determine and record the daily average of all 
recorded readings.
    (d) You must conduct a performance evaluation of each CPMS in 
accordance with your site-specific monitoring plan.
    (e) You must operate and maintain the CPMS in continuous operation 
according to the site-specific monitoring plan.
    (f) For each dry electrostatic precipitator subject to the opacity 
operating limit in Sec. 63.9590(b)(3)(i), you must install, operate, 
and maintain each COMS according to the requirements in paragraphs 
(f)(1) through (4) of this section.
    (1) You must install each COMS and conduct a performance evaluation 
of each COMS according to Sec. 63.8 and Performance Specification 1 in 
appendix B to 40 CFR part 60.
    (2) You must develop and implement a quality control program for 
operating and maintaining each COMS according to Sec. 63.8. At a 
minimum, the quality control program must include a daily calibration 
drift assessment, quarterly performance audit, and annual zero alignment 
of each COMS.
    (3) You must operate and maintain each COMS according to Sec. 
63.8(e) and your quality control program. You must also identify periods 
the COMS is out of control, including any periods that the COMS fails to 
pass a daily calibration drift assessment, quarterly performance audit, 
or annual zero alignment audit.
    (4) You must determine and record the 6-minute average opacity for 
periods during which the COMS is not out of control.



Sec. 63.9633  How do I monitor and collect data to demonstrate continuous 
compliance?

    (a) Except for monitoring malfunctions, associated repairs, and 
required quality assurance or control activities (including as 
applicable, calibration checks and required zero and span adjustments), 
you must monitor continuously (or collect data at all required 
intervals) at all times an affected source is operating.
    (b) You may not use data recorded during monitoring malfunctions, 
associated repairs, and required quality assurance or control activities 
in data averages and calculations used to report emission or operating 
levels, or to fulfill a minimum data availability requirement. You must 
use all the data collected during all other periods in assessing 
compliance.
    (c) A monitoring malfunction is any sudden, infrequent, not 
reasonably preventable failure of the monitoring system to provide valid 
data. Monitoring failures that are caused in part by poor

[[Page 76]]

maintenance or careless operation are not considered malfunctions.



Sec. 63.9634  How do I demonstrate continuous compliance with the emission 
limitations that apply to me?

    (a) For each affected source subject to an emission limit in Table 1 
to this subpart, you must demonstrate continuous compliance by meeting 
the requirements in paragraphs (b) through (f) of this section.
    (b) For ore crushing and handling affected sources and finished 
pellet handling affected sources, you must demonstrate continuous 
compliance by meeting the requirements in paragraphs (b)(1) through (3) 
of this section.
    (1) The flow-weighted mean concentration of particulate matter for 
all ore crushing and handling emission units and for all finished pellet 
handling emission units must be maintained at or below the emission 
limits in Table 1 to this subpart.
    (2) You must conduct subsequent performance tests for emission units 
in the ore crushing and handling and finished pellet handling affected 
sources following the schedule in your title V permit. If a title V 
permit has not been issued, you must conduct subsequent performance 
tests according to a testing plan approved by the Administrator or 
delegated authority.
    (3) For emission units not selected for initial performance testing 
and defined within a group of similar emission units in accordance with 
Sec. 63.9620(e), you must calculate the daily average value of each 
operating parameter for the similar air pollution control device applied 
to each similar emission unit within a defined group using Equation 1 of 
this section.
[GRAPHIC] [TIFF OMITTED] TR30OC03.004

Where:

Pk = Daily average operating parameter value for all emission 
units within group ``k'';
Pi = Daily average parametric monitoring parameter value 
corresponding to emission unit ``i'' within group ``k''; and
n = Total number of emission units within group, including emission 
units that have been selected for performance tests and those that have 
not been selected for performance tests.

    (c) For ore dryers and indurating furnaces, you must demonstrate 
continuous compliance by meeting the requirements in paragraphs (c)(1) 
and (2) of this section.
    (1) The flow-weighted mean concentration of particulate matter for 
all stacks from the ore dryer or indurating furnace must be maintained 
at or below the emission limits in Table 1 to this subpart.
    (2) For ore dryers, you must conduct subsequent performance tests 
following the schedule in your title V permit. For indurating furnaces, 
you must conduct subsequent performance tests following the schedule in 
your title V permit, but no less frequent than twice per 5-year permit 
term. If a title V permit has not been issued, you must conduct 
subsequent performance tests according to a testing plan approved by the 
Administrator or delegated authority.
    (d) For each baghouse applied to meet any particulate emission limit 
in Table 1 to this subpart, you must demonstrate continuous compliance 
by completing the requirements in paragraphs (d)(1) and (2) of this 
section.
    (1) Maintaining records of the time you initiated corrective action 
in the event of a bag leak detection system alarm, the corrective 
action(s) taken, and the date on which corrective action was completed.
    (2) Inspecting and maintaining each baghouse according to the 
requirements in Sec. 63.9631(a)(1) through (8) and recording all 
information needed to document conformance with these requirements. If 
you increase or decrease the sensitivity of the bag leak detection 
system beyond the limits specified in your site-specific monitoring 
plan, you must include a copy of the required written certification by a 
responsible official in the next semiannual compliance report.
    (e) Except as provided in paragraph (f) of this section, for each 
wet scrubber subject to the operating limits for pressure drop and 
scrubber water flow rate in Sec. 63.9590(b)(1), you must demonstrate 
continuous compliance by completing the requirements of paragraphs 
(e)(1) through (4) of this section.

[[Page 77]]

    (1) Maintaining the daily average pressure drop and daily average 
scrubber water flow rate at or above the minimum levels established 
during the initial or subsequent performance test.
    (2) Operating and maintaining each wet scrubber CPMS according to 
Sec. 63.9632(b) and recording all information needed to document 
conformance with these requirements.
    (3) Collecting and reducing monitoring data for pressure drop and 
scrubber water flow rate according to Sec. 63.9632(c) and recording all 
information needed to document conformance with these requirements.
    (4) If the daily average pressure drop or daily average scrubber 
water flow rate is below the operating limits established for a 
corresponding emission unit or group of similar emission units, you must 
then follow the corrective action procedures in paragraph (j) of this 
section.
    (f) For each dynamic wet scrubber subject to the operating limits 
for scrubber water flow rate and either the fan amperage or pressure 
drop in Sec. 63.9590(b)(2), you must demonstrate continuous compliance 
by completing the requirements of paragraphs (f)(1) through (4) of this 
section.
    (1) Maintaining the daily average scrubber water flow rate and 
either the daily average fan amperage or the daily average pressure drop 
at or above the minimum levels established during the initial or 
subsequent performance test.
    (2) Operating and maintaining each dynamic wet scrubber CPMS 
according to Sec. 63.9632(b) and recording all information needed to 
document conformance with these requirements.
    (3) Collecting and reducing monitoring data for scrubber water flow 
rate and either fan amperage or pressure drop according to Sec. 
63.9632(c) and recording all information needed to document conformance 
with these requirements.
    (4) If the daily average scrubber water flow rate, daily average fan 
amperage, or daily average pressure drop is below the operating limits 
established for a corresponding emission unit or group of similar 
emission units, you must then follow the corrective action procedures in 
paragraph (j) of this section.
    (g) For each dry electrostatic precipitator subject to operating 
limits in Sec. 63.9590(b)(3), you must demonstrate continuous 
compliance by completing the requirements of paragraph (g)(1) or (2) of 
this section.
    (1) If the operating limit for your dry electrostatic precipitator 
is a 6-minute average opacity of emissions value, then you must follow 
the requirements in paragraphs (g)(1)(i) through (iii) of this section.
    (i) Maintaining the 6-minute average opacity of emissions at or 
below the maximum level established during the initial or subsequent 
performance test.
    (ii) Operating and maintaining each COMS and reducing the COMS data 
according to Sec. 63.9632(f).
    (iii) If the 6-minute average opacity of emissions is above the 
operating limits established for a corresponding emission unit, you must 
then follow the corrective action procedures in paragraph (j) of this 
section.
    (2) If the operating limit for your dry electrostatic precipitator 
is the daily average secondary voltage and daily average secondary 
current for each field, then you must follow the requirements in 
paragraphs (g)(2)(i) through (iv) of this section.
    (i) Maintaining the daily average secondary voltage or daily average 
secondary current for each field at or above the minimum levels 
established during the initial or subsequent performance test.
    (ii) Operating and maintaining each dry electrostatic precipitator 
CPMS according to Sec. 63.9632(b) and recording all information needed 
to document conformance with these requirements.
    (iii) Collecting and reducing monitoring data for secondary voltage 
or secondary current for each field according to Sec. 63.9632(c) and 
recording all information needed to document conformance with these 
requirements.
    (iv) If the daily average secondary voltage or daily average 
secondary current for each field is below the operating limits 
established for a corresponding emission unit, you must then follow the 
corrective action procedures in paragraph (j) of this section.

[[Page 78]]

    (h) For each wet electrostatic precipitator subject to the operating 
limits for secondary voltage, stack outlet temperature, and water flow 
rate in Sec. 63.9590(b)(4), you must demonstrate continuous compliance 
by completing the requirements of paragraphs (h)(1) through (4) of this 
section.
    (1) Maintaining the daily average secondary voltage, daily average 
secondary current, and daily average scrubber water flow rate for each 
field at or above the minimum levels established during the initial or 
subsequent performance test. Maintaining the daily average stack outlet 
temperature at or below the maximum levels established during the 
initial or subsequent performance test.
    (2) Operating and maintaining each wet electrostatic precipitator 
CPMS according to Sec. 63.9632(b) and recording all information needed 
to document conformance with these requirements.
    (3) Collecting and reducing monitoring data for secondary voltage, 
stack outlet temperature, and water flow rate according to Sec. 
63.9632(c) and recording all information needed to document conformance 
with these requirements.
    (4) If the daily average secondary voltage, stack outlet 
temperature, or water flow rate does not meet the operating limits 
established for a corresponding emission unit, you must then follow the 
corrective action procedures in paragraph (j) of this section.
    (i) If you use an air pollution control device other than a wet 
scrubber, dynamic wet scrubber, dry electrostatic precipitator, wet 
electrostatic precipitator, or baghouse, you must submit a site-specific 
monitoring plan in accordance with Sec. 63.9631(f). The site-specific 
monitoring plan must include the site-specific procedures for 
demonstrating initial and continuous compliance with the corresponding 
operating limits.
    (j) If the daily average operating parameter value for an emission 
unit or group of similar emission units does not meet the corresponding 
established operating limit, you must then follow the procedures in 
paragraphs (j)(1) through (4) of this section.
    (1) You must initiate and complete initial corrective action within 
10 calendar days and demonstrate that the initial corrective action was 
successful. During any period of corrective action, you must continue to 
monitor and record all required operating parameters for equipment that 
remains in operation. After 10 calendar days, measure and record the 
daily average operating parameter value for the emission unit or group 
of similar emission units on which corrective action was taken. After 
the initial corrective action, if the daily average operating parameter 
value for the emission unit or group of similar emission units meets the 
operating limit established for the corresponding unit or group, then 
the corrective action was successful and the emission unit or group of 
similar emission units is in compliance with the established operating 
limits.
    (2) If the initial corrective action required in paragraph (j)(1) of 
this section was not successful, then you must complete additional 
corrective action within 10 calendar days and demonstrate that the 
subsequent corrective action was successful. During any period of 
corrective action, you must continue to monitor and record all required 
operating parameters for equipment that remains in operation. After the 
second set of 10 calendar days allowed to implement corrective action, 
you must again measure and record the daily average operating parameter 
value for the emission unit or group of similar emission units. If the 
daily average operating parameter value for the emission unit or group 
of similar emission units meets the operating limit established for the 
corresponding unit or group, then the corrective action was successful 
and the emission unit or group of similar emission units is in 
compliance with the established operating limits.
    (3) If the second attempt at corrective action required in paragraph 
(j)(2) of this section was not successful, then you must repeat the 
procedures of paragraph (j)(2) of this section until the corrective 
action is successful. If the third attempt at corrective action is 
unsuccessful, you must conduct another performance test in accordance 
with the procedures in Sec. 63.9622(f) and report to the Administrator 
as a deviation the third unsuccessful attempt at corrective action.

[[Page 79]]

    (4) After the third unsuccessful attempt at corrective action, you 
must submit to the Administrator the written report required in 
paragraph (j)(3) of this section within 5 calendar days after the third 
unsuccessful attempt at corrective action. This report must notify the 
Administrator that a deviation has occurred and document the types of 
corrective measures taken to address the problem that resulted in the 
deviation of established operating parameters and the resulting 
operating limits.



Sec. 63.9635  How do I demonstrate continuous compliance with the work 
practice standards that apply to me?

    (a) You must demonstrate continuous compliance with the work 
practice standard requirements in Sec. 63.9591 by operating in 
accordance with your fugitive dust emissions control plan at all times.
    (b) You must maintain a current copy of the fugitive dust emissions 
control plan required in Sec. 63.9591 onsite and it must be available 
for inspection upon request. You must keep the plan for the life of the 
affected source or until the affected source is no longer subject to the 
requirements of this subpart.



Sec. 63.9636  How do I demonstrate continuous compliance with the 
operation and maintenance requirements that apply to me?

    (a) For each control device subject to an operating limit in Sec. 
63.9590(b), you must demonstrate continuous compliance with the 
operation and maintenance requirements in Sec. 63.9600(b) by completing 
the requirements of paragraphs (a)(1) through (4) of this section.
    (1) Performing preventative maintenance for each control device in 
accordance with Sec. 63.9600(b)(1) and recording all information needed 
to document conformance with these requirements;
    (2) Initiating and completing corrective action for a bag leak 
detection system alarm in accordance with Sec. 63.9600(b)(2) and 
recording all information needed to document conformance with these 
requirements;
    (3) Initiating and completing corrective action for a CPMS when you 
exceed an established operating limit for an air pollution control 
device except for a baghouse in accordance with Sec. 63.9600(b)(3) and 
recording all information needed to document conformance with these 
requirements; and
    (4) Implementing and maintaining site-specific good combustion 
practices for each indurating furnace in accordance with Sec. 
63.9600(b)(4) and recording all information needed to document 
conformance with these requirements.
    (b) You must maintain a current copy of the operation and 
maintenance plan required in Sec. 63.9600(b) onsite, and it must be 
available for inspection upon request. You must keep the plan for the 
life of the affected source or until the affected source is no longer 
subject to the requirements of this subpart.



Sec. 63.9637  What other requirements must I meet to demonstrate continuous 
compliance?

    (a) Deviations. You must report each instance in which you did not 
meet each emission limitation in Table 1 to this subpart that applies to 
you. This includes periods of startup, shutdown, and malfunction in 
accordance with paragraph (b) of this section. You also must report each 
instance in which you did not meet the work practice standards in Sec. 
63.9591 and each instance in which you did not meet each operation and 
maintenance requirement in Sec. 63.9600 that applies to you. These 
instances are deviations from the emission limitations, work practice 
standards, and operation and maintenance requirements in this subpart. 
These deviations must be reported in accordance with the requirements in 
Sec. 63.9641.
    (b) Startups, shutdowns, and malfunctions. During periods of 
startup, shutdown, and malfunction, you must operate in accordance with 
your startup, shutdown, and malfunction plan and the requirements in 
paragraphs (b)(1) and (2) of this section.
    (1) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations 
that occur during a period of startup, shutdown, or malfunction are not 
violations if you demonstrate to the Administrator's satisfaction that 
you were operating in accordance with the startup, shutdown, and 
malfunction plan.

[[Page 80]]

    (2) The Administrator will determine whether deviations that occur 
during a period of startup, shutdown, or malfunction are violations, 
according to the provisions in Sec. 63.6(e).

                   Notifications, Reports, and Records



Sec. 63.9640  What notifications must I submit and when?

    (a) You must submit all of the notifications in Sec. Sec. 63.7(b) 
and (c), 63.8(f)(4), and 63.9(b) through (h) that apply to you by the 
specified dates.
    (b) As specified in Sec. 63.9(b)(2), if you start up your affected 
source before October 30, 2003, you must submit your initial 
notification no later than 120 calendar days after October 30, 2003.
    (c) As specified in Sec. 63.9(b)(3), if you start up your new 
affected source on or after October 30, 2003, you must submit your 
initial notification no later than 120 calendar days after you become 
subject to this subpart.
    (d) If you are required to conduct a performance test, you must 
submit a notification of intent to conduct a performance test at least 
60 calendar days before the performance test is scheduled to begin, as 
required in Sec. 63.7(b)(1).
    (e) If you are required to conduct a performance test or other 
initial compliance demonstration, you must submit a notification of 
compliance status according to Sec. 63.9(h)(2)(ii). The initial 
notification of compliance status must be submitted by the dates 
specified in paragraphs (e)(1) and (2) of this section.
    (1) For each initial compliance demonstration that does not include 
a performance test, you must submit the notification of compliance 
status before the close of business on the 30th calendar day following 
completion of the initial compliance demonstration.
    (2) For each initial compliance demonstration that does include a 
performance test, you must submit the notification of compliance status, 
including the performance test results, before the close of business on 
the 60th calendar day following the completion of the performance test 
according to Sec. 63.10(d)(2).



Sec. 63.9641  What reports must I submit and when?

    (a) Compliance report due dates. Unless the Administrator has 
approved a different schedule, you must submit a semiannual compliance 
report to your permitting authority according to the requirements in 
paragraphs (a)(1) through (5) of this section.
    (1) The first compliance report must cover the period beginning on 
the compliance date that is specified for your affected source in Sec. 
63.9583 and ending on June 30 or December 31, whichever date comes first 
after the compliance date that is specified for your source in Sec. 
63.9583.
    (2) The first compliance report must be postmarked or delivered no 
later than July 31 or January 31, whichever date comes first after your 
first compliance report is due.
    (3) Each subsequent compliance report must cover the semiannual 
reporting period from January 1 through June 30 or the semiannual 
reporting period from July 1 through December 31.
    (4) Each subsequent compliance report must be postmarked or 
delivered no later than July 31 or January 31, whichever date comes 
first after the end of the semiannual reporting period.
    (5) For each affected source that is subject to permitting 
regulations pursuant to 40 CFR part 70 or 40 CFR part 71, and if the 
permitting authority has established dates for submitting semiannual 
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance 
reports according to the dates the permitting authority has established 
instead of according to the dates in paragraphs (a)(1) through (4) of 
this section.
    (b) Compliance report contents. Each compliance report must include 
the information in paragraphs (b)(1) through (3) of this section and, as 
applicable, in paragraphs (b)(4) through (8) of this section.
    (1) Company name and address.
    (2) Statement by a responsible official, with the official's name, 
title, and signature, certifying the truth, accuracy, and completeness 
of the content of the report.

[[Page 81]]

    (3) Date of report and beginning and ending dates of the reporting 
period.
    (4) If you had a startup, shutdown, or malfunction during the 
reporting period and you took actions consistent with your startup, 
shutdown, and malfunction plan, the compliance report must include the 
information in Sec. 63.10(d)(5)(i).
    (5) If there were no deviations from the continuous compliance 
requirements in Sec. Sec. 63.9634 through 63.9636 that apply to you, 
then provide a statement that there were no deviations from the emission 
limitations, work practice standards, or operation and maintenance 
requirements during the reporting period.
    (6) If there were no periods during which a continuous monitoring 
system (including a CPMS or COMS) was out-of-control as specified in 
Sec. 63.8(c)(7), then provide a statement that there were no periods 
during which a continuous monitoring system was out-of-control during 
the reporting period.
    (7) For each deviation from an emission limitation in Table 1 to 
this subpart that occurs at an affected source where you are not using a 
continuous monitoring system (including a CPMS or COMS) to comply with 
an emission limitation in this subpart, the compliance report must 
contain the information in paragraphs (b)(1) through (4) of this section 
and the information in paragraphs (b)(7)(i) and (ii) of this section. 
This includes periods of startup, shutdown, and malfunction.
    (i) The total operating time of each affected source during the 
reporting period.
    (ii) Information on the number, duration, and cause of deviations 
(including unknown cause) as applicable, and the corrective action 
taken.
    (8) For each deviation from an emission limitation occurring at an 
affected source where you are using a continuous monitoring system 
(including a CPMS or COMS) to comply with the emission limitation in 
this subpart, you must include the information in paragraphs (b)(1) 
through (4) of this section and the information in paragraphs (b)(8)(i) 
through (xi) of this section. This includes periods of startup, 
shutdown, and malfunction.
    (i) The date and time that each malfunction started and stopped.
    (ii) The date and time that each continuous monitoring system was 
inoperative, except for zero (low-level) and high-level checks.
    (iii) The date, time, and duration that each continuous monitoring 
system was out-of-control, including the information in Sec. 
63.8(c)(8).
    (iv) The date and time that each deviation started and stopped, and 
whether each deviation occurred during a period of startup, shutdown, or 
malfunction or during another period.
    (v) A summary of the total duration of the deviation during the 
reporting period and the total duration as a percent of the total source 
operating time during that reporting period.
    (vi) A breakdown of the total duration of the deviations during the 
reporting period including those that are due to startup, shutdown, 
control equipment problems, process problems, other known causes, and 
other unknown causes.
    (vii) A summary of the total duration of continuous monitoring 
system downtime during the reporting period and the total duration of 
continuous monitoring system downtime as a percent of the total source 
operating time during the reporting period.
    (viii) A brief description of the process units.
    (ix) A brief description of the continuous monitoring system.
    (x) The date of the latest continuous monitoring system 
certification or audit.
    (xi) A description of any changes in continuous monitoring systems, 
processes, or controls since the last reporting period.
    (c) Immediate startup, shutdown, and malfunction report. If you had 
a startup, shutdown, or malfunction during the semiannual reporting 
period that was not consistent with your startup, shutdown, and 
malfunction plan, you must submit an immediate startup, shutdown, and 
malfunction report according to the requirements in Sec. 
63.10(d)(5)(ii).
    (d) Part 70 monitoring report. If you have obtained a title V 
operating permit for an affected source pursuant to 40 CFR part 70 or 40 
CFR part 71, you

[[Page 82]]

must report all deviations as defined in this subpart in the semiannual 
monitoring report required by 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A). If you submit a compliance report for an affected 
source along with, or as part of, the semiannual monitoring report 
required by 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A), and 
the compliance report includes all the required information concerning 
deviations from any emission limitation or operation and maintenance 
requirement in this subpart, submission of the compliance report 
satisfies any obligation to report the same deviations in the semiannual 
monitoring report. However, submission of a compliance report does not 
otherwise affect any obligation you may have to report deviations from 
permit requirements for an affected source to your permitting authority.
    (e) Immediate corrective action report. If you had three 
unsuccessful attempts of applying corrective action as described in 
Sec. 63.9634(j) on an emission unit or group of emission units, then 
you must submit an immediate corrective action report. Within 5 calendar 
days after the third unsuccessful attempt at corrective action, you must 
submit to the Administrator a written report in accordance with Sec. 
63.9634(j)(3) and (4). This report must notify the Administrator that a 
deviation has occurred and document the types of corrective measures 
taken to address the problem that resulted in the deviation of 
established operating parameters and the resulting operating limits.



Sec. 63.9642  What records must I keep?

    (a) You must keep the records listed in paragraphs (a)(1) through 
(3) of this section.
    (1) A copy of each notification and report that you submitted to 
comply with this subpart, including all documentation supporting any 
initial notification or notification of compliance status that you 
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
    (2) The records in Sec. 63.6(e)(3)(iii) through (v) related to 
startup, shutdown, and malfunction.
    (3) Records of performance tests and performance evaluations as 
required in Sec. 63.10(b)(2)(viii).
    (b) For each COMS, you must keep the records specified in paragraphs 
(b)(1) through (4) of this section.
    (1) Records described in Sec. 63.10(b)(2)(vi) through (xi).
    (2) Monitoring data for COMS during a performance evaluation as 
required in Sec. 63.6(h)(7)(i) and (ii).
    (3) Previous (that is, superceded) versions of the performance 
evaluation plan as required in Sec. 63.8(d)(3).
    (4) Records of the date and time that each deviation started and 
stopped, and whether the deviation occurred during a period of startup, 
shutdown, or malfunction or during another period.
    (c) You must keep the records required in Sec. Sec. 63.9634 through 
63.9636 to show continuous compliance with each emission limitation, 
work practice standard, and operation and maintenance requirement that 
applies to you.



Sec. 63.9643  In what form and how long must I keep my records?

    (a) Your records must be in a form suitable and readily available 
for expeditious review, according to Sec. 63.10(b)(1).
    (b) As specified in Sec. 63.10(b)(1), you must keep each record for 
5 years following the date of each occurrence, measurement, maintenance, 
corrective action, report, or record.
    (c) You must keep each record on site for at least 2 years after the 
date of each occurrence, measurement, maintenance, corrective action, 
report, or record according to Sec. 63.10(b)(1). You can keep the 
records offsite for the remaining 3 years.

                   Other Requirements and Information



Sec. 63.9650  What parts of the General Provisions apply to me?

    Table 2 to this subpart shows which parts of the General Provisions 
in Sec. Sec. 63.1 through 63.15 apply to you.



Sec. 63.9651  Who implements and enforces this subpart?

    (a) This subpart can be implemented and enforced by us, the EPA, or 
a delegated authority such as your State, local, or tribal agency. If 
the EPA Administrator has delegated authority to your State, local, or 
tribal agency, then that agency has the authority to

[[Page 83]]

implement and enforce this subpart. You should contact your EPA Regional 
Office to find out if this subpart is delegated to your State, local, or 
tribal agency.
    (b) In delegating implementation and enforcement authority of this 
subpart to a State, local, or tribal agency under subpart E of this 
part, the authorities contained in paragraph (c) of this section are 
retained by the Administrator of the EPA and are not transferred to the 
State, local, or tribal agency.
    (c) The authorities that will not be delegated to State, local, or 
tribal agencies are specified in paragraphs (c)(1) through (4) of this 
section.
    (1) Approval of non-opacity emission limitations and work practice 
standards under Sec. 63.6(h)(9) and as defined in Sec. 63.90.
    (2) Approval of major alternatives to test methods under Sec. 
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
    (3) Approval of major alternatives to monitoring under Sec. 63.8(f) 
and as defined in Sec. 63.90.
    (4) Approval of major alternatives to recordkeeping and reporting 
under Sec. 63.10(f) and as defined in Sec. 63.90.



Sec. 63.9652  What definitions apply to this subpart?

    Terms used in this subpart are defined in the Clean Air Act, in 
Sec. 63.2, and in this section as follows.
    Affected source means each new or existing ore crushing and handling 
operation, ore dryer, indurating furnace, or finished pellet handling 
operation, at your taconite iron ore processing plant.
    Bag leak detection system means a system that is capable of 
continuously monitoring relative particulate matter (dust) loadings in 
the exhaust of a baghouse to detect bag leaks and other upset 
conditions. A bag leak detection system includes, but is not limited to, 
an instrument that operates on triboelectric, light scattering, light 
transmittance, or other effect to continuously monitor relative 
particulate matter loadings.
    Conveyor belt transfer point means a point in the conveying 
operation where the taconite ore or taconite pellets are transferred to 
or from a conveyor belt, except where the taconite ore or taconite 
pellets are being transferred to a bin or stockpile.
    Crusher means a machine used to crush taconite ore and includes 
feeders or conveyors located immediately below the crushing surfaces. 
Crushers include, but are not limited to, gyratory crushers and cone 
crushers.
    Deviation means any instance in which an affected source subject to 
this subpart, or an owner or operator of such a source:
    (1) Fails to meet any requirement or obligation established by this 
subpart, including but not limited to any emission limitation (including 
operating limits) or operation and maintenance requirement;
    (2) Fails to meet any term or condition that is adopted to implement 
an applicable requirement in this subpart and that is included in the 
operating permit for any affected source required to obtain such a 
permit; or
    (3) Fails to meet any emission limitation in this subpart during 
startup, shutdown, or malfunction, regardless of whether or not such 
failure is permitted by this subpart.
    Dynamic wet scrubber means an air emissions control device which 
utilizes a mechanically powered fan to cause contact between the process 
exhaust gas stream and the scrubbing liquid which are introduced 
concurrently into the fan inlet.
    Emission limitation means any emission limit, opacity limit, or 
operating limit.
    Finished pellet handling means the transfer of fired taconite 
pellets from the indurating furnace to the finished pellet stockpiles at 
the plant. Finished pellet handling includes, but is not limited to, 
furnace discharge or grate discharge, and finished pellet screening, 
transfer, and storage. The atmospheric pellet cooler vent stack and 
gravity conveyor gallery vents designed to remove heat and water vapor 
from the structure are not included as a part of the finished pellet 
handling affected source.
    Fugitive dust emission source means a stationary source from which 
particles are discharged to the atmosphere due to wind or mechanical 
inducement

[[Page 84]]

such as vehicle traffic. Fugitive dust sources include, but are not 
limited to:
    (1) Stockpiles (includes, but is not limited to, stockpiles of 
uncrushed ore, crushed ore, or finished pellets);
    (2) Material transfer points;
    (3) Plant roadways;
    (4) Tailings basins;
    (5) Pellet loading areas; and
    (6) Yard areas.
    Grate feed means the transfer of unfired taconite pellets from the 
pelletizer into the indurating furnace.
    Grate kiln indurating furnace means a furnace system that consists 
of a traveling grate, a rotary kiln, and an annular cooler. The grate 
kiln indurating furnace begins at the point where the grate feed 
conveyor discharges the green balls onto the furnace traveling grate and 
ends where the hardened pellets exit the cooler. The atmospheric pellet 
cooler vent stack is not included as part of the grate kiln indurating 
furnace.
    Indurating means the process whereby unfired taconite pellets, 
called green balls, are hardened at high temperature in an indurating 
furnace. Types of indurating furnaces include straight grate indurating 
furnaces and grate kiln indurating furnaces.
    Ore crushing and handling means the process whereby dry taconite ore 
is crushed and screened. Ore crushing and handling includes, but is not 
limited to, all dry crushing operations (e.g., primary, secondary, and 
tertiary crushing), dry ore conveyance and transfer points, dry ore 
classification and screening, dry ore storage and stockpiling, dry 
milling, dry cobbing (i.e., dry magnetic separation), and the grate 
feed. Ore crushing and handling specifically excludes any operations 
where the dry crushed ore is saturated with water, such as wet milling 
and wet magnetic separation.
    Ore dryer means a rotary dryer that repeatedly tumbles wet taconite 
ore concentrate through a heated air stream to reduce the amount of 
entrained moisture in the taconite ore concentrate.
    Pellet cooler vent stacks means atmospheric vents in the cooler 
section of the grate kiln indurating furnace that exhaust cooling air 
that is not returned for recuperation. Pellet cooler vent stacks are not 
to be confused with the cooler discharge stack, which is in the pellet 
loadout or dumping area.
    Pellet loading area means that portion of a taconite iron ore 
processing plant where taconite pellets are loaded into trucks or 
railcars.
    Responsible official means responsible official as defined in Sec. 
63.2.
    Rod-deck venturi scrubber means a wet scrubber emission control 
device in which the inlet air flows through a bed of parallel metal 
pipes spaced apart to produce a series of parallel venturi throats.
    Screen means a device for separating material according to size by 
passing undersize material through one or more mesh surfaces (screens) 
in series and retaining oversize material on the mesh surfaces 
(screens).
    Storage bin means a facility for storage (including surge bins and 
hoppers) of taconite ore or taconite pellets prior to further processing 
or loading.
    Straight grate indurating furnace means a furnace system that 
consists of a traveling grate that carries the taconite pellets through 
different furnace temperature zones. In the straight grate indurating 
furnace a layer of fired pellets, called the hearth layer, is placed on 
the traveling grate prior to the addition of unfired pellets. The 
straight grate indurating furnace begins at the point where the grate 
feed conveyor discharges the green balls onto the furnace traveling 
grate and ends where the hardened pellets drop off of the traveling 
grate.
    Taconite iron ore processing means the separation and concentration 
of iron ore from taconite, a low-grade iron ore, to produce taconite 
pellets.
    Taconite ore means a low-grade iron ore suitable for concentration 
of magnetite or hematite by fine grinding and magnetic or flotation 
treatment, from which pellets containing iron can be produced.
    Tailings basin means a natural or artificial impoundment in which 
gangue or other refuse material resulting from the washing, 
concentration or treatment of ground taconite iron ore is confined.
    Wet grinding and milling means the process whereby wet taconite ore 
is

[[Page 85]]

finely ground using rod and/or ball mills.

          Table 1 to Subpart RRRRR of Part 63--Emission Limits

    As required in Sec. 63.9590(a), you must comply with each 
applicable emission limit in the following table:

----------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
 
 
 
----------------------------------------------------------------------------------------------------------------
1. Ore crushing and handling emission  Existing..................................  0.008 grains per dry standard
 units.                                                                             cubic foot (gr/dscf).
                                       New.......................................  0.005 gr/dscf.
2. Straight grate indurating furnace   Existing..................................  0.01 gr/dscf.
 processing magnetite.                 New.......................................  0.006 gr/dscf.
3. Grate kiln indurating furnace       Existing..................................  0.01 gr/dscf.
 processing magnetite.                 New.......................................  0.006 gr/dscf.
4. Grate kiln indurating furnace       Existing..................................  0.03 gr/dscf.
 processing hematite.                  New.......................................  0.018 gr/dscf.
5. Finished pellet handling emission   Existing..................................  0.008 gr/dscf.
 units.                                New.......................................  0.005 gr/dscf.
6. Ore dryer.........................  Existing..................................  0.052 gr/dscf.
                                       New.......................................  0.025 gr/dscf.
----------------------------------------------------------------------------------------------------------------

Table 2 to Subpart RRRRR of Part 63--Applicability of General Provisions 
                       to Subpart RRRRR of Part 63

    As required in Sec. 63.9650, you must comply with the requirements 
of the NESHAP General Provisions (40 CFR part 63, subpart A) shown in 
the following table:

----------------------------------------------------------------------------------------------------------------
             Citation                       Subject            Applies to Subpart RRRRR         Explanation
----------------------------------------------------------------------------------------------------------------
Sec. 63.1.......................  Applicability.........  Yes.
Sec. 63.2.......................  Definitions...........  Yes.
Sec. 63.3.......................  Units and               Yes.
                                     Abbreviations.
Sec. 63.4.......................  Prohibited Activities.  Yes.
Sec. 63.5.......................  Construction/           Yes.
                                     Reconstruction.
Sec. 63.6(a)-(g)................  Compliance With         Yes.
                                     Standards and
                                     Maintenance
                                     Requirements.
Sec. 63.6(h)....................  Compliance With         No...........................  Subpart RRRRR does
                                     Opacity and Visible                                    not contain opacity
                                     Emission (VE)                                          and VE standards.
                                     Standards.
Sec. 63.6(i), (j)...............  Extension of            Yes.
                                     Compliance and
                                     Presidential
                                     Compliance Extension.
Sec. 63.7(a)(1)-(2).............  Applicability and       No...........................  Subpart RRRRR
                                     Performance Test                                       specifies
                                     Dates.                                                 performance test
                                                                                            applicability and
                                                                                            dates.
Sec. 63.7(a)(3), (b)-(h)........  Performance Testing     Yes.
                                     Requirements.
Sec. 63.8(a)(1)-(a)(3), (b),      Monitoring              Yes..........................  Continuous monitoring
 (c)(1)-(3), (c)(5)-(8), (d), (e),   Requirements.                                          system (CMS)
 (f)(1)-(5), (g)(1)-(4).                                                                    requirements in Sec.
                                                                                              63.8(c)(5) and (6)
                                                                                            apply only to COMS
                                                                                            for dry
                                                                                            electrostatic
                                                                                            precipitators.
Sec. 63.8(a)(4).................  Additional Monitoring   No...........................  Subpart RRRRR does
                                     Requirements for                                       not require flares.
                                     Control Devices in
                                     Sec. 63.11.
Sec. 63.8(c)(4).................  Continuous Monitoring   No...........................  Subpart RRRRR
                                     System Requirements.                                   specifies
                                                                                            requirements for
                                                                                            operation of CMS.
Sec. 63.8(f)(6).................  Relative Accuracy Test  No...........................  Subpart RRRRR does
                                     Alternative (RATA).                                    not require
                                                                                            continuous emission
                                                                                            monitoring systems.
Sec. 63.8(g)(5).................  Data Reduction........  No...........................  Subpart RRRRR
                                                                                            specifies data
                                                                                            reduction
                                                                                            requirements.

[[Page 86]]

 
Sec. 63.9.......................  Notification            Yes..........................  Additional
                                     Requirements.                                          notifications for
                                                                                            CMS in Sec.
                                                                                            63.9(g) apply to
                                                                                            COMS for dry
                                                                                            electrostatic
                                                                                            precipitators.
Sec. 63.10(a), (b)(1)-(2)(xii),   Recordkeeping and       Yes..........................  Additional records
 (b)(2)(xiv), (b)(3), (c)(1)-(6),    Reporting                                              for CMS in Sec.
 (c)(9)-(15), (d)(1)-(2), (d)(4)-    Requirements.                                          63.10(c)(1)-(6), (9)-
 (5), (e), (f).                                                                             (15), and reports in
                                                                                            Sec. 63.10(d)(1)-
                                                                                            (2) apply only to
                                                                                            COMS for dry
                                                                                            electrostatic
                                                                                            precipitators.
Sec. 63.10(b)(2)(xiii)..........  CMS Records for RATA    No...........................  Subpart RRRRR doesn't
                                     Alternative.                                           require continuous
                                                                                            emission monitoring
                                                                                            systems.
Sec. 63.10(c)(7)-(8)............  Records of Excess       No...........................  Subpart RRRRR
                                     Emissions and                                          specifies record
                                     Parameter Monitoring                                   requirements.
                                     Exceedances for CMS.
Sec. 63.10(d)(3)................  Reporting opacity or    No...........................  Subpart RRRRR does
                                     VE observations.                                       not have opacity and
                                                                                            VE standards.
Sec. 63.11......................  Control Device          No...........................  Subpart RRRRR does
                                     Requirements.                                          not require flares.
Sec. 63.12......................  State Authority and     Yes.
                                     Delegations.
Sec. 63.13-Sec. 63.15.........  Addresses,              Yes.
                                     Incorporation by
                                     Reference,
                                     Availability of
                                     Information.
----------------------------------------------------------------------------------------------------------------

 Subpart SSSSS_National Emission Standards for Hazardous Air Pollutants 
                  for Refractory Products Manufacturing

    Source: 68 FR 18747, Apr. 16, 2003, unless otherwise noted.

                        What This Subpart Covers



Sec. 63.9780  What is the purpose of this subpart?

    This subpart establishes national emission standards for hazardous 
air pollutants (NESHAP) for refractory products manufacturing 
facilities. This subpart also establishes requirements to demonstrate 
initial and continuous compliance with the emission limitations.



Sec. 63.9782  Am I subject to this subpart?

    You are subject to this subpart if you own or operate a refractory 
products manufacturing facility that is, is located at, or is part of, a 
major source of hazardous air pollutant (HAP) emissions according to the 
criteria in paragraphs (a) and (b) of this section.
    (a) A refractory products manufacturing facility is a plant site 
that manufactures refractory products (refractory bricks, refractory 
shapes, monolithics, kiln furniture, crucibles, and other materials used 
for lining furnaces and other high temperature process units), as 
defined in Sec. 63.9824. Refractory products manufacturing facilities 
typically process raw material by crushing, grinding, and screening; 
mixing the processed raw materials with binders and other additives; 
forming the refractory mix into shapes; and drying and firing the 
shapes.
    (b) A major source of HAP is a plant site that emits or has the 
potential to emit any single HAP at a rate of 9.07 megagrams (10 tons) 
or more per year or any combination of HAP at a rate of 22.68 megagrams 
(25 tons) or more per year.



Sec. 63.9784  What parts of my plant does this subpart cover?

    (a) This subpart applies to each new, reconstructed, or existing 
affected source at a refractory products manufacturing facility.
    (b) The existing affected sources are shape dryers, curing ovens, 
and kilns that are used to manufacture refractory products that use 
organic HAP; shape preheaters, pitch working tanks, defumers, and coking 
ovens that are used to produce pitch-impregnated refractory products; 
kilns that are used to manufacture chromium refractory products; and 
kilns that are used to manufacture clay refractory products.

[[Page 87]]

    (c) The new or reconstructed affected sources are shape dryers, 
curing ovens, and kilns that are used to manufacture refractory products 
that use organic HAP; shape preheaters, pitch working tanks, defumers, 
and coking ovens used to produce pitch-impregnated refractory products; 
kilns that are used to manufacture chromium refractory products; and 
kilns that are used to manufacture clay refractory products.
    (d) Shape dryers, curing ovens, kilns, coking ovens, defumers, shape 
preheaters, and pitch working tanks that are research and development 
(R&D) process units are not subject to the requirements of this subpart. 
(See definition of research and development process unit in Sec. 
63.9824).
    (e) A source is a new affected source if you began construction of 
the affected source after June 20, 2002, and you met the applicability 
criteria at the time you began construction.
    (f) An affected source is reconstructed if you meet the criteria as 
defined in Sec. 63.2.
    (g) An affected source is existing if it is not new or 
reconstructed.



Sec. 63.9786  When do I have to comply with this subpart?

    (a) If you have a new or reconstructed affected source, you must 
comply with this subpart according to paragraphs (a)(1) and (2) of this 
section.
    (1) If the initial startup of your affected source is before April 
16, 2003, then you must comply with the emission limitations for new and 
reconstructed sources in this subpart no later than April 16, 2003.
    (2) If the initial startup of your affected source is after April 
16, 2003, then you must comply with the emission limitations for new and 
reconstructed sources in this subpart upon initial startup of your 
affected source.
    (b) If you have an existing affected source, you must comply with 
the emission limitations for existing sources no later than April 17, 
2006.
    (c) You must be in compliance with this subpart when you conduct a 
performance test on an affected source.
    (d) If you have an existing area source that increases its emissions 
or its potential to emit such that it becomes a major source of HAP, you 
must be in compliance with this subpart according to paragraphs (d)(1) 
and (2) of this section.
    (1) Any portion of the existing facility that is a new affected 
source or a new reconstructed source must be in compliance with this 
subpart upon startup.
    (2) All other parts of the existing facility must be in compliance 
with this subpart by 3 years after the date the area source becomes a 
major source.
    (e) If you have a new area source (i.e., an area source for which 
construction or reconstruction was commenced after June 20, 2002) that 
increases its emissions or its potential to emit such that it becomes a 
major source of HAP, you must be in compliance with this subpart upon 
initial startup of your affected source as a major source.
    (f) You must meet the notification requirements in Sec. 63.9812 
according to the schedule in Sec. 63.9812 and in 40 CFR part 63, 
subpart A. Some of the notifications must be submitted before you are 
required to comply with the emission limitations in this subpart.

            Emission Limitations and Work Practice Standards



Sec. 63.9788  What emission limits, operating limits, and work practice 
standards must I meet?

    (a) You must meet each emission limit in Table 1 to this subpart 
that applies to you.
    (b) You must meet each operating limit in Table 2 to this subpart 
that applies to you.
    (c) You must meet each work practice standard in Table 3 to this 
subpart that applies to you.



Sec. 63.9790  What are my options for meeting the emission limits?

    To meet the emission limits in Table 1 to this subpart, you must use 
one or both of the options listed in paragraphs (a) and (b) of this 
section.
    (a) Emissions control system. Use an emissions capture and 
collection system and an add-on air pollution control device (APCD) and 
demonstrate that the resulting emissions or emissions reductions meet 
the applicable emission limits in Table 1 to this subpart, and 
demonstrate that the capture and collection system and APCD meet the

[[Page 88]]

applicable operating limits in Table 2 to this subpart.
    (b) Process changes. Use raw materials that have little or no 
potential to emit HAP during the refractory products manufacturing 
process or implement manufacturing process changes and demonstrate that 
the resulting emissions or emissions reductions meet the applicable 
emission limits in Table 1 to this subpart without an add-on APCD.

                     General Compliance Requirements



Sec. 63.9792  What are my general requirements for complying with this subpart?

    (a) You must be in compliance with the emission limitations 
(including operating limits and work practice standards) in this subpart 
at all times, except during periods specified in paragraphs (a)(1) and 
(2) of this section.
    (1) Periods of startup, shutdown, and malfunction.
    (2) Periods of scheduled maintenance on a control device that is 
used on an affected continuous kiln, as specified in paragraph (e) of 
this section.
    (b) Except as specified in paragraph (e) of this section, you must 
always operate and maintain your affected source, including air 
pollution control and monitoring equipment, according to the provisions 
in Sec. 63.6(e)(1)(i). During the period between the compliance date 
specified for your affected source in Sec. 63.9786 and the date upon 
which continuous monitoring systems have been installed and validated 
and any applicable operating limits have been established, you must 
maintain a log detailing the operation and maintenance of the process 
and emissions control equipment.
    (c) You must develop and implement a written startup, shutdown, and 
malfunction plan (SSMP) according to the provisions in Sec. 63.6(e)(3).
    (d) You must prepare and implement a written operation, maintenance, 
and monitoring (OM&M) plan according to the requirements in Sec. 
63.9794.
    (e) If you own or operate an affected continuous kiln and must 
perform scheduled maintenance on the control device for that kiln, you 
may bypass the kiln control device and continue operating the kiln upon 
approval by the Administrator, provided you satisfy the conditions 
listed in paragraphs (e)(1) through (3) of this section.
    (1) You must request approval from the Administrator to bypass the 
control device while the scheduled maintenance is performed. You must 
submit a separate request each time you plan to bypass the control 
device, and your request must include the information specified in 
paragraphs (e)(1)(i) through (vi) of this section.
    (i) Reason for the scheduled maintenance.
    (ii) Explanation for why the maintenance cannot be performed when 
the kiln is shut down.
    (iii) Detailed description of the maintenance activities.
    (iv) Time required to complete the maintenance.
    (v) How you will minimize HAP emissions from the kiln during the 
period when the control device is out of service.
    (vi) How you will minimize the time when the kiln is operating and 
the control device is out of service for scheduled maintenance.
    (2) You must minimize HAP emissions during the period when the kiln 
is operating and the control device is out of service.
    (3) You must minimize the time period during which the kiln is 
operating and the control device is out of service.
    (f) You must be in compliance with the provisions of subpart A of 
this part, except as noted in Table 11 to this subpart.



Sec. 63.9794  What do I need to know about operation, maintenance, and 
monitoring plans?

    (a) For each continuous parameter monitoring system (CPMS) required 
by this subpart, you must develop, implement, make available for 
inspection, and revise, as necessary, an OM&M plan that includes the 
information in paragraphs (a)(1) through (13) of this section.
    (1) A list and identification of each process and add-on APCD that 
is required by this subpart to be monitored, the type of monitoring 
device that will be used, and the operating parameters that will be 
monitored.

[[Page 89]]

    (2) Specifications for the sensor, signal analyzer, and data 
collection system.
    (3) A monitoring schedule that specifies the frequency that the 
parameter values will be determined and recorded.
    (4) The operating limits for each parameter that represent 
continuous compliance with the emission limitations in Sec. 63.9788, 
based on values of the monitored parameters recorded during performance 
tests.
    (5) Procedures for installing the CPMS at a measurement location 
relative to each process unit or APCD such that measurement is 
representative of control of emissions.
    (6) Procedures for the proper operation and routine and long-term 
maintenance of each process unit and APCD, including a maintenance and 
inspection schedule that is consistent with the manufacturer's 
recommendations.
    (7) Procedures for the proper operation and maintenance of 
monitoring equipment consistent with the requirements in Sec. Sec. 
63.8(c)(1), (3), (4)(ii), (7), and (8), and 63.9804.
    (8) Ongoing data quality assurance procedures in accordance with the 
general requirements of Sec. 63.8(d).
    (9) Procedures for evaluating the performance of each CPMS.
    (10) Procedures for responding to operating parameter deviations, 
including the procedures in paragraphs (a)(10)(i) through (iii) of this 
section:
    (i) Procedures for determining the cause of the operating parameter 
deviation.
    (ii) Actions for correcting the deviation and returning the 
operating parameters to the allowable limits.
    (iii) Procedures for recording the times that the deviation began 
and ended, and when corrective actions were initiated and completed.
    (11) Procedures for keeping records to document compliance and 
reporting in accordance with the requirements of Sec. 63.10(c), (e)(1), 
and (e)(2)(i).
    (12) If you operate a kiln that is subject to the limits on the type 
of fuel used, as specified in items 3 and 4 of Table 3 to subpart SSSSS, 
procedures for using alternative fuels.
    (13) If you operate an affected continuous kiln and you plan to take 
the kiln control device out of service for scheduled maintenance, as 
specified in Sec. 63.9792(e), the procedures specified in paragraphs 
(a)(13)(i) and (ii) of this section.
    (i) Procedures for minimizing HAP emissions from the kiln during 
periods of scheduled maintenance of the kiln control device when the 
kiln is operating and the control device is out of service.
    (ii) Procedures for minimizing any period of scheduled maintenance 
on the kiln control device when the kiln is operating and the control 
device is out of service.
    (b) Changes to the operating limits in your OM&M plan require a new 
performance test. If you are revising an operating limit parameter 
value, you must meet the requirements in paragraphs (b)(1) and (2) of 
this section.
    (1) Submit a Notification of Performance Test to the Administrator 
as specified in Sec. 63.7(b).
    (2) After completing the performance tests to demonstrate that 
compliance with the emission limits can be achieved at the revised 
operating limit parameter value, you must submit the performance test 
results and the revised operating limits as part of the Notification of 
Compliance Status required under Sec. 63.9(h).
    (c) If you are revising the inspection and maintenance procedures in 
your OM&M plan, you do not need to conduct a new performance test.

               Testing and Initial Compliance Requirements



Sec. 63.9796  By what date must I conduct performance tests?

    You must conduct performance tests within 180 calendar days after 
the compliance date that is specified for your source in Sec. 63.9786 
and according to the provisions in Sec. 63.7(a)(2).



Sec. 63.9798  When must I conduct subsequent performance tests?

    (a) You must conduct a performance test every 5 years following the 
initial performance test, as part of renewing your 40 CFR part 70 or 40 
CFR part 71 operating permit.

[[Page 90]]

    (b) You must conduct a performance test when you want to change the 
parameter value for any operating limit specified in your OM&M plan.
    (c) If you own or operate a source that is subject to the emission 
limits specified in items 2 through 9 of Table 1 to this subpart, you 
must conduct a performance test on the source(s) listed in paragraphs 
(c)(1) and (2) of this section before you start production of any 
refractory product for which the organic HAP processing rate is likely 
to exceed by more than 10 percent the maximum organic HAP processing 
rate established during the most recent performance test on that same 
source.
    (1) Each affected shape dryer or curing oven that is used to process 
the refractory product with the higher organic HAP processing rate.
    (2) Each affected kiln that follows an affected shape dryer or 
curing oven and is used to process the refractory product with the 
higher organic HAP processing rate.
    (d) If you own or operate a kiln that is subject to the emission 
limits specified in item 5 or 9 of Table 1 to this subpart, you must 
conduct a performance test on the affected kiln following any process 
changes that are likely to increase organic HAP emissions from the kiln 
(e.g., a decrease in the curing cycle time for a curing oven that 
precedes the affected kiln in the process line).
    (e) If you own or operate a clay refractory products kiln that is 
subject to the emission limits specified in item 10 or 11 of Table 1 to 
this subpart and is controlled with a dry limestone adsorber (DLA), you 
must conduct a performance test on the affected kiln following any 
change in the source of limestone used in the DLA.



Sec. 63.9800  How do I conduct performance tests and establish operating 
limits?

    (a) You must conduct each performance test in Table 4 to this 
subpart that applies to you.
    (b) Before conducting the performance test, you must install and 
validate all monitoring equipment.
    (c) Each performance test must be conducted according to the 
requirements in Sec. 63.7 and under the specific conditions in Table 4 
to this subpart.
    (d) You may not conduct performance tests during periods of startup, 
shutdown, or malfunction, as specified in Sec. 63.7(e)(1).
    (e) You must conduct separate test runs for at least the duration 
specified for each performance test required in this section, as 
specified in Sec. 63.7(e)(3) and Table 4 to this subpart.
    (f) For batch process sources, you must satisfy the requirements 
specified in paragraphs (f)(1) through (5) of this section.
    (1) You must conduct at least two test runs.
    (2) Each test run must last an entire batch cycle unless you develop 
an emissions profile, as specified in items 8(a)(i)(4) and 17(b)(i)(4) 
of Table 4 to this subpart, or you satisfy the conditions for 
terminating a test run prior to the completion of a batch cycle as 
specified in item 8(a)(i)(5) of Table 4 to this subpart.
    (3) Each test run must be performed over a separate batch cycle 
unless you satisfy the conditions for conducting both test runs over a 
single batch cycle, as described in paragraphs (f)(3)(i) and (ii) of 
this section.
    (i) You do not produce the product that corresponds to the maximum 
organic HAP processing rate for that batch process source in consecutive 
batch cycles.
    (ii) To produce that product in two consecutive batch cycles would 
disrupt production of other refractory products.
    (4) If you want to conduct a performance test over a single batch 
cycle, you must include in your Notification of Performance Test the 
rationale for testing over a single batch cycle.
    (5) If you are granted approval to conduct a performance test over a 
single batch cycle, you must use paired sampling trains and collect two 
sets of emissions data. Each set of data can be considered a separate 
test run.
    (g) You must use the data gathered during the performance test and 
the equations in paragraphs (g)(1) through (3) of this section to 
determine compliance with the emission limitations.

[[Page 91]]

    (1) To determine compliance with the total hydrocarbon (THC) 
emission concentration limit listed in Table 1 to this subpart, you must 
calculate your emission concentration corrected to 18 percent oxygen for 
each test run using Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR16AP03.000

Where:

C THC-C=THC concentration, corrected to 18 percent oxygen, 
parts per million by volume, dry basis (ppmvd)
C THC=THC concentration (uncorrected), ppmvd
CO2=oxygen concentration, percent.

    (2) To determine compliance with any of the emission limits based on 
percentage reduction across an emissions control system specified in 
Table 1 to this subpart, you must calculate the percentage reduction for 
each test run using Equation 2 of this section:
[GRAPHIC] [TIFF OMITTED] TR16AP03.001

Where:

PR=percentage reduction, percent
ERi=mass emissions rate of specific HAP or pollutant (THC, 
HF, or HCl) entering the control device, kilograms (pounds) per hour
ERo=mass emissions rate of specific HAP or pollutant (THC, 
HF, or HCl) exiting the control device, kilograms (pounds) per hour.

    (3) To determine compliance with production-based hydrogen fluoride 
(HF) and hydrogen chloride (HCl) emission limits in Table 1 to this 
subpart, you must calculate your mass emissions per unit of uncalcined 
clay processed for each test run using Equation 3 of this section:
[GRAPHIC] [TIFF OMITTED] TR16AP03.002

Where:

MP=mass per unit of production, kilograms of pollutant per megagram 
(pounds per ton) of uncalcined clay processed
ER=mass emissions rate of specific HAP (HF or HCl) during each 
performance test run, kilograms (pounds) per hour
P=average uncalcined clay processing rate for the performance test, 
megagrams (tons) of uncalcined clay processed per hour.

    (h) You must establish each site-specific operating limit in Table 2 
to this subpart that applies to you, as specified in Table 4 to this 
subpart.
    (i) For each affected source that is equipped with an add-on APCD 
that is not addressed in Table 2 to this subpart or that is using 
process changes as a means of meeting the emission limits in Table 1 to 
this subpart, you must meet the requirements in Sec. 63.8(f) and 
paragraphs (i)(1) through (3) of this section.
    (1) For sources subject to the THC concentration limit specified in 
item 3 or 7 of Table 1 to this subpart, you must satisfy the 
requirements specified in paragraphs (i)(1)(i) through (iii) of this 
section.
    (i) You must install a THC continuous emissions monitoring system 
(CEMS) at the outlet of the control device or in the stack of the 
affected source.
    (ii) You must meet the requirements specified in Performance 
Specification (PS) 8 of 40 CFR part 60, appendix B.
    (iii) You must meet the requirements specified in Procedure 1 of 40 
CFR part 60, appendix F.
    (2) For sources subject to the emission limits specified in item 3, 
4, 7, or 8 of Table 1 to this subpart, you must submit a request for 
approval of alternative monitoring methods to the Administrator no later 
than the submittal date for the Notification of Performance Test, as 
specified in Sec. 63.9812(d). The request must contain the information 
specified in paragraphs (i)(2)(i) through (v) of this section.
    (i) Description of the alternative add-on APCD or process changes.
    (ii) Type of monitoring device or method that will be used, 
including the sensor type, location, inspection procedures, quality 
assurance and quality control measures, and data recording device.
    (iii) Operating parameters that will be monitored.
    (iv) Frequency that the operating parameter values will be 
determined and recorded to establish continuous compliance with the 
operating limits.
    (v) Averaging time.

[[Page 92]]

    (3) You must establish site-specific operating limits during the 
performance test based on the information included in the approved 
alternative monitoring methods request and, as applicable, as specified 
in Table 4 to this subpart.



Sec. 63.9802  How do I develop an emissions profile?

    If you decide to develop an emissions profile for an affected batch 
process source; as indicated in item 8(a)(i)(4) or 17(b)(i)(4) of Table 
4 to this subpart, you must measure and record mass emissions of the 
applicable pollutant throughout a complete batch cycle of the affected 
batch process source according to the procedures described in paragraph 
(a) or (b) of this section.
    (a) If your affected batch process source is subject to the THC 
concentration limit specified in item 6(a), 7(a), 8, or 9 of Table 1 to 
this subpart or the THC percentage reduction limit specified in item 
6(b) or 7(b) of Table 1 to this subpart, you must measure and record the 
THC mass emissions rate at the inlet to the control device using the 
test methods, averaging periods, and procedures specified in items 10(a) 
and (b) of Table 4 to this subpart for each complete hour of the batch 
process cycle.
    (b) If your affected batch process source is subject to the HF and 
HCl percentage reduction emission limits in item 11 of Table 1 to this 
subpart, you must measure and record the HF mass emissions rate at the 
inlet to the control device through a series of 1-hour test runs 
according to the test method specified in item 14(a) of Table 4 to this 
subpart for each complete hour of the batch process cycle.



Sec. 63.9804  What are my monitoring system installation, operation, 
and maintenance requirements?

    (a) You must install, operate, and maintain each CPMS required by 
this subpart according to your OM&M plan and the requirements in 
paragraphs (a)(1) through (15) of this section.
    (1) You must satisfy all applicable requirements of performance 
specifications for CPMS specified in 40 CFR part 60, appendix B, upon 
promulgation of such performance specifications.
    (2) You must satisfy all applicable requirements of quality 
assurance (QA) procedures for CPMS specified in 40 CFR part 60, appendix 
F, upon promulgation of such QA procedures.
    (3) You must install each sensor of your CPMS in a location that 
provides representative measurement of the appropriate parameter over 
all operating conditions, taking into account the manufacturer's 
guidelines.
    (4) You must use a CPMS that is capable of measuring the appropriate 
parameter over a range that extends from a value of at least 20 percent 
less than the lowest value that you expect your CPMS to measure, to a 
value of at least 20 percent greater than the highest value that you 
expect your CPMS to measure.
    (5) You must use a data acquisition and recording system that is 
capable of recording values over the entire range specified in paragraph 
(a)(4) of this section.
    (6) You must use a signal conditioner, wiring, power supply, and 
data acquisition and recording system that are compatible with the 
output signal of the sensors used in your CPMS.
    (7) You must perform an initial calibration of your CPMS based on 
the procedures specified in the manufacturer's owner's manual.
    (8) You must use a CPMS that is designed to complete a minimum of 
one cycle of operation for each successive 15-minute period. To have a 
valid hour of data, you must have at least three of four equally-spaced 
data values (or at least 75 percent of the total number of values if you 
collect more than four data values per hour) for that hour (not 
including startup, shutdown, malfunction, or out-of-control periods).
    (9) You must record valid data from at least 90 percent of the hours 
during which the affected source or process operates.
    (10) You must determine and record the 15-minute block averages of 
all measurements, calculated after every 15 minutes of operation as the 
average of the previous 15 operating minutes (not including periods of 
startup, shutdown, or malfunction).
    (11) You must determine and record the 3-hour block averages of all 
15-

[[Page 93]]

minute recorded measurements, calculated after every 3 hours of 
operation as the average of the previous 3 operating hours (not 
including periods of startup, shutdown, or malfunction).
    (12) You must record the results of each inspection, calibration, 
initial validation, and accuracy audit.
    (13) At all times, you must maintain your CPMS including, but not 
limited to, maintaining necessary parts for routine repairs of the CPMS.
    (14) You must perform an initial validation of your CPMS under the 
conditions specified in paragraphs (14)(i) and (ii) of this section.
    (i) Prior to the initial performance test on the affected source for 
which the CPMS is required.
    (ii) Within 180 days of your replacing or relocating one or more of 
the sensors of your CPMS.
    (15) Except for redundant sensors, as defined in Sec. 63.9824, any 
device that you use to conduct an initial validation or accuracy audit 
of your CPMS must meet the accuracy requirements specified in paragraphs 
(15)(i) and (ii) of this section.
    (i) The device must have an accuracy that is traceable to National 
Institute of Standards and Technology (NIST) standards.
    (ii) The device must be at least three times as accurate as the 
required accuracy for the CPMS.
    (b) For each temperature CPMS that is used to monitor the combustion 
chamber temperature of a thermal oxidizer or the catalyst bed inlet 
temperature of a catalytic oxidizer, you must meet the requirements in 
paragraphs (a) and (b)(1) through (6) of this section.
    (1) Use a temperature CPMS with a minimum accuracy of 1.0 percent of the temperature value or 2.8 degrees 
Celsius ( [deg]C) (5 degrees Fahrenheit ( [deg]F)), whichever is 
greater.
    (2) Use a data recording system with a minimum resolution of one-
half or better of the required CPMS accuracy specified in paragraph 
(b)(1) of this section.
    (3) Perform an initial validation of your CPMS according to the 
requirements in paragraph (3)(i) or (ii) of this section.
    (i) Place the sensor of a calibrated temperature measurement device 
adjacent to the sensor of your temperature CPMS in a location that is 
subject to the same environment as the sensor of your temperature CPMS. 
The calibrated temperature measurement device must satisfy the accuracy 
requirements of paragraph (a)(15) of this section. While the process and 
control device that is monitored by your CPMS are operating normally, 
record concurrently and compare the temperatures measured by your 
temperature CPMS and the calibrated temperature measurement device. 
Using the calibrated temperature measurement device as the reference, 
the temperature measured by your CPMS must be within the accuracy 
specified in paragraph (b)(1) of this section.
    (ii) Perform any of the initial validation methods for temperature 
CPMS specified in performance specifications for CPMS established in 40 
CFR part 60, appendix B.
    (4) Perform an accuracy audit of your temperature CPMS at least 
quarterly, according to the requirements in paragraph (b)(4)(i), (ii), 
or (iii) of this section.
    (i) If your temperature CPMS includes a redundant temperature 
sensor, record three pairs of concurrent temperature measurements within 
a 24-hour period. Each pair of concurrent measurements must consist of a 
temperature measurement by each of the two temperature sensors. The 
minimum time interval between any two such pairs of consecutive 
temperature measurements is 1 hour. The measurements must be taken 
during periods when the process and control device that is monitored by 
your temperature CPMS are operating normally. Calculate the mean of the 
three values for each temperature sensor. The mean values must agree 
within the required overall accuracy of the CPMS, as specified in 
paragraph (b)(1) of this section.
    (ii) If your temperature CPMS does not include a redundant 
temperature sensor, place the sensor of a calibrated temperature 
measurement device adjacent to the sensor of your temperature CPMS in a 
location that is subject to the same environment as the sensor of

[[Page 94]]

your temperature CPMS. The calibrated temperature measurement device 
must satisfy the accuracy requirements of paragraph (a)(15) of this 
section. While the process and control device that is monitored by your 
temperature CPMS are operating normally, record concurrently and compare 
the temperatures measured by your CPMS and the calibrated temperature 
measurement device. Using the calibrated temperature measurement device 
as the reference, the temperature measured by your CPMS must be within 
the accuracy specified in paragraph (b)(1) of this section.
    (iii) Perform any of the accuracy audit methods for temperature CPMS 
specified in QA procedures for CPMS established in 40 CFR part 60, 
appendix F.
    (5) Conduct an accuracy audit of your CPMS following any 24-hour 
period throughout which the temperature measured by your CPMS exceeds 
the manufacturer's specified maximum operating temperature range, or 
install a new temperature sensor.
    (6) If your CPMS is not equipped with a redundant temperature 
sensor, perform at least quarterly a visual inspection of all components 
of the CPMS for integrity, oxidation, and galvanic corrosion.
    (c) For each pressure CPMS that is used to monitor the pressure drop 
across a DLA or wet scrubber, you must meet the requirements in 
paragraphs (a) and (c)(1) through (7) of this section.
    (1) Use a pressure CPMS with a minimum accuracy of 5.0 percent or 0.12 kilopascals (kPa) (0.5 inches of 
water column (in. w.c.)), whichever is greater.
    (2) Use a data recording system with a minimum resolution of one-
half the required CPMS accuracy specified in paragraph (c)(1) of this 
section, or better.
    (3) Perform an initial validation of your pressure CPMS according to 
the requirements in paragraph (c)(3)(i) or (ii) of this section.
    (i) Place the sensor of a calibrated pressure measurement device 
adjacent to the sensor of your pressure CPMS in a location that is 
subject to the same environment as the sensor of your pressure CPMS. The 
calibrated pressure measurement device must satisfy the accuracy 
requirements of paragraph (a)(15) of this section. While the process and 
control device that is monitored by your CPMS are operating normally, 
record concurrently and compare the pressure measured by your CPMS and 
the calibrated pressure measurement device. Using the calibrated 
pressure measurement device as the reference, the pressure measured by 
your CPMS must be within the accuracy specified in paragraph (c)(1) of 
this section.
    (ii) Perform any of the initial validation methods for pressure CPMS 
specified in performance specifications for CPMS established in 40 CFR 
part 60, appendix B.
    (4) Perform an accuracy audit of your pressure CPMS at least 
quarterly, according to the requirements in paragraph (c)(4)(i), (ii), 
or (iii) of this section.
    (i) If your pressure CPMS includes a redundant pressure sensor, 
record three pairs of concurrent pressure measurements within a 24-hour 
period. Each pair of concurrent measurements must consist of a pressure 
measurement by each of the two pressure sensors. The minimum time 
interval between any two such pairs of consecutive pressure measurements 
is 1 hour. The measurements must be taken during periods when the 
process and control device that is monitored by your CPMS are operating 
normally. Calculate the mean of the three pressure measurement values 
for each pressure sensor. The mean values must agree within the required 
overall accuracy of the CPMS, as specified in paragraph (c)(1) of this 
section.
    (ii) If your pressure CPMS does not include a redundant pressure 
sensor, place the sensor of a calibrated pressure measurement device 
adjacent to the sensor of your pressure CPMS in a location that is 
subject to the same environment as the sensor of your pressure CPMS. The 
calibrated pressure measurement device must satisfy the accuracy 
requirements of paragraph (a)(15) of this section. While the process and 
control device that is monitored by your pressure CPMS are operating 
normally, record concurrently and compare the pressure measured by your 
CPMS and the calibrated pressure

[[Page 95]]

measurement device. Using the calibrated pressure measurement device as 
the reference, the pressure measured by your CPMS must be within the 
accuracy specified in paragraph (c)(1) of this section.
    (iii) Perform any of the accuracy audit methods for pressure CPMS 
specified in QA procedures for CPMS established in 40 CFR part 60, 
appendix F.
    (5) Conduct an accuracy audit of your CPMS following any 24-hour 
period throughout which the pressure measured by your CPMS exceeds the 
manufacturer's specified maximum operating pressure range, or install a 
new pressure sensor.
    (6) At least monthly, check all mechanical connections on your CPMS 
for leakage.
    (7) If your CPMS is not equipped with a redundant pressure sensor, 
perform at least quarterly a visual inspection of all components of the 
CPMS for integrity, oxidation, and galvanic corrosion.
    (d) For each liquid flow rate CPMS that is used to monitor the 
liquid flow rate in a wet scrubber, you must meet the requirements in 
paragraphs (a) and (d)(1) through (7) of this section.
    (1) Use a flow rate CPMS with a minimum accuracy of 5.0 percent or 1.9 liters per minute (L/min) (0.5 
gallons per minute (gal/min)), whichever is greater.
    (2) Use a data recording system with a minimum resolution of one-
half the required CPMS accuracy specified in paragraph (d)(1) of this 
section, or better.
    (3) Perform an initial validation of your CPMS according to the 
requirements in paragraph (3)(i) or (ii) of this section.
    (i) Use a calibrated flow rate measurement system to measure the 
liquid flow rate in a location that is adjacent to the measurement 
location for your flow rate CPMS and is subject to the same environment 
as your flow rate CPMS. The calibrated flow rate measurement device must 
satisfy the accuracy requirements of paragraph (a)(15) of this section. 
While the process and control device that is monitored by your flow rate 
CPMS are operating normally, record concurrently and compare the flow 
rates measured by your flow rate CPMS and the calibrated flow rate 
measurement device. Using the calibrated flow rate measurement device as 
the reference, the flow rate measured by your CPMS must be within the 
accuracy specified in paragraph (d)(1) of this section.
    (ii) Perform any of the initial validation methods for liquid flow 
rate CPMS specified in performance specifications for CPMS established 
in 40 CFR part 60, appendix B.
    (4) Perform an accuracy audit of your flow rate CPMS at least 
quarterly, according to the requirements in paragraph (d)(4)(i), (ii), 
or (iii) of this section.
    (i) If your flow rate CPMS includes a redundant sensor, record three 
pairs of concurrent flow rate measurements within a 24-hour period. Each 
pair of concurrent measurements must consist of a flow rate measurement 
by each of the two flow rate sensors. The minimum time interval between 
any two such pairs of consecutive flow rate measurements is 1 hour. The 
measurements must be taken during periods when the process and control 
device that is monitored by your flow rate CPMS are operating normally. 
Calculate the mean of the three flow rate measurement values for each 
flow rate sensor. The mean values must agree within the required overall 
accuracy of the CPMS, as specified in paragraph (d)(1) of this section.
    (ii) If your flow rate CPMS does not include a redundant flow rate 
sensor, place the sensor of a calibrated flow rate measurement device 
adjacent to the sensor of your flow rate CPMS in a location that is 
subject to the same environment as the sensor of your flow rate CPMS. 
The calibrated flow rate measurement device must satisfy the accuracy 
requirements of paragraph (a)(15) of this section. While the process and 
control device that is monitored by your flow rate CPMS are operating 
normally, record concurrently and compare the flow rate measured by your 
pressure CPMS and the calibrated flow rate measurement device. Using the 
calibrated flow rate measurement device as the reference, the flow rate 
measured by your CPMS must be within the accuracy specified in paragraph 
(d)(1) of this section.

[[Page 96]]

    (iii) Perform any of the accuracy audit methods for liquid flow rate 
CPMS specified in QA procedures for CPMS established in 40 CFR part 60, 
appendix F.
    (5) Conduct an accuracy audit of your flow rate CPMS following any 
24-hour period throughout which the flow rate measured by your CPMS 
exceeds the manufacturer's specified maximum operating range, or install 
a new flow rate sensor.
    (6) At least monthly, check all mechanical connections on your CPMS 
for leakage.
    (7) If your CPMS is not equipped with a redundant flow rate sensor, 
perform at least quarterly a visual inspection of all components of the 
CPMS for integrity, oxidation, and galvanic corrosion.
    (e) For each pH CPMS that is used to monitor the pH of a wet 
scrubber liquid, you must meet the requirements in paragraphs (a) and 
(e)(1) through (5) of this section.
    (1) Use a pH CPMS with a minium accuracy of 0.2 pH units.
    (2) Use a data recording system with a minimum resolution of 0.1 pH 
units, or better.
    (3) Perform an initial validation of your pH CPMS according to the 
requirements in paragraph (e)(3)(i) or (ii) of this section.
    (i) Perform a single-point calibration using an NIST-certified 
buffer solution that is accurate to within 0.02 pH 
units at 25 [deg]C (77 [deg]F). If the expected pH of the liquid that is 
monitored lies in the acidic range (less than 7 pH), use a buffer 
solution with a pH value of 4.00. If the expected pH of the liquid that 
is monitored is neutral or lies in the basic range (equal to or greater 
than 7 pH), use a buffer solution with a pH value of 10.00. Place the 
electrode of your pH CPMS in the container of buffer solution. Record 
the pH measured by your CPMS. Using the certified buffer solution as the 
reference, the pH measured by your CPMS must be within the accuracy 
specified in paragraph (e)(1) of this section.
    (ii) Perform any of the initial validation methods for pH CPMS 
specified in performance specifications for CPMS established in 40 CFR 
part 60, appendix B.
    (4) Perform an accuracy audit of your pH CPMS at least weekly, 
according to the requirements in paragraph (e)(4)(i), (ii), or (iii) of 
this section.
    (i) If your pH CPMS includes a redundant pH sensor, record the pH 
measured by each of the two pH sensors. The measurements must be taken 
during periods when the process and control device that is monitored by 
your pH CPMS are operating normally. The two pH values must agree within 
the required overall accuracy of the CPMS, as specified in paragraph 
(e)(1) of this section.
    (ii) If your pH CPMS does not include a redundant pH sensor, perform 
a single point calibration using an NIST-certified buffer solution that 
is accurate to within 0.02 pH units at 25 [deg]C 
(77 [deg]F). If the expected pH of the liquid that is monitored lies in 
the acidic range (less than 7 pH), use a buffer solution with a pH value 
of 4.00. If the expected pH of the liquid that is monitored is neutral 
or lies in the basic range (equal to or greater than 7 pH), use a buffer 
solution with a pH value of 10.00. Place the electrode of the pH CPMS in 
the container of buffer solution. Record the pH measured by your CPMS. 
Using the certified buffer solution as the reference, the pH measured by 
your CPMS must be within the accuracy specified in paragraph (e)(1) of 
this section.
    (iii) Perform any of the accuracy audit methods for pH CPMS 
specified in QA procedures for CPMS established in 40 CFR part 60, 
appendix F.
    (5) If your CPMS is not equipped with a redundant pH sensor, perform 
at least monthly a visual inspection of all components of the CPMS for 
integrity, oxidation, and galvanic corrosion.
    (f) For each bag leak detection system, you must meet the 
requirements in paragraphs (f)(1) through (11) of this section.
    (1) Each triboelectric bag leak detection system must be installed, 
calibrated, operated, and maintained according to the ``Fabric Filter 
Bag Leak Detection Guidance'' (EPA-454/R-98-015, September 1997). That 
document is available from the U.S. EPA; Office of Air Quality Planning 
and Standards; Emissions, Monitoring and Analysis

[[Page 97]]

Division; Emission Measurement Center (D205-02), Research Triangle Park, 
NC 27711. It is also available on the Technology Transfer Network (TTN) 
at the following address: http://www.epa.gov/ttn/emc/cem.html. Other 
types of bag leak detection systems must be installed, operated, 
calibrated, and maintained in a manner consistent with the 
manufacturer's written specifications and recommendations.
    (2) The bag leak detection system must be certified by the 
manufacturer to be capable of detecting particulate matter (PM) 
emissions at concentrations of 10 milligrams per actual cubic meter 
(0.0044 grains per actual cubic foot) or less.
    (3) The bag leak detection system sensor must provide an output of 
relative PM loadings.
    (4) The bag leak detection system must be equipped with a device to 
continuously record the output signal from the sensor.
    (5) The bag leak detection system must be equipped with an alarm 
system that will be engaged automatically when an increase in relative 
PM emissions over a preset level is detected. The alarm must be located 
where it is easily recognized by plant operating personnel.
    (6) For positive pressure fabric filter systems, a bag leak detector 
must be installed in each baghouse compartment or cell.
    (7) For negative pressure or induced air fabric filters, the bag 
leak detector must be installed downstream of the fabric filter.
    (8) Where multiple detectors are required, the system's 
instrumentation and alarm may be shared among detectors.
    (9) The baseline output must be established by adjusting the range 
and the averaging period of the device and establishing the alarm set 
points and the alarm delay time according to section 5.0 of the ``Fabric 
Filter Bag Leak Detection Guidance.''
    (10) Following initial adjustment of the system, the owner or 
operator must not adjust the sensitivity or range, averaging period, 
alarm set points, or alarm delay time except as detailed in the OM&M 
plan. In no case may the sensitivity be increased by more than 100 
percent or decreased by more than 50 percent over a 365-day period 
unless such adjustment follows a complete fabric filter inspection that 
demonstrates that the fabric filter is in good operating condition. You 
must record each adjustment of your bag leak detection system.
    (11) Record the results of each inspection, calibration, and 
validation check.
    (g) For each lime feed rate measurement device that is used to 
monitor the lime feed rate of a dry injection fabric filter (DIFF) or 
dry lime scrubber/fabric filter (DLS/FF), or the chemical feed rate of a 
wet scrubber, you must meet the requirements in paragraph (a) of this 
section.
    (h) For each affected source that is subject to the emission limit 
specified in item 3, 4, 7, or 8 of Table 1 to this subpart, you must 
satisfy the requirements of paragraphs (h)(1) through (3) of this 
section.
    (1) Install a THC CEMS at the outlet of the control device or in the 
stack of the affected source.
    (2) Meet the requirements of PS-8 of 40 CFR part 60, appendix B.
    (3) Meet the requirements of Procedure 1 of 40 CFR part 60, appendix 
F.
    (i) Requests for approval of alternate monitoring methods must meet 
the requirements in Sec. Sec. 63.9800(i)(2) and 63.8(f).



Sec. 63.9806  How do I demonstrate initial compliance with the emission 
limits, operating limits, and work practice standards?

    (a) You must demonstrate initial compliance with each emission limit 
that applies to you according to the requirements specified in Table 5 
to this subpart.
    (b) You must establish each site-specific operating limit in Table 2 
to this subpart that applies to you according to the requirements 
specified in Sec. 63.9800 and Table 4 to this subpart.
    (c) You must demonstrate initial compliance with each work practice 
standard that applies to you according to the requirements specified in 
Table 6 to this subpart.
    (d) You must submit the Notification of Compliance Status containing 
the results of the initial compliance demonstration according to the 
requirements in Sec. 63.9812(e).

[[Page 98]]

                   Continuous Compliance Requirements



Sec. 63.9808  How do I monitor and collect data to demonstrate continuous 
compliance?

    (a) You must monitor and collect data according to this section.
    (b) At all times, you must maintain your monitoring systems 
including, but not limited to, maintaining necessary parts for routine 
repairs of the monitoring equipment.
    (c) Except for, as applicable, monitoring system malfunctions, 
associated repairs, and required quality assurance or quality control 
activities, you must monitor continuously whenever your affected process 
unit is operating. For purposes of calculating data averages, you must 
not use data recorded during monitoring system malfunctions, associated 
repairs, and required quality assurance or quality control activities. 
You must use all the data collected during all other periods in 
assessing compliance. A monitoring system malfunction is any sudden, 
infrequent, not reasonably preventable failure of the monitoring system 
to provide valid data. Monitoring system malfunctions include out of 
control continuous monitoring systems (CMS), such as a CPMS. Any 
averaging period for which you do not have valid monitoring data as a 
result of a monitoring system malfunction and for which such data are 
required constitutes a deviation, and you must notify the Administrator 
in accordance with Sec. 63.9814(e). Monitoring system failures are 
different from monitoring system malfunctions in that they are caused in 
part by poor maintenance or careless operation. Any period for which 
there is a monitoring system failure and data are not available for 
required calculations constitutes a deviation and you must notify the 
Administrator in accordance with Sec. 63.9814(e).



Sec. 63.9810  How do I demonstrate continuous compliance with the emission 
limits, operating limits, and work practice standards?

    (a) You must demonstrate continuous compliance with each emission 
limit specified in Table 1 to this subpart that applies to you according 
to the requirements specified in Table 7 to this subpart.
    (b) You must demonstrate continuous compliance with each operating 
limit specified in Table 2 to this subpart that applies to you according 
to the requirements specified in Table 8 to this subpart.
    (c) You must demonstrate continuous compliance with each work 
practice standard specified in Table 3 to this subpart that applies to 
you according to the requirements specified in Table 9 to this subpart.
    (d) For each affected source that is equipped with an add-on APCD 
that is not addressed in Table 2 to this subpart or that is using 
process changes as a means of meeting the emission limits in Table 1 to 
this subpart, you must demonstrate continuous compliance with each 
emission limit in Table 1 to this subpart and each operating limit 
established as required in Sec. 63.9800(i)(3) according to the methods 
specified in your approved alternative monitoring methods request as 
described in Sec. 63.9800(i)(2).
    (e) You must report each instance in which you did not meet each 
emission limit and each operating limit in this subpart that applies to 
you. This includes periods of startup, shutdown, and malfunction. These 
instances are deviations from the emission limitations in this subpart. 
These deviations must be reported according to the requirements in Sec. 
63.9814.
    (1) During periods of startup, shutdown, and malfunction, you must 
operate according to your SSMP.
    (2) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations 
that occur during a period of startup, shutdown, or malfunction are not 
violations if you demonstrate to the Administrator's satisfaction that 
you were operating according to your SSMP and your OM&M plan. The 
Administrator will determine whether deviations that occur during a 
period of startup, shutdown, or malfunction are violations, according to 
the provisions in Sec. 63.6(e).

                   Notifications, Reports, and Records



Sec. 63.9812  What notifications must I submit and when?

    (a) You must submit all of the notifications in Sec. Sec. 63.7(b) 
and (c), 63.8(f)(4),

[[Page 99]]

and 63.9 (b) through (e) and (h) that apply to you by the dates 
specified.
    (b) As specified in Sec. 63.9(b)(2) and (3), if you start up your 
affected source before April 16, 2003, you must submit an Initial 
Notification not later than 120 calendar days after April 16, 2003.
    (c) As specified in Sec. 63.9(b)(3), if you start up your new or 
reconstructed affected source on or after April 16, 2003, you must 
submit an Initial Notification not later than 120 calendar days after 
you become subject to this subpart.
    (d) If you are required to conduct a performance test, you must 
submit a Notification of Performance Test at least 60 calendar days 
before the performance test is scheduled to begin, as required in Sec. 
63.7(b)(1).
    (e) If you are required to conduct a performance test, you must 
submit a Notification of Compliance Status as specified in Sec. 63.9(h) 
and paragraphs (e)(1) and (2) of this section.
    (1) For each compliance demonstration that includes a performance 
test conducted according to the requirements in Table 4 to this subpart, 
you must submit the Notification of Compliance Status, including the 
performance test results, before the close of business on the 60th 
calendar day following the completion of the performance test, according 
to Sec. 63.10(d)(2).
    (2) In addition to the requirements in Sec. 63.9(h)(2)(i), you must 
include the information in paragraphs (e)(2)(i) through (iv) of this 
section in your Notification of Compliance Status.
    (i) The operating limit parameter values established for each 
affected source with supporting documentation and a description of the 
procedure used to establish the values.
    (ii) Design information and analysis with supporting documentation 
demonstrating conformance with requirements for capture/collection 
systems in Table 2 to this subpart.
    (iii) A description of the methods used to comply with any 
applicable work practice standard.
    (iv) For each APCD that includes a fabric filter, analysis and 
supporting documentation demonstrating conformance with EPA guidance and 
specifications for bag leak detection systems in Sec. 63.9804(f).
    (f) If you operate a clay refractory products kiln or a chromium 
refractory products kiln that is subject to the work practice standard 
specified in item 3 or 4 of Table 3 to this subpart, and you intend to 
use a fuel other than natural gas or equivalent to fire the affected 
kiln, you must submit a notification of alternative fuel use within 48 
hours of the declaration of a period of natural gas curtailment or 
supply interruption, as defined in Sec. 63.9824. The notification must 
include the information specified in paragraphs (f)(1) through (5) of 
this section.
    (1) Company name and address.
    (2) Identification of the affected kiln.
    (3) Reason you are unable to use natural gas or equivalent fuel, 
including the date when the natural gas curtailment was declared or the 
natural gas supply interruption began.
    (4) Type of alternative fuel that you intend to use.
    (5) Dates when the alternative fuel use is expected to begin and 
end.
    (g) If you own or operate an affected continuous kiln and must 
perform scheduled maintenance on the control device for that kiln, you 
must request approval from the Administrator before bypassing the 
control device, as specified in Sec. 63.9792(e). You must submit a 
separate request for approval each time you plan to bypass the kiln 
control device.



Sec. 63.9814  What reports must I submit and when?

    (a) You must submit each report in Table 10 to this subpart that 
applies to you.
    (b) Unless the Administrator has approved a different schedule for 
submission of reports under Sec. 63.10(a), you must submit each report 
by the date in Table 10 to this subpart and as specified in paragraphs 
(b)(1) through (5) of this section.
    (1) The first compliance report must cover the period beginning on 
the compliance date that is specified for your affected source in Sec. 
63.9786 and ending on June 30 or December 31 and lasting at least 6 
months but less than 12 months. For example, if your compliance date is 
March 1, then the first semiannual reporting period would

[[Page 100]]

begin on March 1 and end on December 31.
    (2) The first compliance report must be postmarked or delivered no 
later than July 31 or January 31 for compliance periods ending on June 
30 and December 31, respectively.
    (3) Each subsequent compliance report must cover the semiannual 
reporting period from January 1 through June 30 or the semiannual 
reporting period from July 1 through December 31.
    (4) Each subsequent compliance report must be postmarked or 
delivered no later than July 31 or January 31 for compliance periods 
ending on June 30 and December 31, respectively.
    (5) For each affected source that is subject to permitting 
regulations pursuant to 40 CFR part 70 or 40 CFR part 71 and, if the 
permitting authority has established dates for submitting semiannual 
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance 
reports according to the dates the permitting authority has established 
instead of according to the dates in paragraphs (b)(1) through (4) of 
this section. In such cases, you must notify the Administrator of this 
change.
    (c) The compliance report must contain the information in paragraphs 
(c)(1) through (6) of this section.
    (1) Company name and address.
    (2) Statement by a responsible official with that official's name, 
title, and signature, certifying that, based on information and belief 
formed after reasonable inquiry, the statements and information in the 
report are true, accurate, and complete.
    (3) Date of report and beginning and ending dates of the reporting 
period.
    (4) If you had a startup, shutdown, or malfunction during the 
reporting period, and you took actions consistent with your SSMP and 
OM&M plan, the compliance report must include the information specified 
in Sec. 63.10(d)(5)(i).
    (5) If there are no deviations from any emission limitations 
(emission limit, operating limit, or work practice standard) that apply 
to you, the compliance report must include a statement that there were 
no deviations from the emission limitations during the reporting period.
    (6) If there were no periods during which any affected CPMS was out 
of control as specified in Sec. 63.8(c)(7), the compliance report must 
include a statement that there were no periods during which the CPMS was 
out of control during the reporting period.
    (d) For each deviation from an emission limitation (emission limit, 
operating limit, or work practice standard) that occurs at an affected 
source where you are not using a CPMS to comply with the emission 
limitations in this subpart, the compliance report must contain the 
information in paragraphs (c)(1) through (4) and (d)(1) and (2) of this 
section. This includes periods of startup, shutdown, and malfunction.
    (1) The compliance report must include the total operating time of 
each affected source during the reporting period.
    (2) The compliance report must include information on the number, 
duration, and cause of deviations (including unknown cause, if 
applicable) and the corrective action taken.
    (e) For each deviation from an emission limitation (emission limit, 
operating limit, or work practice standard) occurring at an affected 
source where you are using a CPMS to comply with the emission limitation 
in this subpart, the compliance report must include the information in 
paragraphs (c)(1) through (4) and (e)(1) through (13) of this section. 
This includes periods of startup, shutdown, and malfunction.
    (1) The total operating time of each affected source during the 
reporting period.
    (2) The date and time that each startup, shutdown, or malfunction 
started and stopped.
    (3) The date, time, and duration that each CPMS was inoperative.
    (4) The date, time and duration that each CPMS was out of control, 
including the information in Sec. 63.8(c)(8), as required by your OM&M 
plan.
    (5) The date and time that each deviation from an emission 
limitation (emission limit, operating limit, or work practice standard) 
started and stopped, and whether each deviation occurred during a period 
of startup, shutdown, or malfunction.

[[Page 101]]

    (6) A description of corrective action taken in response to a 
deviation.
    (7) A summary of the total duration of the deviations during the 
reporting period and the total duration as a percentage of the total 
source operating time during that reporting period.
    (8) A breakdown of the total duration of the deviations during the 
reporting period into those that are due to startup, shutdown, control 
equipment problems, process problems, other known causes, and other 
unknown causes.
    (9) A summary of the total duration of CPMS downtime during the 
reporting period and the total duration of CPMS downtime as a percentage 
of the total source operating time during that reporting period.
    (10) A brief description of the process units.
    (11) A brief description of the CPMS.
    (12) The date of the latest CPMS initial validation or accuracy 
audit.
    (13) A description of any changes in CPMS, processes, or controls 
since the last reporting period.
    (f) If you have obtained a title V operating permit pursuant to 40 
CFR part 70 or 40 CFR part 71, you must report all deviations as defined 
in this subpart in the semiannual monitoring report required by 40 CFR 
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A). If you submit a 
compliance report according to Table 10 to this subpart along with, or 
as part of, the semiannual monitoring report required by 40 CFR 
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A), and the compliance 
report includes all required information concerning deviations from any 
emission limitation (including any operating limit), then submitting the 
compliance report will satisfy any obligation to report the same 
deviations in the semiannual monitoring report. However, submitting a 
compliance report will not otherwise affect any obligation you may have 
to report deviations from permit requirements to the permit authority.
    (g) If you operate a clay refractory products kiln or a chromium 
refractory products kiln that is subject to the work practice standard 
specified in item 3 or 4 of Table 3 to this subpart, and you use a fuel 
other than natural gas or equivalent to fire the affected kiln, you must 
submit a report of alternative fuel use within 10 working days after 
terminating the use of the alternative fuel. The report must include the 
information in paragraphs (g)(1) through (6) of this section.
    (1) Company name and address.
    (2) Identification of the affected kiln.
    (3) Reason for using the alternative fuel.
    (4) Type of alternative fuel used to fire the affected kiln.
    (5) Dates that the use of the alternative fuel started and ended.
    (6) Amount of alternative fuel used.



Sec. 63.9816  What records must I keep?

    (a) You must keep the records listed in paragraphs (a)(1) through 
(3) of this section.
    (1) A copy of each notification and report that you submitted to 
comply with this subpart, including all documentation supporting any 
Initial Notification or Notification of Compliance Status that you 
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
    (2) The records in Sec. 63.6(e)(3)(iii) through (v) related to 
startup, shutdown, and malfunction.
    (3) Records of performance tests as required in Sec. 
63.10(b)(2)(viii).
    (b) You must keep the records required in Tables 7 through 9 to this 
subpart to show continuous compliance with each emission limitation that 
applies to you.
    (c) You must also maintain the records listed in paragraphs (c)(1) 
through (10) of this section.
    (1) Records of emission data used to develop an emissions profile, 
as indicated in items 8(a)(i)(4) and 17(b)(i)(4) of Table 4 to this 
subpart.
    (2) Records that document how you comply with any applicable work 
practice standard.
    (3) For each bag leak detection system, records of each alarm, the 
time of the alarm, the time corrective action was initiated and 
completed, and a brief description of the cause of the alarm and the 
corrective action taken.
    (4) For each kiln controlled with a DLA, records that document the 
source of limestone used.
    (5) For each deviation of an operating limit parameter value, the 
date, time, and duration of the deviation, a brief

[[Page 102]]

explanation of the cause of the deviation and the corrective action 
taken, and whether the deviation occurred during a period of startup, 
shutdown, or malfunction.
    (6) For each affected source, records of production rate on a 
process throughput basis (either feed rate to the process unit or 
discharge rate from the process unit).
    (7) Records of any approved alternative monitoring method(s) or test 
procedure(s).
    (8) Records of maintenance activities and inspections performed on 
control devices, including all records associated with the scheduled 
maintenance of continuous kiln control devices, as specified in Sec. 
63.9792(e).
    (9) If you operate a source that is subject to the THC emission 
limits specified in item 2, 3, 6, or 7 of Table 1 to this subpart and is 
controlled with a catalytic oxidizer, records of annual checks of 
catalyst activity levels and subsequent corrective actions.
    (10) Current copies of the SSMP and the OM&M plan, including any 
revisions and records documenting conformance with those revisions.



Sec. 63.9818  In what form and how long must I keep my records?

    (a) Your records must be in a form suitable and readily available 
for expeditious review, according to Sec. 63.10(b)(1).
    (b) As specified in Sec. 63.10(b)(1), you must keep each record for 
5 years following the date of each occurrence, measurement, maintenance, 
corrective action, report, or record.
    (c) You must keep each record onsite for at least 2 years after the 
date of each occurrence, measurement, maintenance, corrective action, 
report, or record, according to Sec. 63.10(b)(1). You may keep the 
records offsite for the remaining 3 years.

                   Other Requirements and Information



Sec. 63.9820  What parts of the General Provisions apply to me?

    Table 11 to this subpart shows which parts of the General Provisions 
specified in Sec. Sec. 63.1 through 63.15 apply to you.



Sec. 63.9822  Who implements and enforces this subpart?

    (a) This subpart can be implemented and enforced by us, the U.S. 
Environmental Protection Agency (U.S. EPA), or a delegated authority 
such as your State, local, or tribal agency. If the U.S. EPA 
Administrator has delegated authority to your State, local, or tribal 
agency, then that agency, in addition to the U.S. EPA, has the authority 
to implement and enforce this subpart. You should contact your U.S. EPA 
Regional Office to find out if implementation and enforcement to this 
subpart is delegated to your State, local, or tribal agency.
    (b) In delegating implementation and enforcement authority to this 
subpart to a State, local, or tribal agency under 40 CFR part 63, 
subpart E, the authorities contained in paragraph (c) of this section 
are retained by the Administrator of the U.S. EPA and are not 
transferred to the State, local, or tribal agency.
    (c) The authorities that cannot be delegated to State, local, or 
tribal agencies are as specified in paragraphs (c)(1) through (4) of 
this section.
    (1) Approval of alternatives to the applicability requirements in 
Sec. Sec. 63.9782 and 63.9784, the compliance date requirements in 
Sec. 63.9786, and the emission limitations in Sec. 63.9788.
    (2) Approval of major changes to test methods under Sec. 
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
    (3) Approval of major changes to monitoring under Sec. 63.8(f) and 
as defined in Sec. 63.90.
    (4) Approval of major changes to recordkeeping and reporting under 
Sec. 63.10(f) and as defined in Sec. 63.90.



Sec. 63.9824  What definitions apply to this subpart?

    Terms used in this subpart are defined in the Clean Air Act, in 40 
CFR 63.2, the General Provisions of this part, and in this section as 
follows:
    Additive means a minor addition of a chemical, mineral, or metallic 
substance that is added to a refractory mixture to facilitate processing 
or impart specific properties to the final refractory product.
    Add-on air pollution control device (APCD) means equipment installed 
on

[[Page 103]]

a process vent that reduces the quantity of a pollutant that is emitted 
to the air.
    Autoclave means a vessel that is used to impregnate fired and/or 
unfired refractory shapes with pitch to form pitch-impregnated 
refractory products. Autoclaves also can be used as defumers following 
the impregnation process.
    Bag leak detection system means an instrument that is capable of 
monitoring particulate matter loadings in the exhaust of a fabric filter 
in order to detect bag failures. A bag leak detection system includes, 
but is not limited to, an instrument that operates on triboelectric, 
light-scattering, light-transmittance, or other effects to monitor 
relative PM loadings.
    Basket means the metal container used to hold refractory shapes for 
pitch impregnation during the shape preheating, impregnation, defuming, 
and, if applicable, coking processes.
    Batch process means a process in which a set of refractory shapes is 
acted upon as a single unit according to a predetermined schedule, 
during which none of the refractory shapes being processed are added or 
removed. A batch process does not operate continuously.
    Binder means a substance added to a granular material to give it 
workability and green or dry strength.
    Catalytic oxidizer means an add-on air pollution control device that 
is designed specifically to destroy organic compounds in a process 
exhaust gas stream by catalytic incineration. A catalytic oxidizer 
includes a bed of catalyst media through which the process exhaust 
stream passes to promote combustion and incineration at a lower 
temperature than would be possible without the catalyst.
    Chromium refractory product means a refractory product that contains 
at least 1 percent chromium by weight.
    Clay refractory product means a refractory product that contains at 
least 10 percent uncalcined clay by weight prior to firing in a kiln. In 
this definition, the term ``clay'' means any of the following six 
classifications of clay defined by the U.S. Geologic Survey: ball clay, 
bentonite, common clay and shale, fire clay, fuller's earth, and kaolin.
    Coking oven means a thermal process unit that operates at a peak 
temperature typically between 540[deg] and 870 [deg]C (1000[deg] and 
1600 [deg]F) and is used to drive off the volatile constituents of 
pitch-impregnated refractory shapes under a reducing or oxygen-deprived 
atmosphere.
    Continuous parameter monitoring system (CPMS) means the total 
equipment that is used to measure and record temperature, pressure, 
liquid flow rate, gas flow rate, or pH on a continuous basis in one or 
more locations. ``Total equipment'' includes the sensor, mechanical 
components, electronic components, data acquisition system, data 
recording system, electrical wiring, and other components of a CPMS.
    Continuous process means a process that operates continuously. In a 
continuous process unit, the materials or shapes that are processed are 
either continuously charged (fed) to and discharged from the process 
unit, or are charged and discharged at regular time intervals without 
the process unit being shut down. Continuous thermal process units, such 
as tunnel kilns, generally include temperature zones that are maintained 
at relatively constant temperature and through which the materials or 
shapes being processed are conveyed continuously or at regular time 
intervals.
    Curing oven means a thermal process unit that operates at a peak 
temperature typically between 90[deg] and 340 [deg]C (200[deg] and 650 
[deg]F) and is used to activate a thermosetting resin, pitch, or other 
binder in refractory shapes. Curing ovens also perform the same function 
as shape dryers in removing the free moisture from refractory shapes.
    Defumer means a process unit that is used for holding pitch-
impregnated refractory shapes as the shapes defume or cool immediately 
following the impregnation process. This definition includes autoclaves 
that are opened and exhausted to the atmosphere following an 
impregnation cycle and used for holding pitch-impregnated refractory 
shapes while the shapes defume or cool.
    Deviation means any instance in which an affected source subject to 
this

[[Page 104]]

subpart, or an owner or operator of such a source:
    (1) Fails to meet any requirement or obligation established by this 
subpart including, but not limited to, any emission limitation (emission 
limit, operating limit, or work practice standard);
    (2) Fails to meet any term or condition that is adopted to implement 
an applicable requirement in this subpart for any affected source 
required to obtain such a permit; or
    (3) Fails to meet any emission limitation (emission limit, operating 
limit, or work practice standard) in this subpart during startup, 
shutdown, or malfunction, regardless of whether or not such failure is 
permitted by this subpart.
    Dry injection fabric filter (DIFF) means an add-on air pollution 
control device that includes continuous injection of hydrated lime or 
other sorbent into a duct or reaction chamber followed by a fabric 
filter.
    Dry lime scrubber/fabric filter (DLS/FF) means an add-on air 
pollution control device that includes continuous injection of 
humidified hydrated lime or other sorbent into a reaction chamber 
followed by a fabric filter. These systems may include recirculation of 
some of the sorbent.
    Dry limestone adsorber (DLA) means an air pollution control device 
that includes a limestone storage bin, a reaction chamber that is 
essentially a packed-tower filled with limestone, and may or may not 
include a peeling drum that mechanically scrapes reacted limestone to 
regenerate the stone for reuse.
    Emission limitation means any restriction on the emissions a process 
unit may discharge.
    Fabric filter means an add-on air pollution control device used to 
capture particulate matter by filtering a process exhaust stream through 
a filter or filter media; a fabric filter is also known as a baghouse.
    Fired refractory shape means a refractory shape that has been fired 
in a kiln.
    HAP means any hazardous air pollutant that appears in section 112(b) 
of the Clean Air Act.
    Kiln means a thermal process unit that operates at a peak 
temperature greater than 820 [deg]C (1500 [deg]F) and is used for firing 
or sintering refractory, ceramic, or other shapes.
    Kiln furniture means any refractory shape that is used to hold, 
support, or position ceramic or refractory products in a kiln during the 
firing process.
    Maximum organic HAP processing rate means the combination of process 
and refractory product formulation that has the greatest potential to 
emit organic HAP. The maximum organic HAP processing rate is a function 
of the organic HAP processing rate, process operating temperature, and 
other process operating parameters that affect emissions of organic HAP. 
(See also the definition of organic HAP processing rate.)
    Organic HAP processing rate means the rate at which the mass of 
organic HAP materials contained in refractory shapes are processed in an 
affected thermal process unit. The organic HAP processing rate is a 
function of the amount of organic HAP contained in the resins, binders, 
and additives used in a refractory mix; the amounts of those resins, 
binders, and additives in the refractory mix; and the rate at which the 
refractory shapes formed from the refractory mix are processed in an 
affected thermal process unit. For continuous process units, the organic 
HAP processing rate is expressed in units of mass of organic HAP per 
unit of time (e.g., pounds per hour). For batch process units, the 
organic HAP processing rate is expressed in units of mass of organic HAP 
per unit mass of refractory shapes processed during the batch process 
cycle (e.g., pounds per ton).
    Particulate matter (PM) means, for the purposes of this subpart, 
emissions of particulate matter that serve as a measure of total 
particulate emissions as measured by EPA Method 5 of 40 CFR part 60, 
appendix A.
    Peak emissions period means the period of consecutive hourly mass 
emissions of the applicable pollutant that is greater than any other 
period of consecutive hourly mass emissions for the same pollutant over 
the course of a specified batch process cycle, as defined in paragraphs 
(1) and (2) of this definition. The peak emissions period is a function 
of the rate at which the

[[Page 105]]

temperature of the refractory shapes is increased, the mass and loading 
configuration of the shapes in the process unit, the constituents of the 
refractory mix, and the type of pollutants emitted.
    (1) The 3-hour peak THC emissions period is the period of 3 
consecutive hours over which the sum of the hourly THC mass emissions 
rates is greater than the sum of the hourly THC mass emissions rates for 
any other period of 3 consecutive hours during the same batch process 
cycle.
    (2) The 3-hour peak HF emissions period is the period of 3 
consecutive hours over which the sum of the hourly HF mass emissions 
rates is greater than the sum of the hourly HF mass emissions rates for 
any other period of 3 consecutive hours during the same batch process 
cycle.
    Period of natural gas curtailment or supply interruption means a 
period of time during which the supply of natural gas to an affected 
facility is halted for reasons beyond the control of the facility. An 
increase in the cost or unit price of natural gas does not constitute a 
period of natural gas curtailment or supply interruption.
    Pitch means the residue from the distillation of petroleum or coal 
tar.
    Pitch-bonded refractory product means a formed refractory product 
that is manufactured using pitch as a bonding agent. Pitch-bonded 
refractory products are manufactured by mixing pitch with magnesium 
oxide, graphite, alumina, silicon carbide, silica, or other refractory 
raw materials, and forming the mix into shapes. After forming, pitch-
bonded refractory products are cured in a curing oven and may be 
subsequently fired in a kiln.
    Pitch-impregnated refractory product means a refractory shape that 
has been fired in a kiln, then impregnated with heated coal tar or 
petroleum pitch under pressure. After impregnation, pitch-impregnated 
refractory shapes may undergo the coking process in a coking oven. The 
total carbon content of a pitch-impregnated refractory product is less 
than 50 percent.
    Pitch working tank means a tank that is used for heating pitch to 
the impregnation temperature, typically between 150[deg] and 260 [deg]C 
(300[deg] and 500 [deg]F); temporarily storing heated pitch between 
impregnation cycles; and transferring pitch to and from the autoclave 
during the impregnation step in manufacturing pitch-impregnated 
refractory products.
    Plant site means all contiguous or adjoining property that is under 
common control, including properties that are separated only by a road 
or other public right-of-way. Common control includes properties that 
are owned, leased, or operated by the same entity, parent entity, 
subsidiary, or any combination thereof.
    Redundant sensor means a second sensor or a back-up sensor that is 
integrated into a CPMS and is used to check the parameter value (e.g., 
temperature, pressure) measured by the primary sensor of the CPMS.
    Refractory product means nonmetallic materials containing less than 
50 percent carbon by weight and having those chemical and physical 
properties that make them applicable for structures, or as components of 
systems, that are exposed to environments above 538 [deg]C (1000 
[deg]F). This definition includes, but is not limited to: refractory 
bricks, kiln furniture, crucibles, refractory ceramic fiber, and other 
materials used as linings for boilers, kilns, and other processing units 
and equipment where extremes of temperature, corrosion, and abrasion 
would destroy other materials.
    Refractory products that use organic HAP means resin-bonded 
refractory products, pitch-bonded refractory products, and other 
refractory products that are produced using a substance that is an 
organic HAP, that releases an organic HAP during production of the 
refractory product, or that contains an organic HAP, such as methanol or 
ethylene glycol.
    Refractory shape means any refractory piece forming a stable mass 
with specific dimensions.
    Research and development process unit means any process unit whose 
purpose is to conduct research and development for new processes and 
products and is not engaged in the manufacture of products for 
commercial sale, except in a de minimis manner.
    Resin-bonded refractory product means a formed refractory product 
that is

[[Page 106]]

manufactured using a phenolic resin or other type of thermosetting resin 
as a bonding agent. Resin-bonded refractory products are manufactured by 
mixing resin with alumina, magnesium oxide, graphite, silica, zirconia, 
or other refractory raw materials, and forming the mix into shapes. 
After forming, resin-bonded refractory products are cured in a curing 
oven and may be subsequently fired in a kiln.
    Responsible official means one of the following:
    (1) For a corporation: a president, secretary, treasurer, or vice-
president of the corporation in charge of a principal business function, 
or any other person who performs similar policy or decisionmaking 
functions for the corporation, or a duly authorized representative of 
such person if the representative is responsible for the overall 
operation of one or more manufacturing, production, or operating 
facilities applying for or subject to a permit and either:
    (i) The facilities employ more than 250 persons or have gross annual 
sales or expenditures exceeding $25 million (in second quarter 1980 
dollars); or
    (ii) The delegation of authority to such representatives is approved 
in advance by the Administrator;
    (2) For a partnership or sole proprietorship: a general partner or 
the proprietor, respectively;
    (3) For a municipality, State, Federal, or other public agency: 
either a principal executive officer or ranking elected official. For 
the purposes of this part, a principal executive officer of a Federal 
agency includes the chief executive officer having responsibility for 
the overall operations of a principal geographic unit of the agency 
(e.g., a Regional Administrator of EPA); or
    (4) For affected sources (as defined in this subpart) applying for 
or subject to a title V permit: ``responsible official'' shall have the 
same meaning as defined in part 70 or Federal title V regulations in 
this chapter (42 U.S.C. 7661), whichever is applicable.
    Shape dryer means a thermal process unit that operates at a peak 
temperature typically between 40[deg] and 700 [deg]C (100[deg] and 1300 
[deg]F) and is used exclusively to reduce the free moisture content of a 
refractory shape. Shape dryers generally are the initial thermal process 
step following the forming step in refractory products manufacturing. 
(See also the definition of a curing oven.)
    Shape preheater means a thermal process unit that operates at a peak 
temperature typically between 180[deg] and 320 [deg]C (350[deg] and 600 
[deg]F) and is used to heat fired refractory shapes prior to the 
impregnation step in manufacturing pitch-impregnated refractory 
products.
    Thermal oxidizer means an add-on air pollution control device that 
includes one or more combustion chambers and is designed specifically to 
destroy organic compounds in a process exhaust gas stream by 
incineration.
    Uncalcined clay means clay that has not undergone thermal processing 
in a calciner.
    Wet scrubber means an add-on air pollution control device that 
removes pollutants from a gas stream by bringing them into contact with 
a liquid, typically water.
    Work practice standard means any design, equipment, work practice, 
or operational standard, or combination thereof, that is promulgated 
pursuant to section 112(h) of the Clean Air Act.

          Table 1 to Subpart SSSSS of Part 63--Emission Limits

    As stated in Sec. 63.9788, you must comply with the emission limits 
for affected sources in the following table:

[[Page 107]]



------------------------------------------------------------------------
 
 
------------------------------------------------------------------------
1. Each new or existing curing oven,     As specified in items 2 through
 shape dryer, and kiln that is used to    9 of this table.
 process refractory products that use
 organic HAP; each new or existing
 coking oven and defumer that is used
 to produce pitch-impregnated
 refractory products; each new shape
 preheater that is used to produce
 pitch-impregnated refractory products;
 AND each new or existing process unit
 that is exhausted to a thermal or
 catalytic oxidizer that also controls
 emissions from an affected shape
 preheater or pitch working tank.
2. Continuous process units that are     a. The 3-hour block average THC
 controlled with a thermal or catalytic   concentration must not exceed
 oxidizer.                                20 parts per million by
                                          volume, dry basis (ppmvd),
                                          corrected to 18 percent
                                          oxygen, at the outlet of the
                                          control device; or
                                         b. The 3-hour block average THC
                                          mass emissions rate must be
                                          reduced by at least 95
                                          percent.
3. Continuous process units that are     a. The 3-hour block average THC
 equipped with a control device other     concentration must not exceed
 than a thermal or catalytic oxidizer.    20 ppmvd, corrected to 18
                                          percent oxygen, at the outlet
                                          of the control device; or
                                         b. The 3-hour block average THC
                                          mass emissions rate must be
                                          reduced by at least 95
                                          percent.
4. Continuous process units that use     The 3-hour block average THC
 process changes to reduce organic HAP    concentration must not exceed
 emissions.                               20 ppmvd, corrected to 18
                                          percent oxygen, at the outlet
                                          of the process gas stream.
5. Continuous kilns that are not         The 3-hour block average THC
 equipped with a control device.          concentration must not exceed
                                          20 ppmvd, corrected to 18
                                          percent oxygen, at the outlet
                                          of the process gas stream.
6. Batch process units that are          a. The 2-run block average THC
 controlled with a thermal or catalytic   concentration for the 3-hour
 oxidizer.                                peak emissions period must not
                                          exceed 20 ppmvd, corrected to
                                          18 percent oxygen, at the
                                          outlet of the control device;
                                          or
                                         b. The 2-run block average THC
                                          mass emissions rate for the 3-
                                          hour peak emissions period
                                          must be reduced by at least 95
                                          percent.
7. Batch process units that are          a. The 2-run block average THC
 equipped with a control device other     concentration for the 3-hour
 than a thermal or catalytic oxidizer.    peak emissions period must not
                                          exceed 20 ppmvd, corrected to
                                          18 percent oxygen, at the
                                          outlet of the control device;
                                          or
                                         b. The 2-run block average THC
                                          mass emissions rate for the 3-
                                          hour peak emissions period
                                          must be reduced by at least 95
                                          percent.
8. Batch process units that use process  The 2-run block average THC
 changes to reduce organic HAP            concentration for the 3-hour
 emissions.                               peak emissions period must not
                                          exceed 20 ppmvd, corrected to
                                          18 percent oxygen, at the
                                          outlet of the process gas
                                          stream.
9. Batch process kilns that are not      The 2-run block average THC
 equipped with a control device.          concentration for the 3-hour
                                          peak emissions period must not
                                          exceed 20 ppmvd, corrected to
                                          18 percent oxygen, at the
                                          outlet of the process gas
                                          stream.
10. Each new continuous kiln that is     a. The 3-hour block average HF
 used to produce clay refractory          emissions must not exceed
 products.                                0.019 kilograms per megagram
                                          (kg/Mg) (0.038 pounds per ton
                                          (lb/ton)) of uncalcined clay
                                          processed, OR the 3-hour block
                                          average HF mass emissions rate
                                          must be reduced by at least 90
                                          percent; and
                                         b. The 3-hour block average HCl
                                          emissions must not exceed
                                          0.091 kg/Mg (0.18 lb/ton) of
                                          uncalcined clay processed, OR
                                          the 3-hour block average HCl
                                          mass emissions rate must be
                                          reduced by at least 30
                                          percent.
11. Each new batch process kiln that is  a. The 2-run block average HF
 used to produce clay refractory          mass emissions rate for the 3-
 products.                                hour peak emissions period
                                          must be reduced by at least 90
                                          percent; and
                                         b. The 2-run block average HCl
                                          mass emissions rate for the 3-
                                          hour peak emissions period
                                          must be reduced by at least 30
                                          percent.
------------------------------------------------------------------------

          Table 2 to Subpart SSSSS of Part 63--Operating Limits

    [As stated in Sec. 63.9788, you must comply with the operating 
limits for affected sources in the following table:]

------------------------------------------------------------------------
 
------------------------------------------------------------------------
1. Each affected source listed in Table  a. Operate all affected sources
 1 to this subpart.                       according to the requirements
                                          to this subpart on and after
                                          the date on which the initial
                                          performance test is conducted
                                          or required to be conducted,
                                          whichever date is earlier; and

[[Page 108]]

 
                                         b. Capture emissions and vent
                                          them through a closed system;
                                          and
                                         c. Operate each control device
                                          that is required to comply
                                          with this subpart on each
                                          affected source during all
                                          periods that the source is
                                          operating, except where
                                          specified in Sec.
                                          63.9792(e), item 2 of this
                                          table, and item 13 of Table 4
                                          to this subpart; and
                                         d. Record all operating
                                          parameters specified in Table
                                          8 to this subpart for the
                                          affected source; and
                                         e. Prepare and implement a
                                          written OM&M plan as specified
                                          in Sec. 63.9792(d).
2. Each affected continuous kiln that    a. Receive approval from the
 is equipped with an emission control     Administrator before taking
 device.                                  the control device on the
                                          affected kiln out of service
                                          for scheduled maintenance, as
                                          specified in Sec.
                                          63.9792(e); and
                                         b. Minimize HAP emissions from
                                          the affected kiln during all
                                          periods of scheduled
                                          maintenance of the kiln
                                          control device when the kiln
                                          is operating and the control
                                          device is out of service; and
                                         c. Minimize the duration of all
                                          periods of scheduled
                                          maintenance of the kiln
                                          control device when the kiln
                                          is operating and the control
                                          device is out of service.
3. Each new or existing curing oven,     Satisfy the applicable
 shape dryer, and kiln that is used to    operating limits specified in
 process refractory products that use     items 4 through 9 of this
 organic HAP; each new or existing        table.
 coking oven and defumer that is used
 to produce pitch-impregnated
 refractory products; each new shape
 preheater that is used to produce
 pitch-impregnated refractory products;
 AND each new or existing process unit
 that is exhausted to a thermal or
 catalytic oxidizer that also controls
 emissions from an affected shape
 preheater or pitch working tank.
4. Each affected continuous process      Maintain the 3-hour block
 unit.                                    average organic HAP processing
                                          rate (pounds per hour) at or
                                          below the maximum organic HAP
                                          processing rate established
                                          during the most recent
                                          performance test.
5. Continuous process units that are     Maintain the 3-hour block
 equipped with a thermal oxidizer.        average operating temperature
                                          in the thermal oxidizer
                                          combustion chamber at or above
                                          the minimum allowable
                                          operating temperature for the
                                          oxidizer established during
                                          the most recent performance
                                          test.
6. Continuous process units that are     a. Maintain the 3-hour block
 equipped with a catalytic oxidizer.      average operating temperature
                                          at the inlet of the catalyst
                                          bed of the oxidizer at or
                                          above the minimum allowable
                                          operating temperature for the
                                          oxidizer established during
                                          the most recent performance
                                          test; and
                                         b. Check the activity level of
                                          the catalyst at least every 12
                                          months.
7. Each affected batch process unit....  For each batch cycle, maintain
                                          the organic HAP processing
                                          rate (pounds per batch) at or
                                          below the maximum organic HAP
                                          processing rate established
                                          during the most recent
                                          performance test.
8. Batch process units that are          a. From the start of each batch
 equipped with a thermal oxidizer.        cycle until 3 hours have
                                          passed since the process unit
                                          reached maximum temperature,
                                          maintain the hourly average
                                          operating temperature in the
                                          thermal oxidizer combustion
                                          chamber at or above the
                                          minimum allowable operating
                                          temperature established for
                                          the corresponding period
                                          during the most recent
                                          performance test, as
                                          determined according to item
                                          11 of Table 4 to this subpart;
                                          and
                                         b. For each subsequent hour of
                                          the batch cycle, maintain the
                                          hourly average operating
                                          temperature in the thermal
                                          oxidizer combustion chamber at
                                          or above the minimum allowable
                                          operating temperature
                                          established for the
                                          corresponding hour during the
                                          most recent performance test,
                                          as specified in item 13 of
                                          Table 4 to this subpart.
9. Batch process units that are          a. From the start of each batch
 equipped with a catalytic oxidizer.      cycle until 3 hours have
                                          passed since the process unit
                                          reached maximum temperature,
                                          maintain the hourly average
                                          operating temperature at the
                                          inlet of the catalyst bed at
                                          or above the minimum allowable
                                          operating temperature
                                          established for the
                                          corresponding period during
                                          the most recent performance
                                          test, as determined according
                                          to item 12 of Table 4 to this
                                          subpart; and

[[Page 109]]

 
                                         b. For each subsequent hour of
                                          the batch cycle, maintain the
                                          hourly average operating
                                          temperature at the inlet of
                                          the catalyst bed at or above
                                          the minimum allowable
                                          operating temperature
                                          established for the
                                          corresponding hour during the
                                          most recent performance test,
                                          as specified in item 13 of
                                          Table 4 to this subpart; and
                                         c. Check the activity level of
                                          the catalyst at least every 12
                                          months.
10. Each new kiln that is used to        Satisfy the applicable
 process clay refractory products.        operating limits specified in
                                          items 11 through 13 of this
                                          table.
11. Each affected kiln that is equipped  a. Maintain the 3-hour block
 with a DLA.                              average pressure drop across
                                          the DLA at or above the
                                          minimum levels established
                                          during the most recent
                                          performance test; and
                                         b. Maintain free-flowing
                                          limestone in the feed hopper,
                                          silo, and DLA at all times;
                                          and
                                         c. Maintain the limestone
                                          feeder at or above the level
                                          established during the most
                                          recent performance test; and
                                         d. Use the same grade of
                                          limestone from the same source
                                          as was used during the most
                                          recent performance test and
                                          maintain records of the source
                                          and type of limestone used.
12. Each affected kiln that is equipped  a. Initiate corrective action
 with a DIFF or DLS/FF.                   within 1 hour of a bag leak
                                          detection system alarm and
                                          complete corrective actions in
                                          accordance with the OM&M plan;
                                          and
                                         b. Verify at least once each 8-
                                          hour shift that lime is free-
                                          flowing by means of a visual
                                          check, checking the output of
                                          a load cell, carrier gas/lime
                                          flow indicator, or carrier gas
                                          pressure drop measurement
                                          system; and
                                         c. Record the lime feeder
                                          setting daily to verify that
                                          the feeder setting is at or
                                          above the level established
                                          during the most recent
                                          performance test.
13. Each affected kiln that is equipped  a. Maintain the 3-hour block
 with a wet scrubber.                     average pressure drop across
                                          the scrubber, liquid pH, and
                                          liquid flow rate at or above
                                          the minimum levels established
                                          during the most recent
                                          performance test; and
                                         b. If chemicals are added to
                                          the scrubber liquid, maintain
                                          the 3-hour block average
                                          chemical feed rate at or above
                                          the minimum chemical feed rate
                                          established during the most
                                          recent performance test.
------------------------------------------------------------------------

      Table 3 to Subpart SSSSS of Part 63--Work Practice Standards

    As stated in Sec. 63.9788, you must comply with the work practice 
standards for affected sources in the following table:

------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. Each basket or container that  a. Control POM      i. At least every
 is used for holding fired         emissions from      10 preheating
 refractory shapes in an           any affected        cycles, clean the
 existing shape preheater and      shape preheater.    residual pitch
 autoclave during the pitch                            from the surfaces
 impregnation process.                                 of the basket or
                                                       container by
                                                       abrasive blasting
                                                       prior to placing
                                                       the basket or
                                                       container in the
                                                       affected shape
                                                       preheater; or
                                                      ii. At least every
                                                       10 preheating
                                                       cycles, subject
                                                       the basket or
                                                       container to a
                                                       thermal process
                                                       cycle that meets
                                                       or exceeds the
                                                       operating
                                                       temperature and
                                                       cycle time of the
                                                       affected
                                                       preheater, AND is
                                                       conducted in a
                                                       process unit that
                                                       is exhausted to a
                                                       thermal or
                                                       catalytic
                                                       oxidizer that is
                                                       comparable to the
                                                       control device
                                                       used on an
                                                       affected defumer
                                                       or coking oven;
                                                       or
                                                      iii. Capture
                                                       emissions from
                                                       the affected
                                                       shape preheater
                                                       and vent them to
                                                       the control
                                                       device that is
                                                       used to control
                                                       emissions from an
                                                       affected defumer
                                                       or coking oven,
                                                       or to a
                                                       comparable
                                                       thermal or
                                                       catalytic
                                                       oxidizer.

[[Page 110]]

 
2. Each new or existing pitch     Control POM         Capture emissions
 working tank.                     emissions.          from the affected
                                                       pitch working
                                                       tank and vent
                                                       them to the
                                                       control device
                                                       that is used to
                                                       control emissions
                                                       from an affected
                                                       defumer or coking
                                                       oven, OR to a
                                                       comparable
                                                       thermal or
                                                       catalytic
                                                       oxidizer.
3. Each new or existing chromium  Minimize fuel-      Use natural gas,
 refractory products kiln.         based HAP           or equivalent, as
                                   emissions.          the kiln fuel,
                                                       except during
                                                       periods of
                                                       natural gas
                                                       curtailment or
                                                       supply
                                                       interruption, as
                                                       defined in Sec.
                                                       63.9824.
4. Each existing clay refractory  Minimize fuel-      Use natural gas,
 products kiln.                    based HAP           or equivalent, as
                                   emissions.          the kiln fuel,
                                                       except during
                                                       periods of
                                                       natural gas
                                                       curtailment or
                                                       supply
                                                       interruption, as
                                                       defined in Sec.
                                                       63.9824.
------------------------------------------------------------------------

 Table 4 to Subpart SSSSS to Part 63--Requirements for Performance Tests

    As stated in Sec. 63.9800, you must comply with the requirements 
for performance tests for affected sources in the following table:

----------------------------------------------------------------------------------------------------------------
 
 
 
----------------------------------------------------------------------------------------------------------------
1. Each affected source listed in     a. Conduct performance    i. The requirements of   (1) Record the date of
 Table 1 to this subpart.              tests.                    the general provisions   the test; and
                                                                 in subpart A of this    (2) Identify the
                                                                 part and the             emission source that
                                                                 requirements to this     is tested; and
                                                                 subpart.                (3) Collect and record
                                                                                          the corresponding
                                                                                          operating parameter
                                                                                          and emission test data
                                                                                          listed in this table
                                                                                          for each run of the
                                                                                          performance test; and
                                                                                         (4) Repeat the
                                                                                          performance test at
                                                                                          least every 5 years;
                                                                                          and
                                                                                         (5) Repeat the
                                                                                          performance test
                                                                                          before changing the
                                                                                          parameter value for
                                                                                          any operating limit
                                                                                          specified in your OM&M
                                                                                          plan; and
                                                                                         (6) If complying with
                                                                                          the THC concentration
                                                                                          or THC percentage
                                                                                          reduction limits
                                                                                          specified in items 2
                                                                                          through 9 of Table 1
                                                                                          to this subpart,
                                                                                          repeat the performance
                                                                                          test under the
                                                                                          conditions specified
                                                                                          in items 2.a.2. and
                                                                                          2.a.3. of this table;
                                                                                          and
                                                                                         (7) If complying with
                                                                                          the emission limits
                                                                                          for new clay
                                                                                          refractory products
                                                                                          kilns specified in
                                                                                          items 10 and 11 of
                                                                                          Table 1 to this
                                                                                          subpart, repeat the
                                                                                          performance test under
                                                                                          the conditions
                                                                                          specified in items
                                                                                          14.a.i.4. and
                                                                                          17.a.i.4. of this
                                                                                          table.
                                      b. Select the locations   i. Method 1 or 1A of 40  (1) To demonstrate
                                       of sampling ports and     CFR part 60, appendix    compliance with the
                                       the number of traverse    A.                       percentage reduction
                                       points.                                            limits specified in
                                                                                          items 2.b., 3.b.,
                                                                                          6.b., 7.b., 10, and 11
                                                                                          of Table 1 to this
                                                                                          subpart, locate
                                                                                          sampling sites at the
                                                                                          inlet of the control
                                                                                          device and at either
                                                                                          the outlet of the
                                                                                          control device or at
                                                                                          the stack prior to any
                                                                                          releases to the
                                                                                          atmosphere; and
                                                                                         (2) To demonstrate
                                                                                          compliance with any
                                                                                          other emission limit
                                                                                          specified in Table 1
                                                                                          to this subpart,
                                                                                          locate all sampling
                                                                                          sites at the outlet of
                                                                                          the control device or
                                                                                          at the stack prior to
                                                                                          any releases to the
                                                                                          atmosphere.

[[Page 111]]

 
                                      c. Determine gas          Method 2, 2A, 2C, 2D,    Measure gas velocities
                                       velocity and volumetric   2F, or 2G of 40 CFR      and volumetric flow
                                       flow rate.                part 60, appendix A.     rates at 1-hour
                                                                                          intervals throughout
                                                                                          each test run.
                                      d. Conduct gas molecular  (i) Method 3, 3A, or 3B  As specified in the
                                       weight analysis.          of 40 CFR part 60,       applicable test
                                                                 appendix A; or           method.
                                                                (ii) ASME PTC 19.10-     You may use ASME PTC
                                                                 1981-Part 10.            19.10-1981-Part 10
                                                                                          (available for
                                                                                          purchase from Three
                                                                                          Park Avenue, New York,
                                                                                          NY 10016-5990) as an
                                                                                          alternative to EPA
                                                                                          Method 3B.
                                      e. Measure gas moisture   Method 4 of 40 CFR part  As specified in the
                                       content.                  60, appendix A.          applicable test
                                                                                          method.
2. Each new or existing curing oven,  a. Conduct performance    .......................  (1) Conduct the
 shape dryer, and kiln that is used    tests.                                             performance test while
 to process refractory products that                                                      the source is
 use organic HAP; each new or                                                             operating at the
 existing coking oven and defumer                                                         maximum organic HAP
 that is used to produce pitch-                                                           processing rate, as
 impregnated refractory products;                                                         defined in Sec.
 each new shape preheater that is                                                         63.9824, reasonably
 used to produce pitch-impregnated                                                        expected to occur; and
 refractory products; AND each new                                                       (2) Repeat the
 or existing process unit that is                                                         performance test
 exhausted to a thermal or catalytic                                                      before starting
 oxidizer that also controls                                                              production of any
 emissions from an affected shape                                                         product for which the
 preheater or pitch working tank.                                                         organic HAP processing
                                                                                          rate is likely to
                                                                                          exceed the maximum
                                                                                          organic HAP processing
                                                                                          rate established
                                                                                          during the most recent
                                                                                          performance test by
                                                                                          more than 10 percent,
                                                                                          as specified in Sec.
                                                                                          63.9798(c); and
                                                                                         (3) Repeat the
                                                                                          performance test on
                                                                                          any affected
                                                                                          uncontrolled kiln
                                                                                          following process
                                                                                          changes (e.g., shorter
                                                                                          curing oven cycle
                                                                                          time) that could
                                                                                          increase organic HAP
                                                                                          emissions from the
                                                                                          affected kiln, as
                                                                                          specified in Sec.
                                                                                          63.9798(d).
                                      b. Satisfy the
                                       applicable requirements
                                       listed in items 3
                                       through 13 of this
                                       table.
3. Each affected continuous process   a. Perform a minimum of   The appropriate test     Each test run must be
 unit.                                 3 test runs.              methods specified in     at least 1 hour in
                                                                 items 1, 4, and 5 of     duration.
                                                                 this table.
                                      b. Establish the          i. Method 311 of 40 CFR  (1) Calculate and
                                       operating limit for the   part 63, appendix A,     record the organic HAP
                                       maximum organic HAP       OR material safety       content of all
                                       processing rate.          data sheets (MSDS), OR   refractory shapes that
                                                                 product labels to        are processed during
                                                                 determine the mass       the performance test,
                                                                 fraction of organic      based on the mass
                                                                 HAP in each resin,       fraction of organic
                                                                 binder, or additive;     HAP in the resins,
                                                                 and                      binders, or additives;
                                                                                          the mass fraction of
                                                                                          each resin, binder, or
                                                                                          additive, in the
                                                                                          product; and the
                                                                                          process feed rate; and

[[Page 112]]

 
                                                                ii. Product formulation  (2) Calculate and
                                                                 data that specify the    record the organic HAP
                                                                 mass fraction of each    processing rate
                                                                 resin, binder, and       (pounds per hour) for
                                                                 additive in the          each test run; and
                                                                 products that are
                                                                 processed during the
                                                                 performance test; and
                                                                iii. Process feed rate   (3) Calculate and
                                                                 data (tons per hour).    record the maximum
                                                                                          organic HAP processing
                                                                                          rate as the average of
                                                                                          the organic HAP
                                                                                          processing rates for
                                                                                          the three test runs.
                                      c. Record the operating   Process data...........  During each test run
                                       temperature of the                                 and at least once per
                                       affected source.                                   hour, record the
                                                                                          operating temperature
                                                                                          in the highest
                                                                                          temperature zone of
                                                                                          the affected source.
4. Each continuous process unit that  a. Measure THC            i. Method 25A of 40 CFR  (1) Each minute,
 is subject to the THC emission        concentrations at the     part 60, appendix A.     measure and record the
 limit listed in item 2.a., 3.a., 4,   outlet of the control                              concentrations of THC
 or 5 of Table 1 to this subpart.      device or in the stack.                            in the exhaust stream;
                                                                                          and
                                                                                         (2) Provide at least 50
                                                                                          1-minute measurements
                                                                                          for each valid hourly
                                                                                          average THC
                                                                                          concentration.
                                      b. Measure oxygen         i. Method 3A of 40 CFR   (1) Each minute,
                                       concentrations at the     part 60, appendix A.     measure and record the
                                       outlet of the control                              concentrations of
                                       device or in the stack.                            oxygen in the exhaust
                                                                                          stream; and
                                                                                         (2) Provide at least 50
                                                                                          1-minute measurements
                                                                                          for each valid hourly
                                                                                          average THC
                                                                                          concentration.
                                      c. Determine the hourly   i. Equation 1 of Sec. (1) Calculate the
                                       average THC               63.9800(g)(1); and.      hourly average THC
                                       concentration,           ii. The 1-minute THC      concentration for each
                                       corrected to 18 percent   and oxygen               hour of the
                                       oxygen.                   concentration data.      performance test as
                                                                                          the average of the 1-
                                                                                          minute THC
                                                                                          measurements; and
                                                                                         (2) Calculate the
                                                                                          hourly average oxygen
                                                                                          concentration for each
                                                                                          hour of the
                                                                                          performance test as
                                                                                          the average of the 1-
                                                                                          minute oxygen
                                                                                          measurements; and
                                                                                         (3) Correct the hourly
                                                                                          average THC
                                                                                          concentrations to 18
                                                                                          percent oxygen using
                                                                                          Equation 1 of Sec.
                                                                                          63.9800(g)(1).
                                      d. Determine the 3-hour   The hourly average       Calculate the 3-hour
                                       block average THC         concentration of THC,    block average THC
                                       emission concentration,   corrected to 18          emission
                                       corrected to 18 percent   percent oxygen, for      concentration,
                                       oxygen.                   each test run.           corrected to 18
                                                                                          percent oxygen, as the
                                                                                          average of the hourly
                                                                                          average THC emission
                                                                                          concentrations,
                                                                                          corrected to 18
                                                                                          percent oxygen.
5. Each continuous process unit that  a. Measure THC            i. Method 25A of 40 CFR  (1) Each minute,
 is subject to the THC percentage      concentrations at the     part 60, appendix A.     measure and record the
 reduction limit listed in item 2.b.   inlet and outlet of the                            concentrations of THC
 or 3.b. of Table 1 to this subpart.   control device.                                    at the inlet and
                                                                                          outlet of the control
                                                                                          device; and
                                                                                         (2) Provide at least 50
                                                                                          1-minute measurements
                                                                                          for each valid hourly
                                                                                          average THC
                                                                                          concentration at the
                                                                                          control device inlet
                                                                                          and outlet.
                                      b. Determine the hourly   i. The 1-minute THC      Calculate the hourly
                                       THC mass emissions        concentration data at    THC mass emissions
                                       rates at the inlet and    the control device       rates at the control
                                       outlet of the control     inlet and outlet; and    device inlet and
                                       device.                  ii. The volumetric flow   outlet for each hour
                                                                 rates at the control     of the performance
                                                                 device inlet and         test.
                                                                 outlet.

[[Page 113]]

 
                                      c. Determine the 3-hour   i. The hourly THC mass   (1) Calculate the
                                       block average THC         emissions rates at the   hourly THC percentage
                                       percentage reduction.     inlet and outlet of      reduction for each
                                                                 the control device.      hour of the
                                                                                          performance test using
                                                                                          Equation 2 of Sec.
                                                                                          63.9800(g)(1); and
                                                                                         (2) Calculate the 3-
                                                                                          hour block average THC
                                                                                          percentage reduction.
6. Each continous process unit that   a. Establish the          i. Continuous recording  (1) At least every 15
 is equipped with a thermal oxidizer.  operating limit for the   of the output of the     minutes, measure and
                                       minimum allowable         combustion chamber       record the thermal
                                       thermal oxidizer          temperature              oxidizer combustion
                                       combustion chamber        measurement device.      chamber temperature;
                                       temperature.                                       and
                                                                                         (2) Provide at least
                                                                                          one measurement during
                                                                                          at least three 15-
                                                                                          minute periods per
                                                                                          hour of testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average thermal
                                                                                          oxidizer combustion
                                                                                          chamber temperature
                                                                                          for each hour of the
                                                                                          performance test; and
                                                                                         (4) Calculate the
                                                                                          minimum allowable
                                                                                          combustion chamber
                                                                                          temperature as the
                                                                                          average of the
                                                                                          combustion chamber
                                                                                          temperatures for the
                                                                                          three test runs, minus
                                                                                          14 [deg]C (25 [deg]F).
7. Each continuous process unit that  a. Establish the          i. Continuous recording  (1) At least every 15
 is equipped with a catalytic          operating limit for the   of the output of the     minutes, measure and
 oxidizer.                             minimum allowable         temperature              record the temperature
                                       temperature at the        measurement device.      at the inlet of the
                                       inlet of the catalyst                              catalyst bed; and
                                       bed.                                              (2) Provide at least
                                                                                          one catalyst bed inlet
                                                                                          temperature
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average
                                                                                          catalyst bed inlet
                                                                                          temperature for each
                                                                                          hour of the
                                                                                          performance test; and
                                                                                         (4) Calculate the
                                                                                          minimum allowable
                                                                                          catalyst bed inlet
                                                                                          temperature as the
                                                                                          average of the
                                                                                          catalyst bed inlet
                                                                                          temperatures for the
                                                                                          three test runs, minus
                                                                                          14 [deg]C (25 [deg]F).
8. Each affected batch process unit.  a. Perform a minimum of   i. The appropriate test  (1) Each test run must
                                       two test runs.            methods specified in     be conducted over a
                                                                 items 1, 9, and 10 of    separate batch cycle
                                                                 this table.              unless you satisfy the
                                                                                          requirements of Sec.
                                                                                          63.9800(f)(3) and (4);
                                                                                          and
                                                                                         (2) Each test run must
                                                                                          begin with the start
                                                                                          of a batch cycle,
                                                                                          except as specified in
                                                                                          item 8.a.i.4. of this
                                                                                          table; and
                                                                                         (3) Each test run must
                                                                                          continue until the end
                                                                                          of the batch cycle,
                                                                                          except as specified in
                                                                                          items 8.a.i.4. and
                                                                                          8.a.i.5. of this
                                                                                          table; and
                                                                                         (4) If you develop an
                                                                                          emissions profile, as
                                                                                          described in Sec.
                                                                                          63.9802(a), AND for
                                                                                          sources equipped with
                                                                                          a thermal or catalytic
                                                                                          oxidizer, you do not
                                                                                          reduce the oxidizer
                                                                                          operating temperature,
                                                                                          as specified in item
                                                                                          13 of this table, you
                                                                                          can limit each test
                                                                                          run to the 3-hour peak
                                                                                          THC emissions period;
                                                                                          and

[[Page 114]]

 
                                                                                         (5) If you do not
                                                                                          develop an emissions
                                                                                          profile, a test run
                                                                                          can be stopped, and
                                                                                          the results of that
                                                                                          run considered
                                                                                          complete, if you
                                                                                          measure emissions
                                                                                          continuously until at
                                                                                          least 3 hours after
                                                                                          the affected process
                                                                                          unit has reached
                                                                                          maximum temperature,
                                                                                          AND the hourly average
                                                                                          THC mass emissions
                                                                                          rate has not increased
                                                                                          during the 3-hour
                                                                                          period since maximum
                                                                                          process temperature
                                                                                          was reached, and the
                                                                                          hourly average
                                                                                          concentrations of THC
                                                                                          at the inlet of the
                                                                                          control device have
                                                                                          not exceeded 20 ppmvd,
                                                                                          corrected to 18
                                                                                          percent oxygen, during
                                                                                          the 3-hour period
                                                                                          since maximum process
                                                                                          temperature was
                                                                                          reached or the hourly
                                                                                          average THC percentage
                                                                                          reduction has been at
                                                                                          least 95 percent
                                                                                          during the 3-hour
                                                                                          period since maximum
                                                                                          process temperature
                                                                                          was reached, AND, for
                                                                                          sources equipped with
                                                                                          a thermal or catalytic
                                                                                          oxidizer, at least 1
                                                                                          hour has passed since
                                                                                          any reduction in the
                                                                                          operating temperature
                                                                                          of the oxidizer, as
                                                                                          specified in item 13
                                                                                          of this table.
                                      b. Establish the          i. Method 311 of 40 CFR  (1) Calculate and
                                       operating limit for the   part 63, appendix A,     record the organic HAP
                                       maximum organic HAP       OR MSDS, OR product      content of all
                                       processing rate.          labels to determine      refractory shapes that
                                                                 the mass fraction of     are processed during
                                                                 organic HAP in each      the performance test,
                                                                 resin, binder, or        based on the mass
                                                                 additive; and            fraction of HAP in the
                                                                                          resins, binders, or
                                                                                          additives; the mass
                                                                                          fraction of each
                                                                                          resin, binder, or
                                                                                          additive, in the
                                                                                          product, and the batch
                                                                                          weight prior to
                                                                                          processing; and
                                                                ii. Product formulation  (2) Calculate and
                                                                 data that specify the    record the organic HAP
                                                                 mass fraction of each    processing rate
                                                                 resin, binder, and       (pounds per batch) for
                                                                 additive in the          each test run; and
                                                                 products that are       (3) Calculate and
                                                                 processed during the     record the maximum
                                                                 performance test; and    organic HAP processing
                                                                iii. Batch weight         rate as the average of
                                                                 (tons).                  the organic HAP
                                                                                          processing rates for
                                                                                          the two test runs.
                                      c. Record the batch       Process data...........  Record the total
                                       cycle time.                                        elapsed time from the
                                                                                          start to the
                                                                                          completion of the
                                                                                          batch cycle.
                                      d. Record the operating   Process data...........  Record the operating
                                       temperature of the                                 temperature of the
                                       affected source.                                   affected source at
                                                                                          least once every hour
                                                                                          from the start to the
                                                                                          completion of the
                                                                                          batch cycle.
9. Each batch process unit that is    a. Measure THC            i. Method 25A of 40 CFR  (1) Each minute,
 subject to the THC emission limit     concentrations at the     part 60, appendix A.     measure and record the
 listed in item 6.a., 7.a., 8, or 9    outlet of the control                              concentrations of THC
 of Table 1 to this subpart.           device or in the stack.                            in the exhaust stream;
                                                                                          and
                                                                                         (2) Provide at least 50
                                                                                          1-minute measurements
                                                                                          for each valid hourly
                                                                                          average THC
                                                                                          concentration.

[[Page 115]]

 
                                      b. Measure oxygen         i. Method 3A of 40 CFR   (1) Each minute,
                                       concentrations at the     part 60, appendix A.     measure and record the
                                       outlet of the control                              concentrations of
                                       device or in the stack.                            oxygen in the exhaust
                                                                                          stream; and
                                                                                         (2) Provide at least 50
                                                                                          1-minute measurements
                                                                                          for each valid hourly
                                                                                          average oxygen
                                                                                          concentration.
                                      c. Determine the hourly   i. Equation 1 of Sec. (1) Calculate the
                                       average THC               63.9800(g)(1); and.      hourly average THC
                                       concentration,           ii. The 1-minute THC      concentration for each
                                       corrected to 18 percent   and oxygen               hour of the
                                       oxygen.                   concentration data.      performance test as
                                                                                          the average of the 1-
                                                                                          minute THC
                                                                                          measurements; and
                                                                                         (2) Calculate the
                                                                                          hourly average oxygen
                                                                                          concentration for each
                                                                                          hour of the
                                                                                          performance test as
                                                                                          the average of the 1-
                                                                                          minute oxygen
                                                                                          measurements; and
                                                                                         (3) Correct the hourly
                                                                                          average THC
                                                                                          concentrations to 18
                                                                                          percent oxygen using
                                                                                          Equation 1 of Sec.
                                                                                          63.9800(g)(1).
                                      d. Determine the 3-hour   The hourly average THC   Select the period of 3
                                       peak THC emissions        concentrations,          consecutive hours over
                                       period for each test      corrected to 18          which the sum of the
                                       run.                      percent oxygen.          hourly average THC
                                                                                          concentrations,
                                                                                          corrected to 18
                                                                                          percent oxygen, is
                                                                                          greater than the sum
                                                                                          of the hourly average
                                                                                          THC emission
                                                                                          concentrations,
                                                                                          corrected to 18
                                                                                          percent oxygen, for
                                                                                          any other period of 3
                                                                                          consecutive hours
                                                                                          during the test run.
                                      e. Determine the average  The hourly average THC   Calculate the average
                                       THC concentration,        emission                 of the hourly average
                                       corrected to 18 percent   concentrations,          THC concentrations,
                                       oxygen, for each test     corrected to 18          corrected to 18
                                       run.                      percent oxygen, for      percent oxygen, for
                                                                 the 3-hour peak THC      the 3 hours of the
                                                                 emissions period.        peak emissions period
                                                                                          for each test run.
                                      f. Determine the 2-run    The average THC          Calculate the average
                                       block average THC         concentration,           of the average THC
                                       concentration,            corrected to 18          concentrations,
                                       corrected to 18 percent   percent oxygen, for      corrected to 18
                                       oxygen, for the           each test run.           percent oxygen, for
                                       emission test.                                     each run.
10. Each batch process unit that is   a. Measure THC            i. Method 25A of 40 CFR  (1) Each minute,
 subject to the THC percentage         concentrations at the     part 60, appendix A.     measure and record the
 reduction limit listed in item 6.b.   inlet and outlet of the                            concentrations of THC
 or 7.b. of Table 1 to this subpart.   control device.                                    at the control device
                                                                                          inlet and outlet; and
                                                                                         (2) Provide at least 50
                                                                                          1-minute measurements
                                                                                          for each valid hourly
                                                                                          average THC
                                                                                          concentration at the
                                                                                          control device inlet
                                                                                          and outlet.
                                      b. Determine the hourly   i. The 1-minute THC      (1) Calculate the
                                       THC mass emissions        concentration data at    hourly mass emissions
                                       rates at the control      the control device       rates at the control
                                       device inlet and outlet.  inlet and outlet; and    device inlet and
                                                                ii. The volumetric flow   outlet for each hour
                                                                 rates at the control     of the performance
                                                                 device inlet and         test.
                                                                 outlet.
                                      c. Determine the 3-hour   The hourly THC mass      Select the period of 3
                                       peak THC emissions        emissions rates at the   consecutive hours over
                                       period for each test      control device inlet.    which the sum of the
                                       run.                                               hourly THC mass
                                                                                          emissions rates at the
                                                                                          control device inlet
                                                                                          is greater than the
                                                                                          sum of the hourly THC
                                                                                          mass emissions rates
                                                                                          at the control device
                                                                                          inlet for any other
                                                                                          period of 3
                                                                                          consecutive hours
                                                                                          during the test run.
                                      d. Determine the average  i. Equation 2 of Sec. Calculate the average
                                       THC percentage            63.9800(g)(2); and.      THC percentage
                                       reduction for each test  ii. The hourly THC mass   reduction for each
                                       run.                      emissions rates at the   test run using
                                                                 control device inlet     Equation 2 of Sec.
                                                                 and outlet for the 3-    63.9800(g)(2).
                                                                 hour peak THC
                                                                 emissions period.

[[Page 116]]

 
                                      e. Determine the 2-run    The average THC          Calculate the average
                                       block average THC         percentage reduction     of the average THC
                                       percentage reduction      for each test run.       percentage reductions
                                       for the emission test.                             for each test run.
11. Each batch process unit that is   a. Establish the          i. Continuous recording  (1) At least every 15
 equipped with a thermal oxidizer.     operating limit for the   of the output of the     minutes, measure and
                                       minimum thermal           combustion chamber       record the thermal
                                       oxidizer combustion       temperature              oxidizer combustion
                                       chamber temperature.      measurement device.      chamber temperature;
                                                                                          and
                                                                                         (2) Provide at least
                                                                                          one temperature
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average
                                                                                          combustion chamber
                                                                                          temperature for each
                                                                                          hour of the 3-hour
                                                                                          peak emissions period,
                                                                                          as defined in item
                                                                                          9.d. or 10.c. of this
                                                                                          table, whichever
                                                                                          applies; and
                                                                                         (4) Calculate the
                                                                                          minimum allowable
                                                                                          thermal oxidizer
                                                                                          combustion chamber
                                                                                          operating temperature
                                                                                          as the average of the
                                                                                          hourly combustion
                                                                                          chamber temperatures
                                                                                          for the 3-hour peak
                                                                                          emissions period,
                                                                                          minus 14 [deg]C (25
                                                                                          [deg]F).
12. Each batch process unit that is   a. Establish the          i. Continuous recording  (1) At least every 15
 equipped with a catalytic oxidizer.   operating limit for the   of the output of the     minutes, measure and
                                       minimum temperature at    temperature              record the temperature
                                       the inlet of the          measurement device.      at the inlet of the
                                       catalyst bed.                                      catalyst bed; and
                                                                                         (2) Provide at least
                                                                                          one catalyst bed inlet
                                                                                          temperature
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average
                                                                                          catalyst bed inlet
                                                                                          temperature for each
                                                                                          hour of the 3-hour
                                                                                          peak emissions period,
                                                                                          as defined in item
                                                                                          9.d. or 10.c. of this
                                                                                          table, whichever
                                                                                          applies; and
                                                                                         (4) Calculate the
                                                                                          minimum allowable
                                                                                          catalytic oxidizer
                                                                                          catalyst bed inlet
                                                                                          temperature as the
                                                                                          average of the hourly
                                                                                          catalyst bed inlet
                                                                                          temperatures for the 3-
                                                                                          hour peak emissions
                                                                                          period, minus 14
                                                                                          [deg]C (25 [deg]F).
13. Each batch process unit that is   a. During each test run,                           (1) The oxidizer can be
 equipped with a thermal or            maintain the applicable                            shut off or the
 catalytic oxidizer.                   operating temperature                              oxidizer operating
                                       of the oxidizer until                              temperature can be
                                       emission levels allow                              reduced if you do not
                                       the oxidizer to be shut                            use an emission
                                       off or the operating                               profile to limit
                                       temperature of the                                 testing to the 3-hour
                                       oxidizer to be reduced.                            peak emissions period,
                                                                                          as specified in item
                                                                                          8.a.i.4. of this
                                                                                          table; and
                                                                                         (2) At least 3 hours
                                                                                          have passed since the
                                                                                          affected process unit
                                                                                          reached maximum
                                                                                          temperature; and
                                                                                         (3) The applicable
                                                                                          emission limit
                                                                                          specified in item 6.a.
                                                                                          or 6.b. of Table 1 to
                                                                                          this subpart was met
                                                                                          during each of the
                                                                                          previous three 1-hour
                                                                                          periods; and
                                                                                         (4) The hourly average
                                                                                          THC mass emissions
                                                                                          rate did not increase
                                                                                          during the 3-hour
                                                                                          period since maximum
                                                                                          process temperature
                                                                                          was reached; and

[[Page 117]]

 
                                                                                         (5) The applicable
                                                                                          emission limit
                                                                                          specified in item 6.a.
                                                                                          and 6.b. of Table 1 to
                                                                                          this subpart was met
                                                                                          during each of the
                                                                                          four 15-minute periods
                                                                                          immediately following
                                                                                          the oxidizer
                                                                                          temperature reduction;
                                                                                          and
                                                                                         (6) If the applicable
                                                                                          emission limit
                                                                                          specified in item 6.a.
                                                                                          or 6.b. of Table 1 to
                                                                                          this subpart was not
                                                                                          met during any of the
                                                                                          four 15-minute periods
                                                                                          immediately following
                                                                                          the oxidizer
                                                                                          temperature reduction,
                                                                                          you must return the
                                                                                          oxidizer to its normal
                                                                                          operating temperature
                                                                                          as soon as possible
                                                                                          and maintain that
                                                                                          temperature for at
                                                                                          least 1 hour; and
                                                                                         (7) Continue the test
                                                                                          run until the
                                                                                          applicable emission
                                                                                          limit specified in
                                                                                          items 6.a. and 6.b. of
                                                                                          Table 1 to this
                                                                                          subpart is met for at
                                                                                          least four consecutive
                                                                                          15-minute periods that
                                                                                          immediately follow the
                                                                                          temperature reduction;
                                                                                          and
                                                                                         (8) Calculate the
                                                                                          hourly average
                                                                                          oxidizer operating
                                                                                          temperature for each
                                                                                          hour of the
                                                                                          performance test since
                                                                                          the affected process
                                                                                          unit reached maximum
                                                                                          temperature.
14. Each new continuous kiln that is  a. Measure emissions of   i. Method 26A of 40 CFR  (1) Conduct the test
 used to process clay refractory       HF and HCl.               part 60, appendix A;     while the kiln is
 products.                                                       or                       operating at the
                                                                ii. Method 26 of 40 CFR   maximum production
                                                                 part 60, appendix A;     level; and
                                                                 or.                     (2) You may use Method
                                                                iii. Method 320 of 40     26 of 40 CFR part 60,
                                                                 CFR part 63, appendix    appendix A, only if no
                                                                 A.                       acid PM (e.g., HF or
                                                                                          HCl dissolved in water
                                                                                          droplets emitted by
                                                                                          sources controlled by
                                                                                          a wet scrubber) is
                                                                                          present; and
                                                                                         (3) If you use Method
                                                                                          320 of 40 CFR part 63,
                                                                                          appendix A, you must
                                                                                          follow the analyte
                                                                                          spiking procedures of
                                                                                          Section 13 of Method
                                                                                          320 unless you can
                                                                                          demonstrate that the
                                                                                          complete spiking
                                                                                          procedure has been
                                                                                          conducted at a similar
                                                                                          source; and
                                                                                         (4) Repeat the
                                                                                          performance test if
                                                                                          the affected source is
                                                                                          controlled with a DLA
                                                                                          and you change the
                                                                                          source of the
                                                                                          limestone used in the
                                                                                          DLA.
                                      b. Perform a minimum of   The appropriate test     Each test run must be
                                       3 test runs.              methods specified in     at least 1 hour in
                                                                 items 1 and 14.a. of     duration.
                                                                 this table.
15. Each new continuous kiln that is  a. Record the uncalcined  i. Production data; and  (1) Record the
 subject to the production-based HF    clay processing rate.    ii. Product formulation   production rate (tons
 and HCl emission limits specified                               data that specify the    per hour of fired
 in items 10.a. and 10.b. of Table 1                             mass fraction of         product); and
 to this subpart.                                                uncalcined clay in the  (2) Calculate and
                                                                 products that are        record the average
                                                                 processed during the     rate at which
                                                                 performance test.        uncalcined clay is
                                                                                          processed (tons per
                                                                                          hour) for each test
                                                                                          run; and
                                                                                         (3) Calculate and
                                                                                          record the 3-run
                                                                                          average uncalcined
                                                                                          clay processing rate
                                                                                          as the average of the
                                                                                          average uncalcined
                                                                                          clay processing rates
                                                                                          for each test run.

[[Page 118]]

 
                                      b. Determine the HF mass  i. Method 26A of 40 CFR  Calculate the HF mass
                                       emissions rate at the     part 60, appendix A;     emissions rate for
                                       outlet of the control     or                       each test.
                                       device or in the stack.  ii. Method 26 of 40 CFR
                                                                 part 60, appendix A;
                                                                 or.
                                                                iii. Method 320 of 40
                                                                 CFR part 63, appendix
                                                                 A.
                                      c. Determine the 3-hour   i. The HF mass           (1) Calculate the
                                       block average             emissions rate for       hourly production-
                                       production-based HF       each test run; and       based HF emissions
                                       emissions rate.          ii. The average           rate for each test run
                                                                 uncalcined clay          using Equation 3 of
                                                                 processing rate.         Sec. 63.9800(g)(3);
                                                                                          and
                                                                                         (2) Calculate the 3-
                                                                                          hour block average
                                                                                          production-based HF
                                                                                          emissions rate as the
                                                                                          average of the hourly
                                                                                          production-based HF
                                                                                          emissions rates for
                                                                                          each test run.
                                      d. Determine the HCl      i. Method 26A of 40 CFR  Calculate the HCl mass
                                       mass emissions rate at    part 60, appendix A;     emissions rate for
                                       the outlet of the         or                       each test run.
                                       control device or in     ii. Method 26 of 40 CFR
                                       the stack.                part 60, appendix A;
                                                                 or.
                                                                iii. Method 320 of 40
                                                                 CFR part 63, appendix
                                                                 A.
                                      e. Determine the 3-hour   i. The HCl mass          (1) Calculate the
                                       block average             emissions rate for       hourly production-
                                       production-based HCl      each test run; and       based HCl emissions
                                       emissions rate.          ii. The average           rate for each test run
                                                                 uncalcined clay          using Equation 3 of
                                                                 processing rate.         Sec. 63.9800(g)(3);
                                                                                          and
                                                                                         (2) Calculate the 3-
                                                                                          hour block average
                                                                                          production-based HCl
                                                                                          emissions rate as the
                                                                                          average of the
                                                                                          production-based HCl
                                                                                          emissions rates for
                                                                                          each test run.
16. Each new continuous kiln that is  a. Measure the HF mass    i. Method 26A of 40 CFR  Calculate the HF mass
 subject to the HF and HCl             emissions rates at the    part 60, appendix A;     emissions rates at the
 percentage reduction limits           inlet and outlet of the   or                       control device inlet
 specified in items 10.a. and 10.b.    control device.          ii. Method 26 of 40 CFR   and outlet for each
 of Table 1 to this subpart.                                     part 60, appendix A;     test run.
                                                                 or.
                                                                iii. Method 320 of 40
                                                                 CFR part 63, appendix
                                                                 A.
                                      b. Determine the 3-hour   i. The HF mass           (1) Calculate the
                                       block average HF          emissions rates at the   hourly HF percentage
                                       percentage reduction.     inlet and outlet of      reduction using
                                                                 the control device for   Equation 2 of Sec.
                                                                 each test run            63.9800(g)(2); and
                                                                                         (2) Calculate the 3-
                                                                                          hour block average HF
                                                                                          percentage reduction
                                                                                          as the average of the
                                                                                          HF percentage
                                                                                          reductions for each
                                                                                          test run.
                                      c. Measure the HCl mass   i. Method 26A of 40 CFR  Calculate the HCl mass
                                       emissions rates at the    part 60, appendix A;     emissions rates at the
                                       inlet and outlet of the   or                       control device inlet
                                       control device.          ii. Method 26 of 40 CFR   and outlet for each
                                                                 part 60, appendix A;     test run.
                                                                 or.
                                                                iii. Method 320 of 40
                                                                 CFR part 63, appendix
                                                                 A.
                                      d. Determine the 3-hour   i. The HCl mass          (1) Calculate the
                                       block average HCl         emissions rates at the   hourly HCl percentage
                                       percentage reduction.     inlet and outlet of      reduction using
                                                                 the control device for   Equation 2 of Sec.
                                                                 each test run.           63.9800(g)(2); and
                                                                                         (2) Calculate the 3-
                                                                                          hour block average HCl
                                                                                          percentage reduction
                                                                                          as the average of HCl
                                                                                          percentage reductions
                                                                                          for each test run.

[[Page 119]]

 
17. Each new batch process kiln that  a. Measure emissions of   i. Method 26A of 40 CFR  (1) Conduct the test
 is used to process clay refractory    HF and HCl at the inlet   part 60, appendix A;     while the kiln is
 products.                             and outlet of the         or                       operating at the
                                       control device.          ii. Method 26 of 40 CFR   maximum production
                                                                 part 60, appendix A;     level; and
                                                                 or.                     (2) You may use Method
                                                                iii. Method 320 of 40     26 of 40 CFR part 60,
                                                                 CFR part 63, appendix    appendix A, only if no
                                                                 A.                       acid PM (e.g., HF or
                                                                                          HCl dissolved in water
                                                                                          droplets emitted by
                                                                                          sources controlled by
                                                                                          a wet scrubber) is
                                                                                          present; and
                                                                                         (3) If you use Method
                                                                                          320 of 40 CFR part 63,
                                                                                          you must follow the
                                                                                          analyte spiking
                                                                                          procedures of Section
                                                                                          13 of Method 320
                                                                                          unless you can
                                                                                          demonstrate that the
                                                                                          complete spiking
                                                                                          procedure has been
                                                                                          conducted at a similar
                                                                                          source; and
                                                                                         (4) Repeat the
                                                                                          performance test if
                                                                                          the affected source is
                                                                                          controlled with a DLA
                                                                                          and you change the
                                                                                          source of the
                                                                                          limestone used in the
                                                                                          DLA.
                                      b. Perform a minimum of   i. The appropriate test  (1) Each test run must
                                       2 test runs.              methods specified in     be conducted over a
                                                                 items 1 and 17.a. of     separate batch cycle
                                                                 this table.              unless you satisfy the
                                                                                          requirements of Sec.
                                                                                          63.9800(f)(3) and (4);
                                                                                          and
                                                                                         (2) Each test run must
                                                                                          consist of a series of
                                                                                          1-hour runs at the
                                                                                          inlet and outlet of
                                                                                          the control device,
                                                                                          beginning with the
                                                                                          start of a batch
                                                                                          cycle, except as
                                                                                          specified in item
                                                                                          17.b.i.4. of this
                                                                                          table; and
                                                                                         (3) Each test run must
                                                                                          continue until the end
                                                                                          of the batch cycle,
                                                                                          except as specified in
                                                                                          item 17.b.i.4. of this
                                                                                          table; and
                                                                                         (4) If you develop an
                                                                                          emissions profile, as
                                                                                          described in Sec.
                                                                                          63.9802(b), you can
                                                                                          limit each test run to
                                                                                          the 3-hour peak HF
                                                                                          emissions period.
                                      c. Determine the hourly   i. The appropriate test  Determine the hourly
                                       HF and HCl mass           methods specified in     mass HF and HCl
                                       emissions rates at the    items 1 and 17.a. of     emissions rates at the
                                       inlet and outlet of the   this table.              inlet and outlet of
                                       control device.                                    the control device for
                                                                                          each hour of each test
                                                                                          run.
                                      d. Determine the 3-hour   The hourly HF mass       Select the period of 3
                                       peak HF emissions         emissions rates at the   consecutive hours over
                                       period.                   inlet of the control     which the sum of the
                                                                 device.                  hourly HF mass
                                                                                          emissions rates at the
                                                                                          control device inlet
                                                                                          is greater than the
                                                                                          sum of the hourly HF
                                                                                          mass emissions rates
                                                                                          at the control device
                                                                                          inlet for any other
                                                                                          period of 3
                                                                                          consecutive hours
                                                                                          during the test run.
                                      e. Determine the 2-run    i. The hourly average    (1) Calculate the HF
                                       block average HF          HF emissions rates at    percentage reduction
                                       percentage reduction      the inlet and outlet     for each hour of the 3-
                                       for the emissions test.   of the control device.   hour peak HF emissions
                                                                                          period using Equation
                                                                                          2 of Sec.
                                                                                          63.9800(g)(2); and
                                                                                         (2) Calculate the
                                                                                          average HF percentage
                                                                                          reduction for each
                                                                                          test run as the
                                                                                          average of the hourly
                                                                                          HF percentage
                                                                                          reductions for the 3-
                                                                                          hour peak HF emissions
                                                                                          period for that run;
                                                                                          and

[[Page 120]]

 
                                                                                         (3) Calculate the 2-run
                                                                                          block average HF
                                                                                          percentage reduction
                                                                                          for the emission test
                                                                                          as the average of the
                                                                                          average HF percentage
                                                                                          reductions for the two
                                                                                          test runs.
                                      f. Determine the 2-run    i. The hourly average    (1) Calculate the HCl
                                       block average HCl         HCl emissions rates at   percentage reduction
                                       percentage reduction      the inlet and outlet     for each hour of the 3-
                                       for the emission test.    of the control device.   hour peak HF emissions
                                                                                          period using Equation
                                                                                          2 Sec.
                                                                                          63.9800(g)(2); and
                                                                                         (2) Calculate the
                                                                                          average HCl percentage
                                                                                          reduction for each
                                                                                          test run as the
                                                                                          average of the hourly
                                                                                          HCl percentage
                                                                                          reductions for the 3-
                                                                                          hour peak HF emissions
                                                                                          period for that run;
                                                                                          and
                                                                                         (3) Calculate the 2-run
                                                                                          block average HCl
                                                                                          percentage reduction
                                                                                          for the emission test
                                                                                          as the average of the
                                                                                          average HCl percentage
                                                                                          reductions for the two
                                                                                          test runs.
18. Each new kiln that is used to     a. Establish the          Data from the pressure   (1) At least every 15
 process clay refractory products      operating limit for the   drop measurement         minutes, measure the
 and is equipped with a DLA.           minimum pressure drop     device during the        pressure drop across
                                       across the DLA.           performance test.        the DLA; and
                                                                                         (2) Provide at least
                                                                                          one pressure drop
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average
                                                                                          pressure drop across
                                                                                          the DLA for each hour
                                                                                          of the performance
                                                                                          test; and
                                                                                         (4) Calculate and
                                                                                          record the minimum
                                                                                          pressure drop as the
                                                                                          average of the hourly
                                                                                          average pressure drops
                                                                                          across the DLA for the
                                                                                          two or three test
                                                                                          runs, whichever
                                                                                          applies.
                                      b. Establish the          Data from the limestone  (1) Ensure that
                                       operating limit for the   feeder during the        limestone in the feed
                                       limestone feeder          performance test.        hopper, silo, and DLA
                                       setting.                                           is free-flowing at all
                                                                                          times during the
                                                                                          performance test; and
                                                                                         (2) Establish the
                                                                                          limestone feeder
                                                                                          setting 1 week prior
                                                                                          to the performance
                                                                                          test; and
                                                                                         (3) Record and maintain
                                                                                          the feeder setting for
                                                                                          the 1-week period that
                                                                                          precedes the
                                                                                          performance test and
                                                                                          during the performance
                                                                                          test.
19. Each new kiln that is used to     a. Document conformance   Data from the            Submit analyses and
 process clay refractory products      with specifications and   installation and         supporting
 and is equipped with a DIFF or DLS/   requirements of the bag   calibration of the bag   documentation
 FF.                                   leak detection system.    leak detection system.   demonstrating
                                                                                          conformance with EPA
                                                                                          guidance and
                                                                                          specifications for bag
                                                                                          leak detection systems
                                                                                          as part of the
                                                                                          Notification of
                                                                                          Compliance Status.
                                      b. Establish the          i. Data from the lime    (1) For continuous lime
                                       operating limit for the   feeder during the        injection systems,
                                       lime feeder setting.      performance test.        ensure that lime in
                                                                                          the feed hopper or
                                                                                          silo is free-flowing
                                                                                          at all times during
                                                                                          the performance test;
                                                                                          and
                                                                                         (2) Record the feeder
                                                                                          setting for the three
                                                                                          test runs; and
                                                                                         (3) If the feed rate
                                                                                          setting varies during
                                                                                          the three test runs,
                                                                                          calculate and record
                                                                                          the average feed rate
                                                                                          for the two or three
                                                                                          test runs, whichever
                                                                                          applies.

[[Page 121]]

 
20. Each new kiln that is used to     a. Establish the          i. Data from the         (1) At least every 15
 process clay refractory products      operating limit for the   pressure drop            minutes, measure the
 and is equipped with a wet scrubber.  minimum scrubber          measurement device       pressure drop across
                                       pressure drop.            during the performance   the scrubber; and
                                                                 test.                   (2) Provide at least
                                                                                          one pressure drop
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average
                                                                                          pressure drop across
                                                                                          the scrubber for each
                                                                                          hour of the
                                                                                          performance test; and
                                                                                         (4) Calculate and
                                                                                          record the minimum
                                                                                          pressure drop as the
                                                                                          average of the hourly
                                                                                          average pressure drops
                                                                                          across the scrubber
                                                                                          for the two or three
                                                                                          test runs, whichever
                                                                                          applies.
                                      b. Establish the          i. Data from the pH      (1) At least every 15
                                       operating limit for the   measurement device       minutes, measure
                                       minimum scrubber liquid   during the performance   scrubber liquid pH;
                                       pH.                       test.                    and
                                                                                         (2) Provide at least
                                                                                          one pH measurement
                                                                                          during at least three
                                                                                          15-minute periods per
                                                                                          hour of testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average pH
                                                                                          values for each hour
                                                                                          of the performance
                                                                                          test; and
                                                                                         (4) Calculate and
                                                                                          record the minimum
                                                                                          liquid pH as the
                                                                                          average of the hourly
                                                                                          average pH
                                                                                          measurements for the
                                                                                          two or three test
                                                                                          runs, whichever
                                                                                          applies.
                                      c. Establish the          i. Data from the flow    (1) At least every 15
                                       operating limit for the   rate measurement         minutes, measure the
                                       minimum scrubber liquid   device during the        scrubber liquid flow
                                       flow rate.                performance test.        rate; and
                                                                                         (2) Provide at least
                                                                                          one flow rate
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average liquid
                                                                                          flow rate for each
                                                                                          hour of the
                                                                                          performance test; and
                                                                                         (4) Calculate and
                                                                                          record the minimum
                                                                                          liquid flow rate as
                                                                                          the average of the
                                                                                          hourly average liquid
                                                                                          flow rates for the two
                                                                                          or three test runs,
                                                                                          whichever applies.
                                      d. If chemicals are       i. Data from the         (1) At least every 15
                                       added to the scrubber     chemical feed rate       minutes, measure the
                                       liquid, establish the     measurement device       scrubber chemical feed
                                       operating limit for the   during the performance   rate; and
                                       minimum scrubber          test.                   (2) Provide at least
                                       chemical feed rate.                                one chemical feed rate
                                                                                          measurement during at
                                                                                          least three 15-minute
                                                                                          periods per hour of
                                                                                          testing; and
                                                                                         (3) Calculate the
                                                                                          hourly average
                                                                                          chemical feed rate for
                                                                                          each hour of the
                                                                                          performance test; and
                                                                                         (4) Calculate and
                                                                                          record the minimum
                                                                                          chemical feed rate as
                                                                                          the average of the
                                                                                          hourly average
                                                                                          chemical feed rates
                                                                                          for the two or three
                                                                                          test runs, whichever
                                                                                          applies.
----------------------------------------------------------------------------------------------------------------

 Table 5 to Subpart SSSSS of Part 63--Initial Compliance with Emission 
                                 Limits

    As stated in Sec. 63.9806, you must show initial compliance with 
the emission limits for affected sources according to the following 
table:

[[Page 122]]



------------------------------------------------------------------------
 
 
 
------------------------------------------------------------------------
1. Each affected source       a. Each applicable    i. Emissions
 listed in Table 1 to this     emission limit        measured using the
 subpart.                      listed in Table 1     test methods
                               to this subpart.      specified in Table
                                                     4 to this subpart
                                                     satisfy the
                                                     applicable emission
                                                     limits specified in
                                                     Table 1 to this
                                                     subpart; and
                                                    ii. You establish
                                                     and have a record
                                                     of the operating
                                                     limits listed in
                                                     Table 2 to this
                                                     subpart over the
                                                     performance test
                                                     period; and
                                                    iii. You report the
                                                     results of the
                                                     performance test in
                                                     the Notification of
                                                     Compliance Status,
                                                     as specified by
                                                     Sec.
                                                     63.9812(e)(1) and
                                                     (2).
2. Each new or existing       As specified in       You have satisfied
 curing oven, shape dryer,     items 3 through 8     the applicable
 and kiln that is used to      of this table.        requirements
 process refractory products                         specified in items
 that use organic HAP; each                          3 through 8 of this
 new or existing coking oven                         table.
 and defumer that is used to
 produce pitch-impregnated
 refractory products; each
 new shape preheater that is
 used to produce pitch-
 impregnated refractory
 products; AND each new or
 existing process unit that
 is exhausted to a thermal
 or catalytic oxidizer that
 also controls emissions
 from an affected shape
 preheater or pitch working
 tank.
3. Each affected continuous   The average THC       The 3-hour block
 process unit that is          concentration must    average THC
 subject to the THC emission   not exceed 20         emission
 concentration limit listed    ppmvd, corrected to   concentration
 in item 2.a., 3.a., 4, or 5   18 percent oxygen.    measured during the
 of Table 1 to this subpart.                         performance test
                                                     using Methods 25A
                                                     and 3A is equal to
                                                     or less than 20
                                                     ppmvd, corrected to
                                                     18 percent oxygen.
4. Each affected continuous   The average THC       The 3-hour block
 process unit that is          percentage            average THC
 subject to the THC            reduction must        percentage
 percentage reduction limit    equal or exceed 95    reduction measured
 listed in item 2.b. or 3.b.   percent.              during the
 of Table 1 to this subpart.                         performance test
                                                     using Method 25A is
                                                     equal to or greater
                                                     than 95 percent.
5. Each affected batch        The average THC       The 2-run block
 process unit that is          concentration must    average THC
 subject to the THC emission   not exceed 20         emission
 concentration limit listed    ppmvd, corrected to   concentration for
 in item 6.a., 7.a., 8, or 9   18 percent oxygen.    the 3-hour peak
 of Table 1 to this subpart.                         emissions period
                                                     measured during the
                                                     performance test
                                                     using Methods 25A
                                                     and 3A is equal to
                                                     or less than 20
                                                     ppmvd, corrected to
                                                     18 percent oxygen.
6. Each affected batch        The average THC       The 2-run block
 process unit that is          percentage            average THC
 subject to the THC            reduction must        percentage
 percentage reduction limit    equal or exceed 95    reduction for the 3-
 listed in item 6.b. or 7.b.   percent.              hour peak emissions
 of Table 1 to this subpart.                         period measured
                                                     during the
                                                     performance test
                                                     using Method 25A is
                                                     equal to or exceeds
                                                     95 percent.
7. Each affected continuous   a. The average THC    i. You have
 or batch process unit that    concentration must    installed a THC
 is equipped with a control    not exceed 20         CEMS at the outlet
 device other than a thermal   ppmvd, corrected to   of the control
 or catalytic oxidizer and     18 percent oxygen;    device or in the
 is subject to the emission    or                    stack of the
 limit listed in item 3 or 7                         affected source;
 of Table 1 to this subpart.                         and
                              b. The average THC    ii. You have
                               percentage            satisfied the
                               reduction must        requirements of PS-
                               equal or exceed 95    8 of 40 CFR part
                               percent.              60, appendix B.
8. Each affected continuous   The average THC       i. You have
 or batch process unit that    concentration must    installed a THC
 uses process changes to       not exceed 20         CEMS at the outlet
 reduce organic HAP            ppmvd, corrected to   of the control
 emissions and is subject to   18 percent oxygen.    device or in the
 the emission limit listed                           stack of the
 in item 4 or 8 of Table 1                           affected source;
 to this subpart.                                    and
                                                    ii. You have
                                                     satisfied the
                                                     requirements of PS-
                                                     8 of 40 CFR part
                                                     60, appendix B.
9. Each new continuous kiln   a. The average HF     i. The 3-hour block
 that is used to process       emissions must not    average production-
 clay refractory products.     exceed 0.019 kg/Mg    based HF emissions
                               (0.038 lb/ton) of     rate measured
                               uncalcined clay       during the
                               processed; OR the     performance test
                               average               using one of the
                               uncontrolled HF       methods specified
                               emissions must be     in item 14.a.i. of
                               reduced by at least   Table 4 to this
                               90 percent.           subpart is equal to
                                                     or less than 0.019
                                                     kg/Mg (0.038 lb/
                                                     ton) of uncalcined
                                                     clay processed; or
                                                    ii. The 3-hour block
                                                     average HF
                                                     emissions reduction
                                                     measured during the
                                                     performance test is
                                                     equal to or greater
                                                     than 90 percent.

[[Page 123]]

 
                              b. The average HCl    i. The 3-hour block
                               emissions must not    average production-
                               exceed 0.091 kg/Mg    based HCl emissions
                               (0.18 lb/ton) of      rate measured
                               uncalcined clay       during the
                               processed; OR the     performance test
                               average               using one of the
                               uncontrolled HCl      methods specified
                               emissions must be     in item 14.a.i. of
                               reduced by at least   Table 4 to this
                               30 percent.           subpart is equal to
                                                     or less than 0.091
                                                     kg/Mg (0.18 lb/ton)
                                                     of uncalcined clay
                                                     processed; or
                                                    ii. The 3-hour block
                                                     average HCl
                                                     emissions reduction
                                                     measured during the
                                                     performance test is
                                                     equal to or greater
                                                     than 30 percent.
10. Each new batch process    a. The average        The 2-run block
 kiln that is used to          uncontrolled HF       average HF emission
 process clay refractory       emissions must be     reduction measured
 products.                     reduced by at least   during the
                               90 percent.           performance test is
                                                     equal to or greater
                                                     than 90 percent.
                              b. The average        The 2-run block
                               uncontrolled HCl      average HCl
                               emissions must be     emissions reduction
                               reduced by at least   measured during the
                               30 percent.           performance test is
                                                     equal to or greater
                                                     than 30 percent.
------------------------------------------------------------------------

   Table 6 to Subpart SSSSS of Part 63--Initial Compliance with Work 
                           Practice Standards

    As stated in Sec. 63.9806, you must show initial compliance with 
the work practice standards for affected sources according to the 
following table:

------------------------------------------------------------------------
 
 
 
------------------------------------------------------------------------
1. Each affected source       a. Each applicable    i. You have selected
 listed in Table 3 to this     work practice         a method for
 subpart.                      standard listed in    performing each of
                               Table 3 to this       the applicable work
                               subpart.              practice standards
                                                     listed in Table 3
                                                     to this subpart;
                                                     and
                                                    ii. You have
                                                     included in your
                                                     Initial
                                                     Notification a
                                                     description of the
                                                     method selected for
                                                     complying with each
                                                     applicable work
                                                     practice standard,
                                                     as required by Sec.
                                                       63.9(b); and
                                                    iii. You submit a
                                                     signed statement
                                                     with the
                                                     Notification of
                                                     Compliance Status
                                                     that you have
                                                     implemented the
                                                     applicable work
                                                     practice standard
                                                     listed in Table 3
                                                     to this subpart;
                                                     and
                                                    iv. You have
                                                     described in your
                                                     OM&M plan the
                                                     method for
                                                     complying with each
                                                     applicable work
                                                     practice standard
                                                     specified in Table
                                                     3 to this subpart.
2. Each basket or container   a. Control POM        i. You have
 that is used for holding      emissions from any    implemented at
 fired refractory shapes in    affected shape        least one of the
 an existing shape preheater   preheater.            work practice
 and autoclave during the                            standards listed in
 pitch impregnation process.                         item 1 of Table 3
                                                     to this subpart;
                                                     and
                                                    ii. You have
                                                     established a
                                                     system for
                                                     recording the date
                                                     and cleaning method
                                                     for each time you
                                                     clean an affected
                                                     basket or
                                                     container.
3. Each affected new or       Control POM           You have captured
 existing pitch working tank.  emissions.            and vented
                                                     emissions from the
                                                     affected pitch
                                                     working tank to the
                                                     device that is used
                                                     to control
                                                     emissions from an
                                                     affected defumer or
                                                     coking oven, or to
                                                     a thermal or
                                                     catalytic oxidizer
                                                     that is comparable
                                                     to the control
                                                     device used on an
                                                     affected defumer or
                                                     coking oven.
4. Each new or existing       Minimize fuel-based   You use natural gas,
 chromium refractory           HAP emissions.        or equivalent, as
 products kiln.                                      the kiln fuel.
5. Each existing clay         Minimize fuel-based   You use natural gas,
 refractory products kiln.     HAP emissions.        or equivalent, as
                                                     the kiln fuel.
------------------------------------------------------------------------


[[Page 124]]

Table 7 to Subpart SSSSS of Part 63--Continuous Compliance with Emission 
                                 Limits

    As stated in Sec. 63.9810, you must show continuous compliance with 
the emission limits for affected sources according to the following 
table:

------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. Each affected source       a. Each applicable    i. Collecting and
 listed in Table 1 to this     emission limit        recording the
 subpart.                      listed in Table 1     monitoring and
                               to this subpart.      process data listed
                                                     in Table 2
                                                     (operating limits)
                                                     to this subpart;
                                                     and
                                                    ii. Reducing the
                                                     monitoring and
                                                     process data
                                                     associated with the
                                                     operating limits
                                                     specified in Table
                                                     2 to this subpart;
                                                     and
                                                    iii. Recording the
                                                     results of any
                                                     control device
                                                     inspections; and
                                                    iv. Reporting, in
                                                     accordance with
                                                     Sec. 63.9814(e),
                                                     any deviation from
                                                     the applicable
                                                     operating limits
                                                     specified in Table
                                                     2 to this subpart.
2. Each new or existing       As specified in       Satisfying the
 curing oven, shape dryer,     items 3 though 7 of   applicable
 and kiln that is used to      this table.           requirements
 process refractory products                         specified in items
 that use organic HAP; each                          3 through 7 of this
 new or existing coking oven                         table.
 and defumer that is used to
 produce pitch-impregnated
 refractory products; each
 new shape preheater that is
 used to produce pitch-
 impregnated refractory
 products; AND each new or
 existing process unit that
 is exhausted to a thermal
 or catalytic oxidizer that
 also controls emissions
 from an affected shape
 preheater or pitch working
 tank.
3. Each affected process      a. The average THC    i. Collecting the
 unit that is equipped with    concentration must    applicable data
 a thermal or catalytic        not exceed 20         measured by the
 oxidizer.                     ppmvd, corrected to   control device
                               18 percent oxygen;    temperature
                               OR the average THC    monitoring system,
                               percentage            as specified in
                               reduction must        items 5, 6, 8, and
                               equal or exceed 95    9 of Table 8 to
                               percent.              this subpart; and
                                                    ii. Reducing the
                                                     applicable data
                                                     measured by the
                                                     control device
                                                     temperature
                                                     monitoring system,
                                                     as specified in
                                                     items 5, 6, 8, and
                                                     9 of Table 8 to
                                                     this subpart; and
                                                    iii. Maintaining the
                                                     average control
                                                     device operating
                                                     temperature for the
                                                     applicable
                                                     averaging period
                                                     specified in items
                                                     5, 6, 8, and 9 of
                                                     Table 2 to this
                                                     subpart at or above
                                                     the minimum
                                                     allowable operating
                                                     temperature
                                                     established during
                                                     the most recent
                                                     performance test.
4. Each affected process      The average THC       Operating and
 unit that is equipped with    concentration must    maintaining a THC
 a control device other than   not exceed 20         CEMS at the outlet
 a thermal or catalytic        ppmvd, corrected to   of the control
 oxidizer.                     18 percent oxygen;    device or in the
                               OR the average THC    stack of the
                               performance           affected source,
                               reduction must        according to the
                               equal or exceed 95    requirements of
                               percent.              Procedure 1 of 40
                                                     CFR part 60,
                                                     appendix F.
5. Each affected process      The average THC       Operating and
 unit that uses process        concentration must    maintaining a THC
 changes to meet the           not exceed 20         CEMS at the outlet
 applicable emission limit.    ppmvd, corrected to   of the control
                               18 percent oxygen.    device or in the
                                                     stack of the
                                                     affected source,
                                                     according to the
                                                     requirements of
                                                     Procedure 1 of 40
                                                     CFR part 60,
                                                     appendix F.
6. Each affected continuous   The average THC       Recording the
 process unit.                 concentration must    organic HAP
                               not exceed 20         processing rate
                               ppmvd, corrected to   (pounds per hour)
                               18 percent oxygen;    and the operating
                               OR the average THC    temperature of the
                               percentage            affected source, as
                               reduction must        specified in items
                               equal or exceed 95    3.b. and 3.c. of
                               percent.              Table 4 to this
                                                     subpart.

[[Page 125]]

 
7. Each affected batch        The average THC       Recording the
 process unit.                 concentration must    organic HAP
                               not exceed 20         processing rate
                               ppmvd, corrected to   (pounds per batch);
                               18 percent oxygen;    and process cycle
                               OR the average THC    time for each batch
                               percentage            cycle; and hourly
                               reduction must        average operating
                               equal or exceed 95    temperature of the
                               percent.              affected source, as
                                                     specified in items
                                                     8.b. through 8.d.
                                                     of Table 4 to this
                                                     subpart.
8. Each kiln that is used to  As specified in       Satisfying the
 process clay refractory       items 9 through 11    applicable
 products.                     of this table.        requirements
                                                     specified in items
                                                     9 through 11 of
                                                     this table.
9. Each affected kiln that    a. The average HF     i. Maintaining the
 is equipped with a DLA.       emissions must not    pressure drop
                               exceed 0.019 kg/Mg    across the DLA at
                               (0.038 lb/ton) of     or above the
                               uncalcined clay       minimum levels
                               processed, OR the     established during
                               average               the most recent
                               uncontrolled HF       performance test;
                               emissions must be     and
                               reduced by at least  ii. Verifying that
                               90 percent; and       the limestone
                              b. The average HCl     hopper contains an
                               emissions must not    adequate amount of
                               exceed 0.091 kg/Mg    free-flowing
                               (0.18 lb/ton) of      limestone by
                               uncalcined clay       performing a daily
                               processed, or the     visual check of the
                               average               limestone in the
                               uncontrolled HCl      feed hopper; and
                               emissions must be    iii. Recording the
                               reduced by at least   limestone feeder
                               30 percent.           setting daily to
                                                     verify that the
                                                     feeder setting is
                                                     at or above the
                                                     level established
                                                     during the most
                                                     recent performance
                                                     test; and
                                                    iv. Using the same
                                                     grade of limestone
                                                     as was used during
                                                     the most recent
                                                     performance test
                                                     and maintaining
                                                     records of the
                                                     source and grade of
                                                     limestone.
10. Each affected kiln that   a. The average HF     i. Verifying at
 is equipped with a DIFF or    emissions must not    least once each 8-
 DLS/FF.                       exceed 0.019 kg/Mg    hour shift that
                               (0.038 lb/ton) of     lime is free-
                               uncalcined clay       flowing by means of
                               processed; OR the     a visual check,
                               average               checking the output
                               uncontrolled HF       of a load cell,
                               emissions must be     carrier gas/lime
                               reduced by at least   flow indicator, or
                               90 percent; and       carrier gas
                                                     pressure drop
                                                     measurement system;
                                                     and
                              b. The average HCl    ii. Recording feeder
                               emissions must not    setting daily to
                               exceed 0.091 kg/Mg    verify that the
                               (0.18 lb/ton) of      feeder setting is
                               uncalcined clay       at or above the
                               processed; OR the     level established
                               average               during the most
                               uncontrolled HCl      recent performance
                               emissions must be     test; and
                               reduced by at least
                               30 percent.
                                                    iii. Initiating
                                                     corrective action
                                                     within 1 hour of a
                                                     bag leak detection
                                                     system alarm AND
                                                     completing
                                                     corrective actions
                                                     in accordance with
                                                     the OM&M plan, AND
                                                     operating and
                                                     maintaining the
                                                     fabric filter such
                                                     that the alarm does
                                                     not engage for more
                                                     than 5 percent of
                                                     the total operating
                                                     time in a 6-month
                                                     block reporting
                                                     period.
11. Each affected kiln that   a. The average HF     i. Maintaining the
 is equipped with a wet        emissions must not    pressure drop
 scrubber.                     exceed 0.019 kg/Mg    across the
                               (0.038 lb/ton) of     scrubber, liquid
                               uncalcined clay       pH, and liquid flow
                               processed; OR the     rate at or above
                               average               the minimum levels
                               uncontrolled HF       established during
                               emissions must be     the most recent
                               reduced by at least   performance test;
                               90 percent; and       and
                              b. The average HCl    ii. If chemicals are
                               emissions must not    added to the
                               exceed 0.091 kg/Mg    scrubber liquid,
                               (0.18 lb/ton) of      maintaining the
                               uncalcined clay       average chemical
                               processed; OR the     feed rate at or
                               average               above the minimum
                               uncontrolled HCl      chemical feed rate
                               emissions must be     established during
                               reduced by at least   the most recent
                               30 percent.           performance test.
------------------------------------------------------------------------

    Table 8 to Subpart SSSSS of Part 63--Continuous Compliance with 
                            Operating Limits

    As stated in Sec. 63.9810, you must show continuous compliance with 
the operating limits for affected sources according to the following 
table:

[[Page 126]]



------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. Each affected source       a. Each applicable    i. Maintaining all
 listed in Table 2 to this     operating limit       applicable process
 subpart.                      listed in Table 2     and control device
                               to this subpart.      operating
                                                     parameters within
                                                     the limits
                                                     established during
                                                     the most recent
                                                     performance test;
                                                     and
                                                    ii. Conducting
                                                     annually an
                                                     inspection of all
                                                     duct work, vents,
                                                     and capture devices
                                                     to verify that no
                                                     leaks exist and
                                                     that the capture
                                                     device is operating
                                                     such that all
                                                     emissions are
                                                     properly vented to
                                                     the control device
                                                     in accordance with
                                                     the OM&M plan.
2. Each affected continuous   a. The operating      i. Operating the
 kiln that is equipped with    limits specified in   control device on
 a control device.             items 2.a. through    the affected kiln
                               2.c. of Table 2 to    during all times
                               this subpart.         except during
                                                     periods of approved
                                                     scheduled
                                                     maintenance, as
                                                     specified in Sec.
                                                     63.9792(e); and
                                                    ii. Minimizing HAP
                                                     emissions from the
                                                     affected kiln
                                                     during all periods
                                                     of scheduled
                                                     maintenance of the
                                                     kiln control device
                                                     when the kiln is
                                                     operating and the
                                                     control device is
                                                     out of service; and
                                                    iii. Minimizing the
                                                     duration of all
                                                     periods of
                                                     scheduled
                                                     maintenance of the
                                                     kiln control device
                                                     when the kiln is
                                                     operating and the
                                                     control device is
                                                     out of service.
3. Each new or existing       As specified in       Satisfying the
 curing oven, shape dryer,     items 4 through 9     applicable
 and kiln that is used to      of this table.        requirements
 process refractory products                         specified in items
 that use organic HAP; each                          4 through 9 of this
 new or existing coking oven                         table.
 and defumer that is used to
 produce pitch-impregnated
 refractory products; each
 new shape preheater that is
 used to produce pitch-
 impregnated refractory
 products; AND each new or
 existing process unit that
 is exhausted to a thermal
 or catalytic oxidizer that
 also controls emissions
 from an affected shape
 preheater or pitch working
 tank.
4. Each affected continuous   Maintain process      i. Recording the
 process unit.                 operating             organic HAP
                               parameters within     processing rate
                               the limits            (pounds per hour);
                               established during    and
                               the most recent      ii. Recording the
                               performance test.     operating
                                                     temperature of the
                                                     affected source at
                                                     least hourly; and
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average organic HAP
                                                     processing rate at
                                                     or below the
                                                     maximum organic HAP
                                                     processing rate
                                                     established during
                                                     the most recent
                                                     performance test.
5. Continuous process units   Maintain the 3-hour   i. Measuring and
 that are equipped with a      block average         recording the
 thermal oxidizer.             operating             thermal oxidizer
                               temperature in the    combustion chamber
                               thermal oxidizer      temperature at
                               combustion chamber    least every 15
                               at or above the       minutes; and
                               minimum allowable    ii. Calculating the
                               operating             hourly average
                               temperature           thermal oxidizer
                               established during    combustion chamber
                               the most recent       temperature; and
                               performance test.    iii. Maintaining the
                                                     3-hour block
                                                     average thermal
                                                     oxidizer combustion
                                                     chamber temperature
                                                     at or above the
                                                     minimum allowable
                                                     operating
                                                     temperature
                                                     established during
                                                     the most recent
                                                     performance test;
                                                     and
                                                    iv. Reporting, in
                                                     accordance with
                                                     Sec. 63.9814(e),
                                                     any 3-hour block
                                                     average operating
                                                     temperature
                                                     measurements below
                                                     the minimum
                                                     allowable thermal
                                                     oxidizer combustion
                                                     chamber operating
                                                     temperature
                                                     established during
                                                     the most recent
                                                     performance test.

[[Page 127]]

 
6. Continuous process units   a. Maintain the 3-    i. Measuring and
 that are equipped with a      hour block average    recording the
 catalytic oxidizer.           temperature at the    temperature at the
                               inlet of the          inlet of the
                               catalyst bed at or    catalyst bed at
                               above the minimum     least every 15
                               allowable catalyst    minutes; and
                               bed inlet            ii. Calculating the
                               temperature           hourly average
                               established during    temperature at the
                               the most recent       inlet of the
                               performance test.     catalyst bed; and
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average temperature
                                                     at the inlet of the
                                                     catalyst bed at or
                                                     above the minimum
                                                     allowable catalyst
                                                     bed inlet
                                                     temperature
                                                     established during
                                                     the most recent
                                                     performance test;
                                                     and
                                                    iv. Reporting, in
                                                     accordance with
                                                     Sec. 63.9814(e),
                                                     any 3-hour block
                                                     average catalyst
                                                     bed inlet
                                                     temperature
                                                     measurements below
                                                     the minimum
                                                     allowable catalyst
                                                     bed inlet
                                                     temperature
                                                     established during
                                                     the most recent
                                                     performance; and
                                                    v. Checking the
                                                     activity level of
                                                     the catalyst at
                                                     least every 12
                                                     months and taking
                                                     any necessary
                                                     corrective action,
                                                     such as replacing
                                                     the catalyst, to
                                                     ensure that the
                                                     catalyst is
                                                     performing as
                                                     designed.
7. Each affected batch        Maintain process      i. Recording the
 process unit.                 operating             organic HAP
                               parameters within     processing rate
                               the limits            (pounds per batch);
                               established during    and
                               the most recent      ii. Recording the
                               performance test.     hourly average
                                                     operating
                                                     temperature of the
                                                     affected source;
                                                     and
                                                    iii. Recording the
                                                     process cycle time
                                                     for each batch
                                                     cycle; and
                                                    iv. Maintaining the
                                                     organic HAP
                                                     processing rate at
                                                     or below the
                                                     maximum organic HAP
                                                     processing rate
                                                     established during
                                                     the most recent
                                                     performance test.
8. Batch process units that   Maintain the hourly   i. Measuring and
 are equipped with a thermal   average temperature   recording the
 oxidizer.                     in the thermal        thermal oxidizer
                               oxidizer combustion   combustion chamber
                               chamber at or above   temperature at
                               the hourly average    least every 15
                               temperature           minutes; and
                               established for the  ii. Calculating the
                               corresponding 1-      hourly average
                               hour period of the    thermal oxidizer
                               cycle during the      combustion chamber
                               most recent           temperature; and
                               performance test.    iii. From the start
                                                     of each batch cycle
                                                     until 3 hours have
                                                     passed since the
                                                     process unit
                                                     reached maximum
                                                     temperature,
                                                     maintaining the
                                                     hourly average
                                                     operating
                                                     temperature in the
                                                     thermal oxidizer
                                                     combustion chamber
                                                     at or above the
                                                     minimum allowable
                                                     operating
                                                     temperature
                                                     established for the
                                                     corresponding
                                                     period during the
                                                     most recent
                                                     performance test,
                                                     as determined
                                                     according to item
                                                     11 of Table 4 to
                                                     this subpart; and
                                                    iv. For each
                                                     subsequent hour of
                                                     the batch cycle,
                                                     maintaining the
                                                     hourly average
                                                     operating
                                                     temperature in the
                                                     thermal oxidizer
                                                     combustion chamber
                                                     at or above the
                                                     minimum allowable
                                                     operating
                                                     temperature
                                                     established for the
                                                     corresponding hour
                                                     during the most
                                                     recent performance
                                                     test, as specified
                                                     in item 13 of Table
                                                     4 to this subpart;
                                                     and
                                                    v. Reporting, in
                                                     accordance with
                                                     Sec. 63.9814(e),
                                                     any temperature
                                                     measurements below
                                                     the minimum
                                                     allowable thermal
                                                     oxidizer combustion
                                                     chamber temperature
                                                     measured during the
                                                     most recent
                                                     performance test.

[[Page 128]]

 
9. Batch process units that   Maintain the hourly   i. Measuring and
 are equipped with a           average temperature   recording
 catalytic oxidizer.           at the inlet of the   temperatures at the
                               catalyst bed at or    inlet of the
                               above the             catalyst bed at
                               corresponding         least every 15
                               hourly average        minutes; and
                               temperature          ii. Calculating the
                               established for the   hourly average
                               corresponding 1-      temperature at the
                               hour period of the    inlet of the
                               cycle during the      catalyst bed; and
                               most recent          iii. From the start
                               performance test.     of each batch cycle
                                                     until 3 hours have
                                                     passed since the
                                                     process unit
                                                     reached maximum
                                                     temperature,
                                                     maintaining the
                                                     hourly average
                                                     operating
                                                     temperature at the
                                                     inlet of the
                                                     catalyst bed at or
                                                     above the minimum
                                                     allowable bed inlet
                                                     temperature
                                                     established for the
                                                     corresponding
                                                     period during the
                                                     most recent
                                                     performance test,
                                                     as determined
                                                     according to item
                                                     12 of Table 4 to
                                                     this subpart; and
                                                    iv. For each
                                                     subsequent hour of
                                                     the batch cycle,
                                                     maintaining the
                                                     hourly average
                                                     operating
                                                     temperature at the
                                                     inlet of the
                                                     catalyst bed at or
                                                     above the minimum
                                                     allowable bed inlet
                                                     temperature
                                                     established for the
                                                     corresponding hour
                                                     during the most
                                                     recent performance
                                                     test, as specified
                                                     in item 13 of Table
                                                     4 to this subpart;
                                                     and
                                                    v. Reporting, in
                                                     accordance with
                                                     Sec. 63.9814(e),
                                                     any catalyst bed
                                                     inlet temperature
                                                     measurements below
                                                     the minimum
                                                     allowable bed inlet
                                                     temperature
                                                     measured during the
                                                     most recent
                                                     performance test;
                                                     and
                                                    vi. Checking the
                                                     activity level of
                                                     the catalyst at
                                                     least every 12
                                                     months and taking
                                                     any necessary
                                                     corrective action,
                                                     such as replacing
                                                     the catalyst, to
                                                     ensure that the
                                                     catalyst is
                                                     performing as
                                                     designed.
10. Each new kiln that is     As specified in       Satisfying the
 used to process clay          items 11 through 13   applicable
 refractory products.          of this table.        requirements
                                                     specified in items
                                                     11 through 13 of
                                                     this table.
11. Each new kiln that is     a. Maintain the       i. Collecting the
 equipped a DLA.               average pressure      DLA pressure drop
                               drop across the DLA   data, as specified
                               for each 3-hour       in item 18.a. of
                               block period at or    Table 4 to this
                               above the minimum     subpart; and
                               pressure drop        ii. Reducing the DLA
                               established during    pressure drop data
                               the most recent       to 1-hour and 3-
                               performance test.     hour block
                                                     averages; and
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average pressure
                                                     drop across the DLA
                                                     at or above the
                                                     minimum pressure
                                                     drop established
                                                     during the most
                                                     recent performance
                                                     test.
                              b. Maintain free-     Verifying that the
                               flowing limestone     limestone hopper
                               in the feed hopper,   has an adequate
                               silo, and DLA.        amount of free-
                                                     flowing limestone
                                                     by performing a
                                                     daily visual check
                                                     of the limestone
                                                     hopper.
                              c. Maintain the       Recording the
                               limestone feeder      limestone feeder
                               setting at or above   setting at least
                               the level             daily to verify
                               established during    that the feeder
                               the most recent       setting is being
                               performance test.     maintained at or
                                                     above the level
                                                     established during
                                                     the most recent
                                                     performance test.
                              d. Use the same       Using the same grade
                               grade of limestone    of limestone as was
                               from the same         used during the
                               source as was used    most recent
                               during the most       performance test
                               recent performance    and maintaining
                               test.                 records of the
                                                     source and grade of
                                                     limestone.

[[Page 129]]

 
12. Each new kiln that is     a. Initiate           i. Initiating
 equipped with a DIFF or DLS/  corrective action     corrective action
 FF.                           within 1 hour of a    within 1 hour of a
                               bag leak detection    bag leak detection
                               system alarm and      system alarm and
                               complete corrective   completing
                               actions in            corrective actions
                               accordance with the   in accordance with
                               OM&M plan; AND        the OM&M plan; and
                               operate and          ii. Operating and
                               maintain the fabric   maintaining the
                               filter such that      fabric filter such
                               the alarm does not    that the alarm does
                               engage for more       not engage for more
                               than 5 percent of     than 5 percent of
                               the total operating   the total operating
                               time in a 6-month     time in a 6-month
                               block reporting       block reporting
                               period.               period; in
                                                     calculating this
                                                     operating time
                                                     fraction, if
                                                     inspection of the
                                                     fabric filter
                                                     demonstrates that
                                                     no corrective
                                                     action is required,
                                                     no alarm time is
                                                     counted; if
                                                     corrective action
                                                     is required, each
                                                     alarm shall be
                                                     counted as a
                                                     minimum of 1 hour;
                                                     if you take longer
                                                     than 1 hour to
                                                     initiate corrective
                                                     action, the alarm
                                                     time shall be
                                                     counted as the
                                                     actual amount of
                                                     time taken by you
                                                     to initiate
                                                     corrective action.
                              b. Maintain free-     i. Verifying at
                               flowing lime in the   least once each 8-
                               feed hopper or silo   hour shift that
                               at all times for      lime is free-
                               continuous            flowing via a load
                               injection systems;    cell, carrier gas/
                               AND maintain feeder   lime flow
                               setting at or above   indicator, carrier
                               the level             gas pressure drop
                               established during    measurement system,
                               the most recent       or other system;
                               performance test      recording all
                               for continuous        monitor or sensor
                               injection systems.    output, and if lime
                                                     is found not to be
                                                     free flowing,
                                                     promptly initiating
                                                     and completing
                                                     corrective actions;
                                                     and
                                                    ii. Recording the
                                                     feeder setting once
                                                     each day of
                                                     operation to verify
                                                     that the feeder
                                                     setting is being
                                                     maintained at or
                                                     above the level
                                                     established during
                                                     the most recent
                                                     performance test.
13. Each new kiln that is     a. Maintain the       i. Collecting the
 used to process clay          average pressure      scrubber pressure
 refractory products and is    drop across the       drop data, as
 equipped with a wet           scrubber for each 3-  specified in item
 scrubber.                     hour block period     20.a. of Table 4 to
                               at or above the       this subpart; and
                               minimum pressure     ii. Reducing the
                               drop established      scrubber pressure
                               during the most       drop data to 1-hour
                               recent performance    and 3-hour block
                               test.                 averages; and
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average scrubber
                                                     pressure drop at or
                                                     above the minimum
                                                     pressure drop
                                                     established during
                                                     the most recent
                                                     performance test.
                              b. Maintain the       i. Collecting the
                               average scrubber      scrubber liquid pH
                               liquid pH for each    data, as specified
                               3-hour block period   in item 20.b. of
                               at or above the       Table 4 to this
                               minimum scrubber      subpart; and
                               liquid pH            ii. Reducing the
                               established during    scrubber liquid pH
                               the most recent       data to 1-hour and
                               performance test.     3-hour block
                                                     averages; and
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average scrubber
                                                     liquid pH at or
                                                     above the minimum
                                                     scrubber liquid pH
                                                     established during
                                                     the most recent
                                                     performance test.
                              c. Maintain the       i. Collecting the
                               average scrubber      scrubber liquid
                               liquid flow rate      flow rate data, as
                               for each 3-hour       specified in item
                               block period at or    20.c. of Table 4 to
                               above the minimum     this subpart; and
                               scrubber liquid      ii. Reducing the
                               flow rate             scrubber liquid
                               established during    flow rate data to 1-
                               the most recent       hour and 3-hour
                               performance test.     block averages; and
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average scrubber
                                                     liquid flow rate at
                                                     or above the
                                                     minimum scrubber
                                                     liquid flow rate
                                                     established during
                                                     the most recent
                                                     performance test.
                              d. If chemicals are   i. Collecting the
                               added to the          scrubber chemical
                               scrubber liquid,      feed rate data, as
                               maintain the          specified in item
                               average scrubber      20.d. of Table 4 to
                               chemical feed rate    this subpart; and
                               for each 3-hour      ii. Reducing the
                               block period at or    scrubber chemical
                               above the minimum     feed rate data to 1-
                               scrubber chemical     hour and 3-hour
                               feed rate             block averages; and
                               established during
                               the most recent
                               performance test.

[[Page 130]]

 
                                                    iii. Maintaining the
                                                     3-hour block
                                                     average scrubber
                                                     chemical feed rate
                                                     at or above the
                                                     minimum scrubber
                                                     chemical feed rate
                                                     established during
                                                     the most recent
                                                     performance test.
------------------------------------------------------------------------

  Table 9 to Subpart SSSSS of Part 63--Continuous Compliance with Work 
                           Practice Standards

    As stated in Sec. 63.9810, you must show continuous compliance with 
the work practice standards for affected sources according to the 
following table:

------------------------------------------------------------------------
 
 
 
 
------------------------------------------------------------------------
1. Each affected source       Each applicable work  i. Performing each
 listed in Table 3 to this     practice              applicable work
 subpart.                      requirement listed    practice standard
                               in Table 3 to this    listed in Table 3
                               subpart.              to this subpart;
                                                     and
                                                    ii. Maintaining
                                                     records that
                                                     document the method
                                                     and frequency for
                                                     complying with each
                                                     applicable work
                                                     practice standard
                                                     listed in Table 3
                                                     to this subpart, as
                                                     required by Sec.
                                                     Sec. 63.10(b) and
                                                     63.9816(c)(2).
2. Each basket or container   Control POM           i. Controlling
 that is used for holding      emissions from any    emissions from the
 fired refractory shapes in    affected shape        volatilization of
 an existing shape preheater   preheater.            residual pitch by
 and autoclave during the                            implementing one of
 pitch impregnation process.                         the work practice
                                                     standards listed in
                                                     item 1 of Table 3
                                                     to this subpart;
                                                     and
                                                    ii. Recording the
                                                     date and cleaning
                                                     method each time
                                                     you clean an
                                                     affected basket or
                                                     container.
3. Each new or existing       Control POM           Capturing and
 pitch working tank.           emissions.            venting emissions
                                                     from the affected
                                                     pitch working tank
                                                     to the control
                                                     device that is used
                                                     to control
                                                     emissions from an
                                                     affected defumer or
                                                     coking oven, or to
                                                     a thermal or
                                                     catalytic oxidizer
                                                     that is comparable
                                                     to the control
                                                     device used on an
                                                     affected defumer or
                                                     coking oven.
4. Each new or existing       Minimize fuel-based   i. Using natural
 chromium refractory           HAP emissions.        gas, or equivalent,
 products kiln.                                      as the kiln fuel at
                                                     all times except
                                                     during periods of
                                                     natural gas
                                                     curtailment or
                                                     supply
                                                     interruption; and
                                                    ii. If you intend to
                                                     use an alternative
                                                     fuel, submitting a
                                                     notification of
                                                     alternative fuel
                                                     use within 48 hours
                                                     of the declaration
                                                     of a per-iod of
                                                     natural gas
                                                     curtailment or
                                                     supply
                                                     interruption, as
                                                     defined in Sec.
                                                     63.9824; and
                                                    iii. Submitting a
                                                     report of
                                                     alternative fuel
                                                     use within 10
                                                     working days after
                                                     terminating the use
                                                     of the alternative
                                                     fuel, as specified
                                                     in Sec.
                                                     63.9814(g).
5. Each existing clay         Minimize fuel-based   i. Using natural
 refractory products kiln.     HAP emissions.        gas, or equivalent,
                                                     as the kiln fuel at
                                                     all times except
                                                     during periods of
                                                     natural gas
                                                     curtailment or
                                                     supply
                                                     interruption; and
                                                    ii. If you intend to
                                                     use an alternative
                                                     fuel, submitting a
                                                     notification of
                                                     alternative fuel
                                                     use within 48 hours
                                                     of the declaration
                                                     of a per-iod of
                                                     natural gas
                                                     curtailment or
                                                     supply
                                                     interruption, as
                                                     defined in Sec.
                                                     63.9824; and
                                                    iii. Submitting a
                                                     report of
                                                     alternative fuel
                                                     use within 10
                                                     working days after
                                                     terminating the use
                                                     of the alternative
                                                     fuel, as specified
                                                     in Sec.
                                                     63.9814(g).
------------------------------------------------------------------------


[[Page 131]]

     Table 10 to Subpart SSSSS of Part 63--Requirements for Reports

    As stated in Sec. 63.9814, you must comply with the requirements 
for reports in the following table:

------------------------------------------------------------------------
 
 
------------------------------------------------------------------------
1. Compliance report........  The information in    Semiannually
                               Sec. 63.9814(c)     according to the
                               through (f).          requirements in
                                                     Sec. 63.9814(a)
                                                     through (f).
2. Immediate startup,         a. Actions taken for  By fax or telephone
 shutdown, and malfunction     the event.            within 2 working
 report if you had a                                 days after starting
 startup, shutdown, or                               actions
 malfunction during the                              inconsistent with
 reporting period that is                            the plan.
 not consistent with your
 SSMP.
                              b. The information    By letter within 7
                               in Sec. working days after
                               63.10(d)(5)(ii).      the end of the
                                                     event unless you
                                                     have made
                                                     alternative
                                                     arrangements with
                                                     the permitting
                                                     authority.
3. Report of alternative      The information in    If you are subject
 fuel use.                     Sec. 63.9814(g)     to the work
                               and items 4 and 5     practice standard
                               of Table 9 to this    specified in item 3
                               subpart.              or 4 of Table 3 to
                                                     this subpart, and
                                                     you use an
                                                     alternative fuel in
                                                     the affected kiln,
                                                     by letter within 10
                                                     working days after
                                                     terminating the use
                                                     of the alternative
                                                     fuel.
------------------------------------------------------------------------

     Table 11 to Subpart SSSSS of Part 63--Applicability of General 
                       Provisions to Subpart SSSSS

    As stated in Sec. 63.9820, you must comply with the applicable 
General Provisions requirements according to the following table:

----------------------------------------------------------------------------------------------------------------
                                                                                             Applies to subpart
             Citation                         Subject                Brief description              SSSSS
----------------------------------------------------------------------------------------------------------------
Sec. 63.1.......................  Applicability.............  ..........................  Yes.
Sec. 63.2.......................  Definitions...............  ..........................  Yes.
Sec. 63.3.......................  Units and Abbreviations...  ..........................  Yes.
Sec. 63.4.......................  Prohibited Activities.....  Compliance date;            Yes.
                                                                 circumvention,
                                                                 severability.
Sec. 63.5.......................  Construction/               Applicability;              Yes.
                                     Reconstruction.             applications; approvals.
Sec. 63.6(a)....................  Applicability.............  General Provisions (GP)     Yes.
                                                                 apply unless compliance
                                                                 extension; GP apply to
                                                                 area sources that become
                                                                 major.
Sec. 63.6(b)(1)-(4).............  Compliance Dates for New    Standards apply at          Yes.
                                     and Reconstructed Sources.  effective date; 3 years
                                                                 after effective date;
                                                                 upon startup; 10 years
                                                                 after construction or
                                                                 reconstruction commences
                                                                 for section 112(f).
Sec. 63.6(b)(5).................  Notification..............  ..........................  Yes.
Sec. 63.6(b)(6).................  [Reserved]                                              ....................
Sec. 63.6(b)(7).................  Compliance Dates for New    Area sources that become    Yes.
                                     and Reconstructed Area      major must comply with
                                     Sources That Become Major.  major source standards
                                                                 immediately upon becoming
                                                                 major, regardless of
                                                                 whether required to
                                                                 comply when they were
                                                                 area sources.
Sec. 63.6(c)(1)-(2).............  Compliance Dates for        Comply according to date    Yes.
                                     Existing Sources.           in subpart, which must be
                                                                 no later than 3 years
                                                                 after effective date; for
                                                                 section 112(f) standards,
                                                                 comply within 90 days of
                                                                 effective date unless
                                                                 compliance extension.
Sec. 63.6(c)(3)-(4).............  [Reserved]                                              ....................
Sec. 63.6(c)(5).................  Compliance Dates for        Area sources that become    Yes.
                                     Existing Area Sources       major must comply with
                                     That Become Major.          major source standards by
                                                                 date indicated in subpart
                                                                 or by equivalent time
                                                                 period (for example, 3
                                                                 years).
Sec. 63.6(d)....................  [Reserved]                                              ....................
Sec. 63.6(e)(1)-(2).............  Operation & Maintenance...  Operate to minimize         Yes.
                                                                 emissions at all times;
                                                                 correct malfunctions as
                                                                 soon as practicable;
                                                                 requirements
                                                                 independently
                                                                 enforceable; information
                                                                 Administrator will use to
                                                                 determine if operation
                                                                 and maintenance
                                                                 requirements were met.

[[Page 132]]

 
Sec. 63.6(e)(3).................  Startup, Shutdown, and      ..........................  Yes.
                                     Malfunction Plan (SSMP).
Sec. 63.6(f)(1).................  Compliance Except During    You must comply with        Yes.
                                     SSM.                        emission standards at all
                                                                 times except during SSM.
Sec. 63.6(f)(2)-(3).............  Methods for Determining     Compliance based on         Yes.
                                     Compliance.                 performance test,
                                                                 operation and maintenance
                                                                 plans, records,
                                                                 inspection.
Sec. 63.6(g)(1)-(3).............  Alternative Standard......  Procedures for getting an   Yes.
                                                                 alternative standard.
Sec. 63.6(h)(1)-(9).............  Opacity/Visible Emission    ..........................  Not applicable.
                                     (VE) Standards.
Sec. 63.6(i)(1)-(14)............  Compliance Extension......  Procedures and criteria     Yes.
                                                                 for Administrator to
                                                                 grant compliance
                                                                 extension.
Sec. 63.6(j)....................  Presidential Compliance     President may exempt        Yes.
                                     Exemption.                  source category.
Sec. 63.7(a)(1)-(2).............  Performance Test Dates....  Dates for conducting        Yes.
                                                                 initial performance
                                                                 testing and other
                                                                 compliance
                                                                 demonstrations; must
                                                                 conduct 180 days after
                                                                 first subject to rule.
Sec. 63.7(a)(3).................  Section 114 Authority.....  Administrator may require   Yes.
                                                                 a performance test under
                                                                 CAA section 114 at any
                                                                 time.
Sec. 63.7(b)(1).................  Notification of             Must notify Administrator   Yes.
                                     Performance Test.           60 days before the test.
Sec. 63.7(b)(2).................  Notification of             Must notify Administrator   Yes.
                                     Rescheduling.               5 days before scheduled
                                                                 date and provide
                                                                 rescheduled date.
Sec. 63.7(c)....................  Quality Assurance/Test      Requirements; test plan     Yes.
                                     Plan.                       approval procedures;
                                                                 performance audit
                                                                 requirements; internal
                                                                 and external QA
                                                                 procedures for testing.
Sec. 63.7(d)....................  Testing Facilities........  ..........................  Yes.
Sec. 63.7(e)(1).................  Conditions for Conducting   Performance tests must be   No, Sec. 63.9800
                                     Performance Tests.          conducted under             specifies
                                                                 representative              requirements; Yes;
                                                                 conditions; cannot          Yes.
                                                                 conduct performance tests
                                                                 during SSM; not a
                                                                 violation to exceed
                                                                 standard during SSM.
Sec. 63.7(e)(2).................  Conditions for Conducting   Must conduct according to   Yes.
                                     Performance Tests.          subpart and EPA test
                                                                 methods unless
                                                                 Administrator approves
                                                                 alternative.
Sec. 63.7(e)(3).................  Test Run Duration.........  Must have three test runs   Yes; Yes, except
                                                                 of at least 1 hour each;    where specified in
                                                                 compliance is based on      Sec. 63.9800 for
                                                                 arithmetic mean of three    batch process
                                                                 runs; conditions when       sources; Yes.
                                                                 data from an additional
                                                                 test run can be used.
Sec. 63.7(f)....................  Alternative Test Method...  ..........................  Yes.
Sec. 63.7(g)....................  Performance Test Data       ..........................  Yes.
                                     Analysis.
Sec. 63.7(h)....................  Waiver of Test............  ..........................  Yes.
Sec. 63.8(a)(1).................  Applicability of            ..........................  Yes.
                                     Monitoring Requirements.
Sec. 63.8(a)(2).................  Performance Specifications  Performance Specifications  Yes.
                                                                 in appendix B of 40 CFR
                                                                 part 60 apply.
Sec. 63.8(a)(3).................  [Reserved]
Sec. 63.8(a)(4).................  Monitoring with Flares....  ..........................  Not applicable.
Sec. 63.8(b)(1).................  Monitoring................  Must conduct monitoring     Yes.
                                                                 according to standard
                                                                 unless Administrator
                                                                 approves alternative.
Sec. 63.8(b)(2)-(3).............  Multiple Effluents and      Specific requirements for   Yes.
                                     Multiple Monitoring         installing and reporting
                                     Systems.                    on monitoring systems.
Sec. 63.8(c)(1).................  Monitoring System           Maintenance consistent      Yes.
                                     Operation and Maintenance.  with good air pollution
                                                                 control practices.
Sec. 63.8(c)(1)(i)..............  Routine and Predictable     Reporting requirements for  Yes.
                                     SSM.                        SSM when action is
                                                                 described in SSMP.
Sec. 63.8(c)(1)(ii).............  SSM not in SSMP...........  Reporting requirements for  Yes.
                                                                 SSM when action is not
                                                                 described in SSMP.
Sec. 63.8(c)(1)(iii)............  Compliance with Operation   How Administrator           Yes.
                                     and Maintenance             determines if source is
                                     Requirements.               complying with operation
                                                                 and maintenance
                                                                 requirements.
Sec. 63.8(c)(2)-(3).............  Monitoring System           Must install to get         Yes.
                                     Installation.               representative emission
                                                                 and parameter
                                                                 measurements.
Sec. 63.8(c)(4).................  CMS Requirements..........  ..........................  No, Sec. 63.9808
                                                                                             specifies
                                                                                             requirements.
Sec. 63.8(c)(5).................  COMS Minimum Procedures...  ..........................  Not applicable.
Sec. 63.8(c)(6).................  CMS Requirements..........  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.

[[Page 133]]

 
Sec. 63.8(c)(7)(i)(A)...........  CMS Requirements..........  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.8(c)(7)(i)(B)...........  CMS Requirements..........  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.8(c)(7)(i)(C)...........  CMS Requirements..........  ..........................  Not applicable.
Sec. 63.8(c)(7)(ii).............  CMS Requirements..........  Corrective action required  Yes.
                                                                 when CMS is out of
                                                                 control.
Sec. 63.8(c)(8).................  CMS Requirements..........  ..........................  Yes.
Sec. 63.8(d)....................  CMS Quality Control.......  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.8(e)....................  CMS Performance Evaluation  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.8(f)(1)-(5).............  Alternative Monitoring      ..........................  Yes.
                                     Method.
Sec. 63.8(f)(6).................  Alternative to Relative     ..........................  Yes.
                                     Accuracy Test.
Sec. 63.8(g)....................  Data Reduction............  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.9(a)....................  Notification Requirements.  ..........................  Yes.
Sec. 63.9(b)(1)-(5).............  Initial Notifications.....  ..........................  Yes.
Sec. 63.9(c)....................  Request for Compliance      ..........................  Yes.
                                     Extension.
Sec. 63.9(d)....................  Notification of Special     ..........................  Yes.
                                     Compliance Requirements
                                     for New Source.
Sec. 63.9(e)....................  Notification of             Notify Administrator 60     Yes.
                                     Performance Test.           days prior.
Sec. 63.9(f)....................  Notification of VE/Opacity  ..........................  Not applicable.
                                     Test.
Sec. 63.9(g)....................  Additional Notifications    ..........................  Applies only to
                                     When Using CMS.                                         sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.9(h)....................  Notification of Compliance  ..........................  Yes.
                                     Status.
Sec. 63.9(i)....................  Adjustment of Submittal     ..........................  Yes.
                                     Deadlines.
Sec. 63.9(j)....................  Change in Previous          ..........................  Yes.
                                     Information.
Sec. 63.10(a)...................  Recordkeeping/Reporting...  ..........................  Yes.
Sec. 63.10(b)(1)................  Recordkeeping/Reporting...  ..........................  Yes.
Sec. 63.10(b)(2)(i)-(v).........  Records Related to          ..........................  Yes.
                                     Startup, Shutdown, and
                                     Malfunction.
Sec. 63.10(b)(2)(vi) and (x-xi).  CMS Records...............  ..........................  Yes.
Sec. 63.10(b)(2)(vii)-(ix)......  Records...................  Measurements to             Yes.
                                                                 demonstrate compliance
                                                                 with emission
                                                                 limitations; performance
                                                                 test, performance
                                                                 evaluation, and visible
                                                                 emission observation
                                                                 results; measurements to
                                                                 determine conditions of
                                                                 performance tests and
                                                                 performance evaluations.
Sec. 63.10(b)(2)(xii)...........  Records...................  Records when under waiver.  Yes.
Sec. 63.10(b)(2)(xiii)..........  Records...................  Records when using          Not applicable.
                                                                 alternative to relative
                                                                 accuracy test.
Sec. 63.10(b)(2)(xiv)...........  Records...................  All documentation           Yes.
                                                                 supporting Initial
                                                                 Notification and
                                                                 Notification of
                                                                 Compliance Status.
Sec. 63.10(b)(3)................  Records...................  Applicability               Yes.
                                                                 Determinations.
Sec. 63.10(c)(1)-(6), (9)-(15)..  Records...................  Additional Records for CMS  Not applicable.
Sec. 63.10(c)(7)-(8)............  Records...................  Records of excess           No, Sec. 63.9816
                                                                 emissions and parameter     specifies
                                                                 monitoring exceedances      requirements.
                                                                 for CMS.
Sec. 63.10(d)(1)................  General Reporting           Requirements for reporting  Yes.
                                     Requirements.
Sec. 63.10(d)(2)................  Report of Performance Test  When to submit to Federal   Yes.
                                     Results.                    or State authority.
Sec. 63.10(d)(3)................  Reporting Opacity or VE     ..........................  Not applicable.
                                     Observations.
Sec. 63.10(d)(4)................  Progress Reports..........  Must submit progress        Yes.
                                                                 reports on schedule if
                                                                 under compliance
                                                                 extension.
Sec. 63.10(d)(5)................  Startup, Shutdown, and      Contents and submission...  Yes.
                                     Malfunction Reports.

[[Page 134]]

 
Sec. 63.10(e)(1)-(2)............  Additional CMS Reports....  ..........................  Applies only to
                                                                                             sources required to
                                                                                             install and operate
                                                                                             a THC CEMS.
Sec. 63.10(e)(3)................  Reports...................  ..........................  No, Sec. 63.9814
                                                                                             specifies
                                                                                             requirements.
Sec. 63.10(e)(4)................  Reporting COMS data.......  ..........................  Not applicable.
Sec. 63.10(f)...................  Waiver for Recordkeeping/   ..........................  Yes.
                                     Reporting.
Sec. 63.11......................  Flares....................  ..........................  Not applicable.
Sec. 63.12......................  Delegation................  ..........................  Yes.
Sec. 63.13......................  Addresses.................  ..........................  Yes.
Sec. 63.14......................  Incorporation by Reference  ..........................  Yes.
Sec. 63.15......................  Availability of             ..........................  Yes.
                                     Information.
----------------------------------------------------------------------------------------------------------------

Subpart TTTTT_National Emissions Standards for Hazardous Air Pollutants 
                     for Primary Magnesium Refining

    Source: 68 FR 58620, Oct. 10, 2003, unless otherwise noted.

                        What This Subpart Covers



Sec. 63.9880  What is the purpose of this subpart?

    This subpart establishes national emission standards for hazardous 
air pollutants (NESHAP) for primary magnesium refineries. This subpart 
also establishes requirements to demonstrate initial and continuous 
compliance with all applicable emission limitations, work practice 
standards, and operation and maintenance requirements.



Sec. 63.9881  Am I subject to this subpart?

    You are subject to this subpart if you own or operate a primary 
magnesium refinery that is (or is part of) a major source of hazardous 
air pollutant (HAP) emissions. Your primary magnesium refinery is a 
major source of HAP if it emits or has the potential to emit any single 
HAP at a rate of 10 tons or more per year or any combination of HAP at a 
rate of 25 tons or more per year.



Sec. 63.9882  What parts of my plant does this subpart cover?

    (a) The affected sources are each new and existing primary magnesium 
refining facility.
    (b) This subpart covers emissions from each spray dryer stack, 
magnesium chloride storage bins scrubber stack, melt/reactor system 
stack, and launder off-gas system stack at your primary magnesium 
refining facility. This subpart also covers fugitive dust emissions.
    (c) Each primary magnesium refining facility is existing if you 
commenced construction or reconstruction of the affected source before 
January 22, 2003.
    (d) Each primary magnesium refining facility is new if you commence 
construction or reconstruction of the affected source on or after 
January 22, 2003. An affected source is reconstructed if it meets the 
definition of reconstruction in Sec. 63.2.



Sec. 63.9883  When do I have to comply with this subpart?

    (a) If you have an existing source, you must comply with each 
emission limitation, work practice standard, and operation and 
maintenance requirement in this subpart that applies to you no later 
than October 11, 2004.
    (b) If you have a new affected source and its initial startup date 
is on or before October 11, 2003, you must comply with each emission 
limitation, work practice standard, and operation and maintenance 
requirement in this subpart that applies to you by October 10, 2003.
    (c) If you have a new affected source and its initial startup date 
is after October 10, 2003, you must comply with each emission 
limitation, work practice standard, and operation and maintenance 
requirement in this subpart that applies to you upon initial startup.
    (d) If your primary magnesium refinery is an area source that 
becomes a major source of HAP, the compliance

[[Page 135]]

dates in paragraphs (d)(1) and (2) of this section apply to you:
    (1) Any portion of the existing primary magnesium refinery that is a 
new affected source or a new reconstructed source must be in compliance 
with this subpart upon startup.
    (2) All other parts of the primary magnesium refinery must be in 
compliance with this subpart no later than 2 years after it becomes a 
major source.
    (e) You must meet the notification and schedule requirements in 
Sec. 63.9930. Several of these notifications must be submitted before 
the compliance date for your affected source.

            Emission Limitations and Work Practice Standards



Sec. 63.9890  What emission limitations must I meet?

    (a) You must meet each emission limit in Table 1 to this subpart 
that applies to you.
    (b) For each wet scrubber applied to meet any particulate matter, 
particulate matter less than 10 microns (PM10), chlorine, 
hydrochloric acid, or dioxins/furans emission limit in Table 1 to this 
subpart, you must maintain the hourly average pressure drop and scrubber 
liquid flow rate at or above the minimum level established during the 
initial or subsequent performance test.



Sec. 63.9891  What work practice standards must I meet for my fugitive 
dust sources?

    (a) You must prepare and at all times operate according to a 
fugitive dust emissions control plan that describes in detail the 
measures that will be put in place to control fugitive dust emissions 
from all unpaved roads and other unpaved operational areas.
    (b) You must submit a copy of your fugitive dust emissions control 
plan for approval to the Administrator on or before the applicable 
compliance date for the affected source as specified in Sec. 63.9883. 
The requirement to operate according to the fugitive dust emissions 
control plan must be incorporated by reference in the source's operating 
permit issued by the permitting authority under 40 CFR part 70 or 40 CFR 
part 71.
    (c) You can use an existing fugitive dust emissions control plan 
provided it meets the requirements in paragraphs (c)(1) through (3) of 
this section.
    (1) The plan satisfies the requirements of paragraph (a) of this 
section.
    (2) The plan describes the current measures to control fugitive dust 
emission sources.
    (3) The plan has been approved as part of a State implementation 
plan or title V permit.
    (d) You must maintain a current copy of the fugitive dust emissions 
control plan on-site and available for inspection upon request. You must 
keep the plan for the life of the affected source or until the affected 
source is no longer subject to the requirements of this subpart.

                 Operation and Maintenance Requirements



Sec. 63.9900  What are my operation and maintenance requirements?

    (a) As required by Sec. 63.6(e)(1)(i), you must always operate and 
maintain your affected source, including air pollution control and 
monitoring equipment, in a manner consistent with good air pollution 
control practices for minimizing emissions at least to the levels 
required by this subpart.
    (b) You must prepare and operate at all times according to a written 
operation and maintenance plan for each control device subject to an 
operating limit in Sec. 63.9890(b). Each plan must address preventative 
maintenance for each control device, including a preventative 
maintenance schedule that is consistent with the manufacturer's 
instructions for routine and long-term maintenance.
    (c) You must maintain a current copy of the operation and 
maintenance plan required in paragraph (b) of this section on-site and 
available for inspection upon request. You must keep the plan for the 
life of the affected source or until the affected source is no longer 
subject to the requirements of this subpart.

[[Page 136]]

                     General Compliance Requirements



Sec. 63.9910  What are my general requirements for complying with this 
subpart?

    (a) You must be in compliance with the emission limitations, work 
practice standards, and operation and maintenance requirements in this 
subpart at all times, except during periods of startup, shutdown, and 
malfunction as defined in Sec. 63.2.
    (b) You must develop and implement a written startup, shutdown and 
malfunction plan according to the provisions in Sec. 63.6(e)(3).

                     Initial Compliance Requirements



Sec. 63.9911  By what date must I conduct performance tests or other 
initial compliance demonstrations?

    (a) As required in Sec. 63.7(a)(2), you must conduct a performance 
test to demonstrate initial compliance with each emission limit in Table 
1 to this subpart that applies to you as indicated in paragraphs (a)(1) 
through (3) of this section:
    (1) Within 180 calendar days after the compliance date that is 
specified in Sec. 63.9883 for your existing affected source;
    (2) By April 7, 2004 for a new source that has an initial startup 
date before October 10, 2003; or
    (3) Within 180 days after initial startup for a new source that has 
an initial startup date after October 10, 2003.
    (b) For each operation and maintenance requirement that applies to 
you where initial compliance is not demonstrated using a performance 
test, you must demonstrate initial compliance within 30 calendar days 
after the compliance date that is specified for your affected source in 
Sec. 63.9883.
    (c) If you commenced construction or reconstruction between January 
22, 2003 and October 10, 2003, you must demonstrate initial compliance 
with either the proposed emission limitation or the promulgated emission 
limitation no later than April 7, 2004 or no later than 180 calendar 
days after startup of the source, whichever is later, according to Sec. 
63.7(a)(2)(ix).
    (d) If you commenced construction or reconstruction between January 
22, 2003 and October 10, 2003, and you chose to comply with the proposed 
emission limit when demonstrating initial compliance, you must conduct a 
second performance test to demonstrate compliance with the promulgated 
emission limit by April 11, 2005, or after startup of the source, 
whichever is later, according to Sec. 63.7(a)(2)(ix).



Sec. 63.9912  When must I conduct subsequent performance tests?

    You must conduct subsequent performance tests to demonstrate 
continuous compliance with all applicable emission limits in Table 1 to 
this subpart no less frequently than twice (at mid-term and renewal) 
during each term of your title V operating permit.



Sec. 63.9913  What test methods and other procedures must I use to 

demonstrate initial compliance with the emission limits for
particulate matter and PM10?

    (a) You must conduct each performance test that applies to your 
affected source according to the requirements in Sec. 63.7(e)(1).
    (b) To determine compliance with the applicable emission limits for 
particulate matter in Table 1 to this subpart, you must follow the test 
methods and procedures in paragraphs (b)(1) and (2) of this section.
    (1) Determine the concentration of particulate matter according to 
the following test methods in appendix A to 40 CFR part 60:
    (i) Method 1 to select sampling port locations and the number of 
traverse points. Sampling ports must be located at the outlet of the 
control device and prior to any releases to the atmosphere.
    (ii) Method 2, 2F, or 2G to determine the volumetric flow rate of 
the stack gas.
    (iii) Method 3, 3A, or 3B to determine the dry molecular weight of 
the stack gas.
    (iv) Method 4 to determine the moisture content of the stack gas.
    (v) Method 5 or 5D, as applicable, to determine the concentration of 
particulate matter.
    (vi) Method 201 or 201A, as applicable, to determine the 
concentration of PM10.
    (2) Collect a minimum sample volume of 60 dry standard cubic feet 
(dscf)

[[Page 137]]

during each particulate matter or PM10 test run. Three valid 
test runs are needed to comprise a performance test.
    (c) Compute the mass emissions rate in pounds per hour (lbs/hr) for 
each test run using Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR10OC03.000

Where:

Elbs/hr = Mass emissions rate of particulate matter or 
PM10 (lbs/hr);
Cs = Concentration of particulate matter or PM10 
in the gas stream, grains per dry standard cubic feet (gr/dscf);
Qstd = Volumetric flow rate of stack gas, dry standard cubic 
feet per minute (dscfm);
60 = Conversion factor, minutes per hour (min/hr); and
7,000 = Conversion factor, grains per pound (gr/lb).



Sec. 63.9914  What test methods and other procedures must I use to 

demonstrate initial compliance with chlorine and hydrochloric acid 
emission limits?

    (a) You must conduct each performance test that applies to your 
affected source according to the requirements in Sec. 63.7(e)(1).
    (b) To determine compliance with the applicable emission limits for 
chlorine and hydrochloric acid in Table 1 to this subpart, you must 
follow the test methods and procedures specified in paragraphs (b)(1) 
and (2) of this section.
    (1) Determine the concentration of chlorine and hydrochloric acid 
according to the following test methods in appendix A to 40 CFR part 60:
    (i) Method 1 to select sampling port locations and the number of 
traverse points. Sampling ports must be located at the outlet of the 
control device and prior to any releases to the atmosphere.
    (ii) Method 2, 2F, or 2G to determine the volumetric flow of the 
stack gas.
    (iii) Method 3, 3A, or 3B to determine the dry molecular weight of 
the stack gas.
    (iv) Method 4 to determine the moisture content of the stack gas.
    (v) Method 26 or 26A, as applicable, to determine the concentration 
of hydrochloric acid and chlorine.
    (2) Collect a minimum sample of 60 dscf during each test run for 
chlorine and hydrochloric acid. Three valid test runs are needed to 
comprise a performance test.
    (c) Compute the mass emissions rate (lbs/hr) for each test run using 
Equation 1 of this section:
[GRAPHIC] [TIFF OMITTED] TR10OC03.001

Where:

Elbs/hr = Mass emissions rate of chlorine or hydrochloric 
acid (lbs/hr);
Cs = Concentration of chlorine or hydrochloric acid in the 
gas stream, milligrams per dry standard cubic meter (mg/dscm);
Qstd = Volumetric flow rate of stack gas (dscfm);
60 = Conversion factor (min/hr);
35.31 = Conversion factor (dscf/dscm); and
454,000 = Conversion factor (mg/lb).



Sec. 63.9915  What test methods and other procedures must I use to 
demonstrate initial compliance with dioxin/furan emission limits?

    (a) You must conduct each performance test that applies to your 
affected source according to the requirements in Sec. 63.7(e)(1).
    (b) To determine compliance with the applicable emission limit for 
dioxins/furans in Table 1 to this subpart, you must follow the test 
methods and procedures specified in paragraphs (b)(1) and (2) of this 
section.
    (1) Determine the concentration of dioxin and furan according to the 
following test methods in appendix A to 40 CFR part 60:
    (i) Method 1 to select sampling port locations and the number of 
traverse points. Sampling ports must be located at the outlet of the 
control device and prior to any releases to the atmosphere.
    (ii) Method 2, 2F, or 2G to determine the volumetric flow of the 
stack gas.
    (iii) Method 3, 3A, or 3B to determine the dry molecular weight of 
the stack gas.
    (iv) Method 4 to determine the moisture content of the stack gas.
    (v) Method 23 to determine the concentration of dioxins/furans. For 
each dioxin/furan congener measured in accordance with this paragraph 
(b)(v), multiply the congener concentration by its corresponding toxic 
equivalency factor specified in Table 2 of this subpart.

[[Page 138]]

    (2) Collect a minimum sample of 100 dscf during each test run. Three 
valid test runs are needed to comprise a performance test.



Sec. 63.9916  What test methods and other procedures must I use to 
establish and demonstrate initial compliance with the operating limits?

    For a wet scrubber subject to operating limits for pressure drop and 
scrubber water flow rate in Sec. 63.9890(b), you must establish site-
specific operating limits according to the procedures in paragraphs (a) 
and (b) of this section.
    (a) Using the continuous parameter monitoring system (CPMS) required 
in Sec. 63.9920, measure and record the pressure drop and scrubber 
water flow rate at least every 15 minutes during each run of the 
particulate matter performance test.
    (b) Compute and record the average pressure drop and scrubber water 
flow rate for each individual test run. Your operating limits are the 
lowest average individual pressure drop and scrubber water flow rate 
values in any of the three runs that meet the applicable emission limit.



Sec. 63.9917  How do I demonstrate initial compliance with the emission 
limitations and work practice standards that apply to me?

    (a) For each affected source subject to an emission limit in Table 1 
to this subpart, you have demonstrated initial compliance if:
    (1) You have met the conditions in Table 3 to this subpart; and
    (2) For each wet scrubber subject to the operating limits for 
pressure drop and scrubber water flow rate in Sec. 63.9890(b), you have 
established appropriate site-specific operating limits and have a record 
of the pressure drop and scrubber water flow rate measured during the 
performance test in accordance with Sec. 63.9916.
    (b) You have demonstrated initial compliance with the work practice 
standards in Sec. 63.9891 if you have certified in your notification of 
compliance status that:
    (1) You have prepared a fugitive dust emissions control plan 
according to the requirements in Sec. 63.9891 and submitted the plan 
for approval; and
    (2) You will operate according to the requirements in the plan.



Sec. 63.9918  How do I demonstrate initial compliance with the operation 
and maintenance requirements that apply to me?

    You must demonstrate initial compliance by certifying in your 
notification of compliance status that you have met the requirements in 
paragraphs (a) and (b) of this section.
    (a) You have prepared the operation and maintenance plan according 
to the requirements in Sec. 63.9910; and
    (b) You will operate each control device according to the procedures 
in the plan.

                   Continuous Compliance Requirements



Sec. 63.9920  What are my continuous monitoring requirements?

    For each wet scrubber subject to the operating limits for pressure 
drop and scrubber water flow rates in Sec. 63.9890(b), you must at all 
times monitor the hourly average pressure drop and liquid flow rate 
using a CPMS according to the requirements in Sec. 63.9921(a).



Sec. 63.9921  What are the installation, operation and maintenance 
requirements for my monitors?

    (a) For each wet scrubber subject to the operating limits in Sec. 
63.9890(b) for pressure drop and scrubber water flow rate, you must 
install, operate, and maintain each CPMS according to the requirements 
in paragraphs (a)(1) and (2) of this section.
    (1) For the pressure drop CPMS, you must:
    (i) Locate the pressure sensor(s) in or as close to a position that 
provides a representative measurement of the pressure and that minimizes 
or eliminates pulsating pressure, vibration, and internal and external 
corrosion.
    (ii) Use a gauge with a minimum measurement sensitivity of 0.5 inch 
of water or a transducer with a minimum measurement sensitivity of 1 
percent of the pressure range.
    (iii) Check the pressure tap for pluggage daily.
    (iv) Using a manometer, check gauge calibration quarterly and 
transducer calibration monthly.

[[Page 139]]

    (v) Conduct calibration checks any time the sensor exceeds the 
manufacturer's specified maximum operating pressure range, or install a 
new pressure sensor.
    (vi) At least monthly, inspect all components for integrity, all 
electrical connections for continuity, and all mechanical connections 
for leakage.
    (2) For the scrubber water flow rate CPMS, you must:
    (i) Locate the flow sensor and other necessary equipment in a 
position that provides a representative flow and that reduces swirling 
flow or abnormal velocity distributions due to upstream and downstream 
disturbances.
    (ii) Use a flow sensor with a minimum measurement sensitivity of 2 
percent of the flow rate.
    (iii) Conduct a flow sensor calibration check at least semiannually 
according to the manufacturer's instructions.
    (iv) At least monthly, inspect all components for integrity, all 
electrical connections for continuity, and all mechanical connections 
for leakage.
    (b) You must install, operate, and maintain each CPMS for a wet 
scrubber according to the requirements in paragraphs (b)(1) through (3) 
of this section.
    (1) Each CPMS must complete a minimum of one cycle of operation for 
each successive 15-minute period.
    (2) Each CPMS must have valid data for at least 95 percent of every 
averaging period.
    (3) Each CPMS must determine and record the hourly average of all 
recorded readings.



Sec. 63.9922  How do I monitor and collect data to demonstrate continuous 
compliance?

    (a) Except for monitoring malfunctions, associated repairs, and 
required quality assurance or control activities (including, as 
applicable, calibration checks and required zero and span adjustments), 
you must monitor continuously (or collect data at all required 
intervals) at all times an affected source is operating.
    (b) You may not use data recorded during monitoring malfunctions, 
associated repairs, and required quality assurance or control activities 
in data averages and calculations used to report emission or operating 
levels or to fulfill a minimum data availability requirement, if 
applicable. You must use all the data collected during all other periods 
in assessing compliance.
    (c) A monitoring malfunction is any sudden, infrequent, not 
reasonably preventable failure of the monitoring to provide valid data. 
Monitoring failures that are caused in part by poor maintenance or 
careless operation are not malfunctions.



Sec. 63.9923  How do I demonstrate continuous compliance with the emission 
limitations and work practice standards that apply to me?

    (a) For each affected source subject to an emission limit in Table 1 
to this subpart, you must demonstrate continuous compliance according to 
the requirements in Table 4 to this subpart.
    (b) For each wet scrubber subject to the operating limits for 
pressure drop and scrubber water flow rate in Sec. 63.9890(b), you must 
demonstrate continuous compliance according to the requirements in 
paragraphs (b)(1) and (2) of this section.
    (1) Collecting and reducing the monitoring data according to Sec. 
63.9921(b); and
    (2) Maintaining the hourly average pressure drop and scrubber water 
flow rate at or above the minimum level established during the initial 
or subsequent performance.
    (c) You must demonstrate continuous compliance with the work 
practice standards in Sec. 63.9891 by operating according to the 
requirements in your fugitive dust emissions control plan and recording 
information needed to document conformance with the requirements.



Sec. 63.9924  How do I demonstrate continuous compliance with the operation 
and maintenance requirements that apply to me?

    For each emission point subject to an emission limit in Table 1 to 
this subpart, you must demonstrate continuous compliance with the 
operation and maintenance requirements in Sec. 63.9900 by performing 
preventive maintenance for each control device according to Sec. 
63.9900(b) and recording

[[Page 140]]

all information needed to document conformance with these requirements.



Sec. 63.9925  What other requirements must I meet to demonstrate continuous 
compliance?

    (a) Deviations. You must report each instance in which you did not 
meet each emission limitation in Sec. 63.9890 or work practice standard 
in Sec. 63.9891 that applies to you. This includes periods of startup, 
shutdown, and malfunction. You must also report each instance in which 
you did not meet each operation and maintenance requirement required in 
Sec. 63.9900 that applies to you. These instances are deviations from 
the emission limitations, work practice standards, and operation and 
maintenance requirements in this subpart. These deviations must be 
reported according to the requirements in Sec. 63.9931.
    (b) Startups, shutdowns, and malfunctions. During periods of 
startup, shutdown, and malfunction, you must operate in accordance with 
your startup, shutdown, and malfunction plan.
    (1) Consistent with Sec. Sec. 63.6(e) and 63.7(e)(1), deviations 
that occur during a period of startup, shutdown, or malfunction are not 
violations if you demonstrate to the Administrator's satisfaction that 
you were operating in accordance with the startup, shutdown, and 
malfunction plan.
    (2) The Administrator will determine whether deviations that occur 
during a period of startup, shutdown, or malfunction are violations, 
according to the provisions in Sec. 63.6(e).

                   Notifications, Reports, and Records



Sec. 63.9930  What notifications must I submit and when?

    (a) You must submit all of the notifications in Sec. Sec. 63.7(b) 
and (c), 63.8(f)(4), 63.9(b), and 63.9(h) that apply to you by the 
specified dates.
    (b) As specified in Sec. 63.9(b)(2), if you startup your affected 
source before October 10, 2003, you must submit your initial 
notification no later than February 9, 2004.
    (c) As specified in Sec. 63.9(b)(3), if you start your new affected 
source on or after October 10, 2003, you must submit your initial 
notification no later that 120 calendar days after you become subject to 
this subpart.
    (d) If you are required to conduct a performance test, you must 
submit a notification of intent to conduct a performance test at least 
60 calendar days before the performance test is scheduled to begin as 
required in Sec. 63.7(b)(1).
    (e) If you are required to conduct a performance test or other 
initial compliance demonstration, you must submit a notification of 
compliance status according to Sec. 63.9(h)(2)(ii), and the 
requirements in paragraphs (e)(1) and (2) of this section:
    (1) For each initial compliance demonstration that does not include 
a performance test, you must submit the notification of compliance 
status before the close of business on the 30th calendar day following 
completion of the initial compliance demonstration.
    (2) For each initial compliance demonstration that does include a 
performance test, you must submit the notification of compliance status, 
including the performance test results, before the close of business on 
the 60th calendar day following the completion of the performance test 
according to Sec. 63.10(d)(2).



Sec. 63.9931  What reports must I submit and when?

    (a) Compliance report due dates. Unless the Administrator has 
approved a different schedule, you must submit a semiannual compliance 
report to your permitting authority according to the requirements in 
paragraphs(a)(1) through (5) of this section.
    (1) The first compliance report must cover the period beginning on 
the compliance date that is specified for your affected source in Sec. 
63.9883 and ending on June 30 or December 31, whichever date comes after 
the compliance date that is specified for your source in Sec. 63.9883.
    (2) The first compliance report must be postmarked or delivered no 
later than July 31 or January 31, whichever date comes first after your 
compliance report is due.
    (3) Each subsequent compliance report must cover the semiannual 
reporting period from January 1 through June 30 or the semiannual 
reporting period from July 1 through December 31.

[[Page 141]]

    (4) Each subsequent compliance report must be postmarked or 
delivered no later than July 31 or January 31, whichever date comes 
first after the end of the semiannual reporting period.
    (5) For each affected source that is subject to permitting 
regulations pursuant to 40 CFR part 70 or 40 CFR part 71, and if the 
permitting authority has established dates for submitting semiannual 
reports pursuant to 40 CFR 70.6(a)(3)(iii)(A) or 40 CFR 
71.6(a)(3)(iii)(A), you may submit the first and subsequent compliance 
reports according to the dates the permitting authority has established 
instead of according to the dates in paragraphs (a)(1) through (4) of 
this section.
    (b) Compliance report contents. Each compliance report must include 
the information in paragraphs (b)(1) through (3) of this section and, as 
applicable, paragraphs (b)(4) through (8) of this section.
    (1) Company name and address.
    (2) Statement by a responsible official, with that official's name, 
title, and signature, certifying the truth, accuracy, and completeness 
of the content of the report.
    (3) Date of report and beginning and ending dates of the reporting 
period.
    (4) If you had a startup, shutdown, or malfunction during the 
reporting period and you took actions consistent with your startup, 
shutdown, and malfunction plan, the compliance report must include the 
information in Sec. 63.10(d)(5)(i).
    (5) If there were no deviations from the continuous compliance 
requirements in Sec. Sec. 63.9923 and 63.9924 that apply to you, a 
statement that there were no deviations from the emission limitations, 
work practice standards, or operation and maintenance requirements 
during the reporting period.
    (6) If there were no periods during which a CPMS was out-of-control 
as specified in Sec. 63.8(c)(7), a statement that there were no periods 
during which the CPMS was out-of-control during the reporting period.
    (7) For each deviation from an emission limitation in Sec. 63.9890 
that occurs at an affected source where you are not using a CPMS to 
comply with an emission limitation in this subpart, the compliance 
report must contain the information in paragraphs (b)(1) through (4) of 
this section and the information in paragraphs (b)(7)(i) and (ii) of 
this section. This includes periods of startup, shutdown, and 
malfunction.
    (i) The total operating time of each affected source during the 
reporting period.
    (ii) Information on the number, duration, and cause of deviations 
(including unknown cause, if applicable) as applicable and the 
corrective action taken.
    (8) For each deviation from an emission limitation occurring at an 
affected source where you are using a CPMS to comply with the emission 
limitation in this subpart, you must include the information in 
paragraphs (b)(1) through (4) of this section and the information in 
paragraphs (b)(8)(i) through (xi) of this section. This includes periods 
of startup, shutdown, and malfunction.
    (i) The date and time that each malfunction started and stopped.
    (ii) The date and time that each continuous monitoring was 
inoperative, except for zero (low-level) and high-level checks.
    (iii) The date, time, and duration that each continuous monitoring 
system was out-of-control, including the information in Sec. 
63.8(c)(8).
    (iv) The date and time that each deviation started and stopped, and 
whether each deviation occurred during a period of startup, shutdown, or 
malfunction or during another period.
    (v) A summary of the total duration of the deviation during the 
reporting period and the total duration as a percent of the total source 
operating time during that reporting period.
    (vi) A breakdown of the total duration of the deviations during the 
reporting period including those that are due to startup, shutdown, 
control equipment problems, process problems, other known causes, and 
other unknown causes.
    (vii) A summary of the total duration of continuous monitoring 
system downtime during the reporting period and the total duration of 
continuous monitoring system downtime as a percent of the total source 
operating time during the reporting period.
    (viii) A brief description of the process units.

[[Page 142]]

    (ix) A brief description of the continuous monitoring system.
    (x) The date of the latest continuous monitoring system 
certification or audit.
    (xi) A description of any changes in continuous monitoring systems, 
processes, or controls since the last reporting period.
    (c) Immediate startup, shutdown, and malfunction report. If you had 
a startup, shutdown, or malfunction during the semiannual reporting 
period that was not consistent with your startup, shutdown, and 
malfunction plan, you must submit an immediate startup, shutdown, and 
malfunction report according to the requirements in Sec. 
63.10(d)(5)(ii).
    (d) Part 70 monitoring report. If you have obtained a title V 
operating permit for an affected source pursuant to 40 CFR part 70 or 40 
CFR part 71, you must report all deviations as defined in this subpart 
in the semiannual monitoring report required by 40 CFR 
70.6(a)(3)(iii)(A) or 40 CFR 71.6(a)(3)(iii)(A). If you submit a 
compliance report for an affected source along with, or as part of, the 
semiannual monitoring report required by 40 CFR 70.6(a)(3)(iii)(A) or 40 
CFR 71.6(a)(3)(iii)(A), and the compliance report includes all the 
required information concerning deviations from any emissions 
limitation, work practice standards, or operation and maintenance 
requirement in this subpart, submission of the compliance report 
satisfies any obligation to report the same deviations in the semiannual 
monitoring report. However, submission of the compliance report does not 
otherwise affect any obligation you may have to report deviations from 
permit requirements for an affected source to your permitting authority.



Sec. 63.9932  What records must I keep?

    (a) You must keep the records as indicated in paragraphs (a)(1) 
through (3) of this section:
    (1) A copy of each notification and report that you submitted to 
comply with this subpart, including all documentation supporting any 
initial notification or notification of compliance status that you 
submitted, according to the requirements in Sec. 63.10(b)(2)(xiv).
    (2) The records in Sec. 63.6(e)(3)(iii) through (v) related to 
startup, shutdown, and malfunction.
    (3) Records of performance tests and performance evaluations as 
required in Sec. 63.10(b)(2)(viii).
    (b) You must keep the records required in Sec. Sec. 63.9932 and 
63.9933 to show continuous compliance with each emission limitation, 
work practice standard, and operating and maintenance requirement that 
applies to you.



Sec. 63.9933  In what form and how long must I keep my records?

    (a) Your records must be in a form suitable and readily available 
for expeditious review, according to Sec. 63.10(b)(1).
    (b) As specified in Sec. 63.10(b)(1), you must keep each record for 
5 years following the date of each occurrence, measurement, maintenance, 
corrective action, report, or record.
    (c) You must keep each record on site for at least 2 years after the 
date of each occurrence, measurement, maintenance, corrective action, 
report, or record according to Sec. 63.10(b)(1). You can keep the 
records off site for the remaining 3 years.
    (d) You must keep your fugitive dust emissions control plan and your 
operation and maintenance plan on-site according to the requirements in 
Sec. Sec. 63.9891(d) and 63.9900(c).

                   Other Requirements and Information



Sec. 63.9940  What parts of the General Provisions apply to me?

    Table 4 to this subpart shows which parts of the General Provisions 
in Sec. Sec. 63.1 through 63.15 apply to you.



Sec. 63.9941  Who implements and enforces this subpart?

    (a) This subpart can be implemented and enforced by us, the United 
States Environmental Protection Agency (U.S. EPA) or a delegated 
authority such as your State, local, or tribal agency. If the EPA 
Administrator has delegated authority to your State, local, or tribal 
agency, then that agency has the authority to implement and enforce this 
subpart. You should contact your EPA Regional Office to find

[[Page 143]]

out if this subpart is delegated to your State, local, or tribal agency.
    (b) In delegating implementation and enforcement authority of this 
subpart to a State, local, or tribal agency under subpart E of this 
part, the authorities contained in paragraph (c) of this section are 
retained by the Administrator of the EPA and are not transferred to the 
State, local, or tribal agency.
    (c) The authorities that will not be delegated to State, local, or 
tribal agencies are specified in paragraphs (c)(1) through (4) of this 
section.
    (1) Approval of alternatives to the non-opacity emission limitations 
in Sec. 63.9890 and work practice standards in Sec. 63.9891 under 
Sec. 63.6(g).
    (2) Approval of major alternatives to test methods under Sec. 
63.7(e)(2)(ii) and (f) and as defined in Sec. 63.90.
    (3) Approval of major alternatives to monitoring under Sec. 63.8(f) 
and as defined in Sec. 63.90.
    (4) Approval of major alternatives to recordkeeping and reporting 
under Sec. 63.10(f) and as defined in Sec. 63.90.



Sec. 63.9942  What definitions apply to this subpart?

    Terms used in this subpart are defined in the Clean Air Act, in 
Sec. 63.2, and in this section as follows:
    Chlorine plant bypass scrubber means the wet scrubber that captures 
chlorine gas during a chlorine plant shut down or failure.
    Deviation means any instance in which an affected source subject to 
this subpart, or an owner or operator of such a source:
    (1) Fails to meet any requirement or obligation established by this 
subpart, including but not limited to any emission limitation (including 
operating limits) or operation and maintenance requirement;
    (2) Fails to meet any term or condition that is adopted to implement 
an applicable requirement in this subpart and that is included in the 
operating permit for any affected source required to obtain such a 
permit; or
    (3) Fails to meet any emission limitation in this subpart during 
startup, shutdown, or malfunction, regardless of whether or not such 
failure is permitted by this subpart.
    Emission limitation means any emission limit, opacity limit, or 
operating limit.
    Launder off-gas system means a system that collects chlorine and 
hydrochloric acid fumes from collection points within the melt/reactor 
system building. The system then removes particulate matter and 
hydrochloric acid from the collected gases prior to discharge to the 
atmosphere.
    Magnesium chloride storage bins means vessels that store dried 
magnesium chloride powder produced from the spray drying operation.
    Melt/reactor system means a system that melts and chlorinates 
dehydrated brine to produce high purity molten magnesium chloride feed 
for electrolysis.
    Primary magnesium refining means the production of magnesium metal 
and magnesium metal alloys from natural sources of magnesium chloride 
such as sea water or water from the Great Salt Lake and magnesium 
bearing ores.
    Responsible official means responsible official as defined in Sec. 
63.2.
    Spray dryer means dryers that evaporate brine to form magnesium 
powder by contact with high temperature gases exhausted from gas 
turbines.
    Wet scrubber means a device that contacts an exhaust gas with a 
liquid to remove particulate matter and acid gases from the exhaust. 
Examples are packed-bed wet scrubbers and venturi scrubbers.
    Work practice standard means any design, equipment, work practice, 
or operational standard, or combination thereof, that is promulgated 
pursuant to section 112(h) of the Clean Air Act.

          Table 1 to Subpart TTTTT of Part 63--Emission Limits

    As required in Sec. 63.9890(a), you must comply with each 
applicable emission limit in the following table:

[[Page 144]]



------------------------------------------------------------------------
 
 
------------------------------------------------------------------------
1. Each spray dryer stack....  a. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                particulate matter in excess of 100 lbs/
                                hr; and
                               b. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                hydrochloric acid in excess of 200 lbs/
                                hr.
2. Each magnesium chloride     a. You must not cause to be discharged to
 storage bins scrubber stack.   the atmosphere any gases that contain
                                hydrochloric acid in excess of 47.5 lbs/
                                hr and 0.35 gr/dscf; and
                               b. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                PM10 in excess of 2.7 lbs/hr and 0.016
                                gr/dscf.
3. Each melt/reactor system    a. You must not cause to be discharged to
 stack.                         the atmosphere any gases that contain
                                PM10 in excess of 13.1 lbs/hr; and
                               b. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                hydrochloric acid in excess of 7.2 lbs/
                                hr; and
                               c. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                chlorine in excess of 100 lbs/hr; and
                               d. You must not cause to be discharged to
                                the atmosphere any gases that contain 36
                                ng TEQ/dscm corrected to 7% oxygen.
4. Each launder off-gas        a. You must not cause to be discharged to
 system stack.                  the atmosphere any gases that contain
                                particulate matter in excess of 37.5 lbs/
                                hr; and
                               b. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                hydrochloric acid in excess of 46.0 lbs/
                                hr; and
                               c. You must not cause to be discharged to
                                the atmosphere any gases that contain
                                chlorine in excess of 26.0 lbs/hr.
------------------------------------------------------------------------

     Table 2 to Subpart TTTTT of Part 63--Toxic Equivalency Factors

------------------------------------------------------------------------
                                                              Toxic
                 Dioxin/furan congener                     equivalency
                                                              factor
------------------------------------------------------------------------
2,3,7,8-tetrachlorinated dibenzo-p-dioxin..............           1
1,2,3,7,8-pentachlorinated dibenzo-p-dioxin............           1
1,2,3,4,7,8-hexachlorinated dibenzo-p-dioxin...........           0.1
1,2,3,7,8,9-hexachlorinated dibenzo-p-dioxin...........           0.1
1,2,3,6,7,8-hexachlorinated dibenzo-p-dioxin...........           0.1
1,2,3,4,6,7,8-heptachlorinated dibenzo-p-dioxin........           0.01
octachlorinated dibenzo-p-dioxin.......................           0.0001
2,3,7,8-tetrachlorinated dibenzofuran..................           0.1
2,3,4,7,8-pentachlorinated dibenzofuran................           0.5
1,2,3,7,8-pentachlorinated dibenzofuran................           0.05
1,2,3,4,7,8-hexachlorinated dibenzofuran...............           0.1
1,2,3,6,7,8-hexachlorinated dibenzofuran...............           0.1
1,2,3,7,8,9-hexachlorinated dibenzofuran...............           0.1
2,3,4,6,7,8-hexachlorinated dibenzofuran...............           0.1
1,2,3,4,6,7,8-heptachlorinated dibenzofuran............           0.01
1,2,3,4,7,8,9-heptachlorinated dibenzofuran............           0.01
octachlorinated dibenzofuran...........................           0.0001
------------------------------------------------------------------------

 Table 3 to Subpart TTTTT of Part 63--Initial Compliance with Emission 
                                 Limits

    As required in 63.9916, you must demonstrate initial compliance with 
the emission limits according to the following table:

------------------------------------------------------------------------
 
 
------------------------------------------------------------------------
1. Each spray dryer stack....  a. The average mass flow of particulate
                                matter from the control system applied
                                to emissions from each spray dryer,
                                measured according to the performance
                                test procedures in Sec. 63.9913(c),
                                did not exceed 100 lbs/hr; and
                               b. The average mass flow of hydrochloric
                                acid from the control system applied to
                                emissions from each spray dryer,
                                determined according to the performance
                                test procedures in Sec. 63.9914(c),
                                did not exceed 200 lbs/hr.
2. Each magnesium chloride     a. The average mass flow of hydrochloric
 storage bin scrubber stack.    acid from the control system applied to
                                the magnesium chloride storage bins
                                scrubber exhaust, measured according to
                                the performance test procedure in Sec.
                                63.9914, did not exceed 47.5 lbs/hr and
                                0.35 gr/dscf; and
                               b. The average mass flow of PM10 from the
                                control system applied to the magnesium
                                chloride storage bins scrubber exhaust,
                                determined according to the performance
                                test procedures in Sec. 63.9913, did
                                not exceed 2.7 lbs/hr and 0.016 gr/dscf.
3. Each melt/reactor system    a. The average mass flow of PM10 from the
 stack.                         control system applied to the melt/
                                reactor system exhaust, measured
                                according to the performance test
                                procedures in Sec. 63.9913, did not
                                exceed 13.1 lbs/hr; and

[[Page 145]]

 
                               b. The average mass flow of hydrochloric
                                acid from the control system applied to
                                the melt/reactor system exhaust,
                                measured according to the performance
                                test procedures in Sec. 63.9914, did
                                not exceed 7.2 lbs/hr; and
                               c. The average mass flow of chlorine from
                                the control system applied to the melt/
                                reactor system exhaust, measured
                                according to the performance test
                                procedures in Sec. 63.9914, did not
                                exceed 100 lbs/hr.
                               d. The average concentration of dioxins/
                                furans from the control system applied
                                to the melt/reactor system exhaust,
                                measured according to the performance
                                test procedures in Sec. 63.9915, did
                                not exceed 36 ng TEQ/dscm corrected to
                                7% oxygen.
4. Each launder off-gas        a. The average mass flow of particulate
 system stack.                  matter from the control system applied
                                to the launder off-gas system collection
                                system exhaust, measured according to
                                the performance test procedures in Sec.
                                 63.9913, did not exceed 37.5 lbs/hr;
                                and
                               b. The average mass flow of hydrochloric
                                acid from the control system applied to
                                the launder off-gas system collection
                                system exhaust, measured according to
                                the performance test procedures in Sec.
                                 63.9914, did not exceed 46.0 lbs/hr;
                                and
                               c. The average mass flow of chlorine from
                                the control system applied to the
                                launder off-gas system collection system
                                exhaust, measured according to the
                                performance test procedures in Sec.
                                63.9914, did not exceed 26.0 lbs/hr.
------------------------------------------------------------------------

Table 4 to Subpart TTTTT of Part 63--Continuous Compliance with Emission 
                                 Limits

    As required in Sec. 63.9923, you must demonstrate continuous 
compliance with the emission limits according to the following table:

------------------------------------------------------------------------
 
 
------------------------------------------------------------------------
1. Each spray dryer stack....  a. Maintaining emissions of PM10 at or
                                below 100 lbs/hr; and
                               b. Maintaining emissions of hydrochloric
                                acid at or below 200 lbs/hr; and
                               c. Conducting subsequent performance
                                tests at least twice during each term of
                                your title V operating permit (at mid-
                                term and renewal).
2. Magnesium chloride storage  a. Maintaining emissions of hydrochloric
 bins scrubber stack.           acid at or below 47.5 lbs/hr and 0.35 gr/
                                dscf; and
                               b. Maintaining emissions of PM10 at or
                                below 2.7 lbs/hr and 0.016 gr/dscf; and
                               c. Conducting subsequent performance
                                tests at least twice during each term of
                                your title V operating permit (at mid-
                                term and renewal).
3. Each melt/reactor system    a. Maintaining emissions of PM10 at or
 stack.                         below 13.1 lbs/hr; and
                               b. Maintaining emissions of hydrochloric
                                acid at or below 7.2 lbs/hr; and
                               c. Maintaining emissions of chlorine at
                                or below 100 lbs/hr; and
                               d. Maintaining emissions of dioxins/
                                furans at or below 36 ng TEQ/dscm
                                corrected to 7% oxygen.
                               e. Conducting subsequent performance test
                                at least twice during each term of your
                                title V operating permit (at mid-term
                                and renewal).
4. Each launder off-gas        a. Maintaining emissions of particulate
 system stack.                  matter at or below 37.5 lbs/hr; and
                               b. Maintaining emissions of hydrochloric
                                acid at or below 46.0 lbs/hr; and
                               c. Maintaining emissions of chlorine at
                                or below 26.0 lbs/hr; and
                               d. Conducting subsequent performance
                                tests at least twice during each term of
                                your title V operating permit (at mid-
                                term and renewal).
------------------------------------------------------------------------

Table 5 to Subpart TTTTT of Part 63--Applicability of General Provisions 
                       to Subpart TTTTT of Part 63

    As required in Sec. 63.9950, you must comply with the requirements 
of the NESHAP General Provisions (40 CFR part 63, subpart A) shown in 
the following table:

----------------------------------------------------------------------------------------------------------------
              Citation                       Subject          Applies to Subpart  TTTTT         Explanation
----------------------------------------------------------------------------------------------------------------
63.1...............................  Applicability.........  Yes.
63.2...............................  Definitions...........  Yes.
63.3...............................  Units and               Yes.
                                      Abbreviations.
63.4...............................  Prohibited Activities.  Yes.
63.5...............................  Construction and        Yes.
                                      Reconstruction.
63.6(a)-(g)........................  Compliance with         Yes.
                                      Standards and
                                      Maintenance
                                      Requirements.
63.6(h)............................  Determining Compliance  No.
                                      with Opacity and
                                      Visible Emission
                                      Standards.
63.6(i)-(j)........................  Extension of            Yes.
                                      Compliance and
                                      Presidential
                                      Compliance Exemption.

[[Page 146]]

 
63.7(a)(1)-(2).....................  Applicability and       No                           Subpart TTTTT
                                      Performance Test                                     specifies performance
                                      Dates.                                               test applicability
                                                                                           and dates.
63.7(a)(3), (b)-(h)................  Performance Testing     Yes.
                                      Requirements.
63.8 except for (a)(4),(c)(4), and   Monitoring              Yes.
 (f)(6).                              Requirements.
63.8(a)(4).........................  Additional Monitoring   No.........................  Subpart TTTTT does not
                                      Requirements for                                     require flares.
                                      Control Devices in
                                      Sec. 63.11.
63.8(c)(4).........................  Continuous Monitoring   No.........................  Subpart TTTTT
                                      System Requirements.                                 specifies
                                                                                           requirements for
                                                                                           operation of CMS.
63.8(f)(6).........................  Relative Accuracy Test  No.........................  Subpart TTTTT does not
                                      Alternative (RATA).                                  require continuous
                                                                                           emission monitoring
                                                                                           systems.
63.9...............................  Notification            Yes.
                                      Requirements.
63.9(g)(5).........................  Data Reduction........  No.........................  Subpart TTTTT
                                                                                           specifies data
                                                                                           reduction
                                                                                           requirements.
63.10 except for (b)(2)(xiii) and    Recordkeeping and       Yes.
 (c)(7)-(8).                          Reporting
                                      Requirements.
63.10(b)(2)(xiii)..................  Continuous Monitoring   No.........................  Subpart TTTTT does not
                                      System (CMS) Records                                 require continuous
                                      for RATA Alternative.                                emission monitoring
                                                                                           systems.
63.10(c)(7)-(8)....................  Records of Excess       No.........................  Subpart TTTTT
                                      Emissions and                                        specifies
                                      Parameter Monitoring                                 recordkeeping
                                      Accedences for CMS.                                  requirements.
63.11..............................  Control Device          No.........................  Subpart TTTTT does not
                                      Requirements.                                        require flares.
63.12..............................  State Authority and     Yes.
                                      Delegations.
63.13-63.15........................  Addresses,              Yes.
                                      Incorporation by
                                      Reference,
                                      Availability of
                                      Information.
----------------------------------------------------------------------------------------------------------------

                   Appendix A to Part 63--Test Methods

   Method 301--Field Validation of Pollutant Measurement Methods from 
                           Various Waste Media

                     1. Applicability and principle

    1.1 Applicability. This method, as specified in the applicable 
subpart, is to be used whenever a source owner or operator (hereafter 
referred to as an ``analyst'') proposes a test method to meet a U.S. 
Environmental Protection Agency (EPA) requirement in the absence of a 
validated method. This Method includes procedures for determining and 
documenting the quality, i.e., systematic error (bias) and random error 
(precision), of the measured concentrations from an effected source. 
This method is applicable to various waste media (i.e., exhaust gas, 
wastewater, sludge, etc.).
    1.1.1 If EPA currently recognizes an appropriate test method or 
considers the analyst's test method to be satisfactory for a particular 
source, the Administrator may waive the use of this protocol or may 
specify a less rigorous validation procedure. A list of validated 
methods may be obtained by contacting the Emission Measurement Technical 
Information Center (EMTIC), Mail Drop 19, U.S. Environmental Protection 
Agency, Research Triangle Park, NC 27711, (919) 541-0200. Procedures for 
obtaining a waiver are in Section 12.0.
    1.1.2 This method includes optional procedures that may be used to 
expand the applicability of the proposed method. Section 7.0 involves 
ruggedness testing (Laboratory Evaluation), which demonstrates the 
sensitivity of the method to various parameters. Section 8.0 involves a 
procedure for including sample stability in bias and precision for 
assessing sample recovery and analysis times; Section 9.0 involves a 
procedure for the determination of the practical limit of quantitation 
for determining the lower limit of the method. These optional procedures 
are required for the waiver consideration outlined in Section 12.0.
    1.2 Principle. The purpose of these procedures is to determine bias 
and precision of a test method at the level of the applicable standard. 
The procedures involve (a) introducing known concentrations of an 
analyte or comparing the test method against a validated test method to 
determine the method's bias and (b) collecting multiple or collocated 
simultaneous samples to determine the method's precision.
    1.2.1 Bias. Bias is established by comparing the method's results 
against a reference value and may be eliminated by employing a 
correction factor established from the data obtained during the 
validation test.

[[Page 147]]

An offset bias may be handled accordingly. Methods that have bias 
correction factors outside 0.7 to 1.3 are unacceptable. Validated method 
to proposed method comparisons, section 6.2, requires a more restrictive 
test of central tendency and a lower correction factor allowance of 0.90 
to 1.10.
    1.2.2 Precision. At the minimum, paired sampling systems shall be 
used to establish precision. The precision of the method at the level of 
the standard shall not be greater than 50 percent relative standard 
deviation. For a validated method to proposed method equivalency 
comparisons, section 6.2, the analyst must demonstrate that the 
precision of the proposed test method is as precise as the validated 
method for acceptance.

                             2. Definitions

    2.1 Negative bias. Bias resulting when the measured result is less 
than the ``true'' value.
    2.2 Paired sampling system. A sampling system capable of obtaining 
two replicate samples that were collected as closely as possible in 
sampling time and sampling location.
    2.3 Positive bias. Bias resulting when the measured result is 
greater than the ``true'' value.
    2.4 Proposed method. The sampling and analytical methodology 
selected for field validation using the method described herein.
    2.5 Quadruplet sampling system. A sampling system capable of 
obtaining four replicate samples that were collected as closely as 
possible in sampling time and sampling location.
    2.6 Surrogate compound. A compound that serves as a model for the 
types of compounds being analyzed (i.e., similar chemical structure, 
properties, behavior). The model can be distinguished by the method from 
the compounds being analyzed.

                          3. Reference Material

    The reference materials shall be obtained or prepared at the level 
of the standard. Additional runs with higher and lower reference 
material concentrations may be made to expand the applicable range of 
the method, in accordance with the ruggedness test procedures.
    3.1 Exhaust Gas Tests. The analyst shall obtain a known 
concentration of the reference material (i.e., analyte of concern) from 
an independent source such as a specialty gas manufacturer, specialty 
chemical company, or commercial laboratory. A list of vendors may be 
obtained from EMTIC (see Section 1.1.1). The analyst should obtain the 
manufacturer's stability data of the analyte concentration and 
recommendations for recertification.
    3.2 Other Waste Media Tests. The analyst shall obtain pure liquid 
components of the reference materials (i.e., analytes of concern) from 
an independent manufacturer and dilute them in the same type matrix as 
the source waste. The pure reference materials shall be certified by the 
manufacturer as to purity and shelf life. The accuracy of all diluted 
reference material concentrations shall be verified by comparing their 
response to independently-prepared materials (independently prepared in 
this case means prepared from pure components by a different analyst).
    3.3 Surrogate Reference Materials. The analyst may use surrogate 
compounds, e.g., for highly toxic or reactive organic compounds, 
provided the analyst can demonstrate to the Administrator's satisfaction 
that the surrogate compound behaves as the analyte. A surrogate may be 
an isotope or one that contains a unique element (e.g., chlorine) that 
is not present in the source or a derivation of the toxic or reactive 
compound, if the derivative formation is part of the method's procedure. 
Laboratory experiments or literature data may be used to show behavioral 
acceptability.
    3.4 Isotopically Labeled Materials. Isotope mixtures may contain the 
isotope and the natural analyte. For best results, the isotope labeled 
analyte concentration should be more than five times the natural 
concentration of the analyte.

                    4. EPA Performance Audit Material

    4.1 To assess the method bias independently, the analyst shall use 
(in addition to the reference material) an EPA performance audit 
material, if it is available. The analyst may contact EMTIC (see section 
1.1.1) to receive a list of currently available EPA audit materials. If 
the analyte is listed, the analyst should request the audit material at 
least 30 days before the validation test. If an EPA audit material is 
not available, request documentation from the validation report 
reviewing authority that the audit material is currently not available 
from EPA. Include this documentation with the field validation report.
    4.2 The analyst shall sample and analyze the performance audit 
sample three times according to the instructions provided with the audit 
sample. The analyst shall submit the three results with the field 
validation report. Although no acceptance criteria are set for these 
performance audit results, the analyst and reviewing authority may use 
them to assess the relative error of sample recovery, sample 
preparation, and analytical procedures and then consider the relative 
error in evaluating the measured emissions.

    5. Procedure for Determination of Bias and Precision in the Field

    The analyst shall select one of the sampling approaches below to 
determine the bias and precision of the data. After analyzing

[[Page 148]]

the samples, the analyst shall calculate the bias and precision 
according to the procedure described in section 6.0. When sampling a 
stationary source, follow the probe placement procedures in section 5.4.
    5.1 Isotopic Spiking. This approach shall be used only for methods 
that require mass spectrometry (MS) analysis. Bias and precision are 
calculated by procedures described in section 6.1.
    5.1.1 Number of Samples and Sampling Runs. Collect a total of 12 
replicate samples by either obtaining six sets of paired samples or 
three sets of quadruplet samples.
    5.1.2 Spiking Procedure. Spike all 12 samples with the reference 
material at the level of the standard. Follow the appropriate spiking 
procedures listed below for the applicable waste medium.
    5.1.2.1 Exhaust Gas Testing. The spike shall be introduced as close 
to the tip of the sampling probe as possible.
    5.1.2.1.1 Gaseous Reference Material with Sorbent or Impinger 
Sampling Trains. Sample the reference material (in the laboratory or in 
the field) at a concentration which is close to the allowable 
concentration standard for the time required by the method, and then 
sample the gas stream for an equal amount of time. The time for sampling 
both the reference material and gas stream should be equal; however, the 
time should be adjusted to avoid sorbent breakthrough.
    5.1.2.1.2 Gaseous Reference Material with Sample Container (Bag or 
Canister). Spike the sample containers after completion of each test run 
with an amount equal to the allowable concentration standard of the 
emission point. The final concentration of the reference material shall 
approximate the level of the emission concentration in the stack. The 
volume amount of reference material shall be less than 10 percent of the 
sample volume.
    5.1.2.1.3 Liquid and Solid Reference Material with Sorbent or 
Impinger Trains. Spike the trains with an amount equal to the allowable 
concentration standard before sampling the stack gas. The spiking should 
be done in the field; however, it may be done in the laboratory.
    5.1.2.1.4 Liquid and Solid Reference Material with Sample Container 
(Bag or Canister). Spike the containers at the completion of each test 
run with an amount equal to the level of the emission standard.
    5.1.2.2 Other Waste Media. Spike the 12 replicate samples with the 
reference material either before or directly after sampling in the 
field.
    5.2 Comparison Against a Validated Test Method. Bias and precision 
are calculated using the procedures described in section 6.2. This 
approach shall be used when a validated method is available and an 
alternative method is being proposed.
    5.2.1 Number of Samples and Sampling Runs. Collect nine sets of 
replicate samples using a paired sampling system (a total of 18 samples) 
or four sets of replicate samples using a quadruplet sampling system (a 
total of 16 samples). In each sample set, the validated test method 
shall be used to collect and analyze half of the samples.
    5.2.2 Performance Audit Exception. Conduct the performance audit as 
required in section 4.0 for the validated test method. Conducting a 
performance audit on the test method being evaluated is recommended.
    5.3 Analyte Spiking. This approach shall be used when sections 5.1 
and 5.2 are not applicable. Bias and precision are calculated using the 
procedures described in Section 6.3.
    5.3.1 Number of Samples and Sampling Runs. Collect a total of 24 
samples using the quadruplet sampling system (a total of 6 sets of 
replicate samples).
    5.3.2 In each quadruplet set, spike half of the samples (two out of 
the four) with the reference material according to the applicable 
procedure in section 5.1.2.1 or 5.1.2.2.
    5.4 Probe Placement and Arrangement for Stationary Source Stack or 
Duct Sampling. The probes shall be placed in the same horizontal plane. 
For paired sample probes the arrangement should be that the probe tip is 
2.5 cm from the outside edge of the other with a pitot tube on the 
outside of each probe. Other paired arrangements for the pitot tube may 
be acceptable. For quadruplet sampling probes, the tips should be in a 
6.0 cm x 6.0 cm square area measured from the center line of the opening 
of the probe tip with a single pitot tube in the center or two pitot 
tubes with their location on either side of the probe tip configuration. 
An alternative arrangement should be proposed whenever the cross-
sectional area of the probe tip configuration is approximately 5 percent 
of the stack or duct cross-sectional area.

                             6. Calculations

    Data resulting from the procedures specified in section 5.0 shall be 
treated as follows to determine bias, correction factors, relative 
standard deviations, precision, and data acceptance.
    6.1 Isotopic Spiking. Analyze the data for isotopic spiking tests as 
outlined in sections 6.1.1 through 6.1.6.
    6.1.1 Calculate the numerical value of the bias using the results 
from the analysis of the isotopically spiked field samples and the 
calculated value of the isotopically labeled spike:

B=CS-Sm Eq. 301=1

where:

B=Bias at the spike level.
Sm=Mean of the measured values of the isotopically spiked 
samples.
CS=Calculated value of the isotopically labeled spike.

[[Page 149]]

    6.1.2 Calculate the standard deviation of the Si values 
as follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.048


Eq. 301-2

where:

S i=Measured value of the isotopically labeled analyte in the 
ith field sample,
n=Number of isotopically spiked samples, 12.
    6.1.3. Calculate the standard deviation of the mean (SDM) as 
follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.049


Eq. 301-3
    6.1.4 Test the bias for statistical significance by calculating the 
t-statistic,
[GRAPHIC] [TIFF OMITTED] TC01MY92.050

Eq. 301-4

and compare it with the critical value of the two-sided t-distribution 
at the 95-percent confidence level and n-1 degrees of freedom. This 
critical value is 2.201 for the eleven degrees of freedom when the 
procedure specified in section 5.1.2 is followed. If the calculated t-
value is greater than the critical value the bias is statistically 
significant and the analyst should proceed to evaluate the correction 
factor.
    6.1.5 Calculation of a Correction Factor. If the t-test does not 
show that the bias is statistically significant, use all analytical 
results without correction and proceed to the precision evaluation. If 
the method's bias is statistically significant, calculate the correction 
factor, CF, using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.051

Eq. 301-5
If the CF is outside the range of 0.70 to 1.30, the data and method are 
considered unacceptable. For correction factors within the range, 
multiply all analytical results by the CF to obtain the final values.
    6.1.6 Calculation of the Relative Standard Deviation (Precision). 
Calculate the relative standard deviation as follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.052

Eq. 301-6
where Sm is the measured mean of the isotopically labeled 
spiked samples.
    6.2 Comparison with Validated Method. Analyze the data for 
comparison with a validated method as outlined in sections 6.2.1 or 
6.2.2, as appropriate. Conduct these procedures in order to determine if 
a proposed method produces results equivalent to a validated method. 
Make all necessary bias corrections for the validated method, as 
appropriate. If the proposed method fails either test, the method 
results are unacceptable, and conclude that the proposed method is not 
as precise or accurate as the validated method. For highly variable 
sources, additional precision checks may be necessary. The analyst 
should consult with the Administrator if a highly variable source is 
suspected.
    6.2.1 Paired Sampling Systems.
    6.2.1.1. Precision. Determine the acceptance of the proposed 
method's variance with respect to the variability of the validated 
method results. If a significant difference is determined, the proposed 
method and the results are rejected. Proposed methods demonstrating F-
values equal to or less than the critical value have acceptable 
precision.
    6.2.1.2 Calculate the variance of the proposed method, 
Sp2, and the variance of the validated method, 
Sv2, using the following equation:

S(porv)2=SD2 Eq. 301-7

where:

SDv=Standard deviation provided with the validated method,
SDp=Standard deviation of the proposed method calculated 
using Equation 301-9a.

    6.2.1.3 The F-test. Determine if the variance of the proposed method 
is significantly different from that of the validated method by 
calculating the F-value using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.053

Eq. 301-8
    Compare the experimental F value with the critical value of F. The 
critical value is 1.0 when the procedure specified in section 5.2.1 for 
paired trains is followed. If the calculated F is greater than the 
critical value, the difference in precision is significant and the data 
and proposed method are unacceptable.
    6.2.1.4 Bias Analysis. Test the bias for statistical significance by 
calculating the t-statistic and determine if the mean of the differences 
between the proposed method and the validated method is significant at 
the 80-percent confidence level. This procedure requires the standard 
deviation of the validated method, SDv, to be known. Employ 
the

[[Page 150]]

value furnished with the method. If the standard deviation of the 
validated method is not available, the paired replicate sampling 
procedure may not be used. Determine the mean of the paired sample 
differences, dm, and the standard deviation, SDd, 
of the differences, d1's, using Equation 301-2 where: 
di replaces Si, dm replaces 
Sm. Calculate the standard deviation of the proposed method, 
SDp, as follows:

SDp=SDd-SDv Eq. 301-9a

(If SDvSDd, let SD=SDd/
1.414).

    Calculate the value of the t-statistic using the following equation:
    [GRAPHIC] [TIFF OMITTED] TC01MY92.054
    
Eq. 301-9

where n is the total number of paired samples. For the procedure in 
section 5.2.1, n equals nine. Compare the calculated t-statistic with 
the corresponding value from the table of the t-statistic. When nine 
runs are conducted, as specified in section 5.2.1, the critical value of 
the t-statistic is 1.397 for eight degrees of freedom. If the calculated 
t-value is greater than the critical value the bias is statistically 
significant and the analyst should proceed to evaluate the correction 
factor.
    6.2.1.5 Calculation of a Correction Factor. If the statistical test 
cited above does not show a significant bias with respect to the 
reference method, assume that the proposed method is unbiased and use 
all analytical results without correction. If the method's bias is 
statistically significant, calculate the correction factor, CF, as 
follows:
[GRAPHIC] [TIFF OMITTED] TC01MY92.055

Eq. 301-10

where Vm is the mean of the validated method's values.
    Multiply all analytical results by CF to obtain the final values. 
The method results, and the method, are unacceptable if the correction 
factor is outside the range of 0.9 to 1.10.
    6.2.2 Quadruplet Replicate Sampling Systems.
    6.2.2.1 Precision. Determine the acceptance of the proposed method's 
variance with respect to the variability of the validated method 
results. If a significant difference is determined the proposed method 
and the results are rejected.
    6.2.2.2 Calculate the variance of the proposed method, 
Sp2, using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.056

Eq. 301-11

where the di's are the differences between the validated 
method values and the proposed method values.

    6.2.2.3 The F-test. Determine if the variance of the proposed method 
is more variable than that of the validated method by calculating the F-
value using Equation 301-8. Compare the experimental F value with the 
critical value of F. The critical value is 1.0 when the procedure 
specified in section 5.2.2 for quadruplet trains is followed. The 
calculated F should be less than or equal to the critical value. If the 
difference in precision is significant the results and the proposed 
method are unacceptable.
    6.2.2.4 Bias Analysis. Test the bias for statistical significance at 
the 80 percent confidence level by calculating the t-statistic. 
Determine the bias (mean of the differences between the proposed method 
and the validated method, dm) and the standard deviation, 
SDd, of the differences. Calculate the standard deviation of 
the differences, SDd, using Equation 301-2 and substituting 
di for Si. The following equation is used to 
calculate di:
[GRAPHIC] [TIFF OMITTED] TC01MY92.057

Eq. 301-12

and: V1i=First measured value of the validated method in the 
ith test sample.
P1i=First measured value of the proposed method in the ith 
test sample.

    Calculate the t-statistic using Equation 301-9 where n is the total 
number of test sample differences (di). For the procedure in 
section 5.2.2, n equals four. Compare the calculated t-statistic with 
the corresponding value from the table of the t-statistic and determine 
if the mean is significant at the 80-percent confidence level. When four 
runs are conducted, as specified in section 5.2.2, the critical value of 
the t-statistic is 1.638 for three degrees of freedom. If the calculated 
t-value is greater than the critical value the bias is statistically 
significant and the analyst should proceed to evaluate the correction 
factor.
    6.2.2.5 Correction Factor Calculation. If the method's bias is 
statistically significant, calculate the correction factor, CF, using 
Equation 301-10. Multiply all analytical results by CF to obtain the 
final values. The method results, and the method, are unacceptable if 
the correction factor is outside the range of 0.9 to 1.10.

[[Page 151]]

    6.3 Analyte Spiking. Analyze the data for analyte spike testing as 
outlined in Sections 6.3.1 through 6.3.3.
    6.3.1 Precision.
    6.3.1.1 Spiked Samples. Calculate the difference, di, 
between the pairs of the spiked proposed method measurements for each 
replicate sample set. Determine the standard deviation (SDs) 
of the spiked values using the following equation:
[GRAPHIC] [TIFF OMITTED] TC01MY92.058

Eq. 301-13

where: n = Number of runs.
    Calculate the relative standard deviation of the proposed spiked 
method using Equation 301-6 where Sm is the measured mean of 
the analyte spiked samples. The proposed method is unacceptable if the 
RSD is greater than 50 percent.
    6.3.1.2 Unspiked Samples. Calculate the standard deviation of the 
unspiked values using Equation 301-13 and the relative standard 
deviation of the proposed unspiked method using Equation 301-6 where 
Sm is the measured mean of the analyte spiked samples. The 
RSD must be less than 50 percent.
    6.3.2 Bias. Calculate the numerical value of the bias using the 
results from the analysis of the spiked field samples, the unspiked 
field samples, and the calculated value of the spike:

B=Sm-Mm-CS
Eq. 301-14

where: B = Bias at the spike level.
Sm = Mean of the spiked samples.
Mm = Mean of the unspiked samples.
CS = Calculated value of the spiked level.
    6.3.2.1 Calculate the standard deviation of the mean using the 
following equation where SDs and SDu are the 
standard deviations of the spiked and unspiked sample values 
respectively as calculated using Equation 301-13.
[GRAPHIC] [TIFF OMITTED] TC01MY92.059

Eq. 301-15

    6.3.2.2 Test the bias for statistical significance by calculating 
the t-statistic using Equation 301-4 and comparing it with the critical 
value of the two-sided t-distribution at the 95-percent confidence level 
and n-1 degrees of freedom. This critical value is 2.201 for the eleven 
degrees of freedom.
    6.3.3 Calculation of a Correction Factor. If the t-test shows that 
the bias is not statistically significant, use all analytical results 
without correction. If the method's bias is statistically significant, 
calculate the correction factor using Equation 301-5. Multiply all 
analytical results by CF to obtain the final values.

                    7. Ruggedness Testing (Optional)

    7.1 Laboratory Evaluation.
    7.1.1 Ruggedness testing is a useful and cost-effective laboratory 
study to determine the sensitivity of a method to certain parameters 
such as sample collection rate, interferant concentration, collecting 
medium temperature, or sample recovery temperature. This Section 
generally discusses the principle of the ruggedness test. A more 
detailed description is presented in citation 10 of Section 13.0.
    7.1.2 In a ruggedness test, several variables are changed 
simultaneously rather than one variable at a time. This reduces the 
number of experiments required to evaluate the effect of a variable. For 
example, the effect of seven variables can be determined in eight 
experiments rather than 128 (W.J. Youden, Statistical Manual of the 
Association of Official Analytical Chemists, Association of Official 
Analytical Chemists, Washington, DC, 1975, pp. 33-36).
    7.1.3 Data from ruggedness tests are helpful in extending the 
applicability of a test method to different source concentrations or 
source categories.

   8. Procedure for Including Sample Stability in Bias and Precision 
                               Evaluations

    8.1 Sample Stability.
    8.1.1 The test method being evaluated must include procedures for 
sample storage and the time within which the collected samples shall be 
analyzed.
    8.1.2 This section identifies the procedures for including the 
effect of storage time in bias and precision evaluations. The evaluation 
may be deleted if the test method specifies a time for sample storage.
    8.2 Stability Test Design. The following procedures shall be 
conducted to identify the effect of storage times on analyte samples. 
Store the samples according to the procedure specified in the test 
method. When using the analyte spiking procedures (section 5.3), the 
study should include equal numbers of spiked and unspiked samples.
    8.2.1 Stack Emission Testing.
    8.2.1.1 For sample container (bag or canister) and impinger sampling 
systems, sections 5.1 and 5.3, analyze six of the samples at the minimum 
storage time. Then analyze the same six samples at the maximum storage 
time.
    8.2.1.2 For sorbent and impinger sampling systems, sections 5.1 and 
5.3, that require extraction or digestion, extract or digest six of the 
samples at the minimum storage time and extract or digest six other 
samples at the maximum storage time. Analyze an aliquot of the first six 
extracts (digestates) at both the minimum and maximum storage

[[Page 152]]

times. This will provide some freedom to analyze extract storage 
impacts.
    8.2.1.3 For sorbent sampling systems, sections 5.1 and 5.3, that 
require thermal desorption, analyze six samples at the minimum storage 
time. Analyze another set of six samples at the maximum storage time.
    8.2.1.4 For systems set up in accordance with section 5.2, the 
number of samples analyzed at the minimum and maximum storage times 
shall be half those collected (8 or 9). The procedures for samples 
requiring extraction or digestion should parallel those in section 
8.2.1.
    8.2.2 Other Waste Media Testing. Analyze half of the replicate 
samples at the minimum storage time and the other half at the maximum 
storage time in order to identify the effect of storage times on analyte 
samples.

   9. Procedure for Determination of Practical Limit of Quantitation 
                               (Optional)

    9.1 Practical Limit of Quantitation.
    9.1.1 The practical limit of quantitation (PLQ) is the lowest level 
above which quantitative results may be obtained with an acceptable 
degree of confidence. For this protocol, the PLQ is defined as 10 times 
the standard deviation, so, at the blank level. This PLQ 
corresponds to an uncertainty of 30 percent at the 
99-percent confidence level.
    9.1.2 The PLQ will be used to establish the lower limit of the test 
method.
    9.2 Procedure I for Estimating so. This procedure is 
acceptable if the estimated PLQ is no more than twice the calculated 
PLQ. If the PLQ is greater than twice the calculated PLQ use Procedure 
II.
    9.2.1 Estimate the PLQ and prepare a test standard at this level. 
The test standard could consist of a dilution of the reference material 
described in section 3.0.
    9.2.2 Using the normal sampling and analytical procedures for the 
method, sample and analyze this standard at least seven times in the 
laboratory.
    9.2.3 Calculate the standard deviation, so, of the 
measured values.
    9.2.4 Calculate the PLQ as 10 times so.
    9.3 Procedure II for Estimating so. This procedure is to 
be used if the estimated PLQ is more than twice the calculated PLQ.
    9.3.1 Prepare two additional standards at concentration levels lower 
than the standard used in Procedure I.
    9.3.2 Sample and analyze each of these standards at least seven 
times.
    9.3.3 Calculate the standard deviation for each concentration level.
    9.3.4 Plot the standard deviations of the three test standards as a 
function of the standard concentrations.
    9.3.5 Draw a best-fit straight line through the data points and 
extrapolate to zero concentration. The standard deviation at zero 
concentration is S0.
    9.3.6 Calculate the PLQ as 10 times S0.

                10.0 Field Validation Report Requirements

    The field validation report shall include a discussion of the 
regulatory objectives for the testing which describe the reasons for the 
test, applicable emission limits, and a description of the source. In 
addition, validation results shall include:
    10.1 Summary of the results and calculations shown in section 6.0.
    10.2 Reference material certification and value(s).
    10.3 Performance audit results or letter from the reviewing 
authority stating the audit material is currently not available.
    10.4 Laboratory demonstration of the quality of the spiking system.
    10.5 Discussion of laboratory evaluations.
    10.6 Discussion of field sampling.
    10.7 Discussion of sample preparations and analysis.
    10.8 Storage times of samples (and extracts, if applicable).
    10.9 Reasons for eliminating any results.

                          11. Followup Testing

    The correction factor calculated in section 6.0 shall be used to 
adjust the sample concentrations in all followup tests conducted at the 
same source. These tests shall consist of at least three replicate 
samples, and the average shall be used to determine the pollutant 
concentration. The number of samples to be collected and analyzed shall 
be as follows, depending on the validated method precision level:
    11.1 Validated relative standard deviation (RSD) <= 15 Percent. Three replicate samples.
    11.2 Validated RSD <= 30 Percent. Six 
replicate samples.
    11.3 Validated RSD <= 50 Percent. Nine 
replicate samples.
    11.4 Equivalent method. Three replicate samples.

                  12. Procedure for Obtaining a Waiver

    12.1 Waivers. These procedures may be waived or a less rigorous 
protocol may be granted for site-specific applications. The following 
are three example situations for which a waiver may be considered.
    12.1.1 ``Similar'' Sources. If the test method has been validated 
previously at a ``similar'' source, the procedures may be waived 
provided the requester can demonstrate to the satisfaction of the 
Administrator that the sources are ``similar.'' The methods's 
applicability to the ``similar'' source may be demonstrated by 
conducting a ruggedness test as described in section 6.0.

[[Page 153]]

    12.1.2 ``Documented'' Methods. In some cases, bias and precision may 
have been documented through laboratory tests or protocols different 
from this method. If the analyst can demonstrate to the satisfaction of 
the Administrator that the bias and precision apply to a particular 
application, the Administrator may waive these procedures or parts of 
the procedures.
    12.1.3 ``Conditional'' Test Methods. When the method has been 
demonstrated to be valid at several sources, the analyst may seek a 
``conditional'' method designation from the Administrator. 
``Conditional'' method status provides an automatic waiver from the 
procedures provided the test method is used within the stated 
applicability.
    12.2 Application for Waiver. In general, the requester shall provide 
a thorough description of the test method, the intended application, and 
results of any validation or other supporting documents. Because of the 
many potential situations in which the Administrator may grant a waiver, 
it is neither possible nor desirable to prescribe the exact criteria for 
a waiver. At a minimum, the requester is responsible for providing the 
following.
    12.2.1 A clearly written test method, preferably in the format of 40 
CFR part 60, appendix A Test Methods. The method must include an 
applicability statement, concentration range, precision, bias 
(accuracy), and time in which samples must be analyzed.
    12.2.2.2 Summaries (see section 10.0) of previous validation tests 
or other supporting documents. If a different procedure from that 
described in this method was used, the requester shall provide 
appropriate documents substantiating (to the satisfaction of the 
Administrator) the bias and precision values.
    12.2.2.3 Results of testing conducted with respect to sections 7.0, 
8.0, and 9.0.
    12.2.3 Discussion of the applicability statement and arguments for 
approval of the waiver. This discussion should address as applicable the 
following: Applicable regulation, emission standards, effluent 
characteristics, and process operations.
    12.3 Requests for Waiver. Each request shall be in writing and 
signed by the analyst. Submit requests to the Director, OAQPS, Technical 
Support Division, U.S. Environmental Protection Agency, Research 
Triangle Park, NC 27711.

                            13. Bibliography

    1. Albritton, J.R., G.B. Howe, S.B. Tompkins, R.K.M. Jayanty, and 
C.E. Decker, 1989. Stability of Parts-Per-Million Organic Cylinder Gases 
and Results of Source Test Analysis Audits, Status Report No. 11. 
Environmental Protection Agency Contract 68-02-4125. Research Triangle 
Institute, Research Triangle Park, NC. September.
    2. DeWees, W.G., P.M. Grohse, K.K. Luk, and F.E. Butler. 1989. 
Laboratory and Field Evaluation of a Methodology for Speciating Nickel 
Emissions from Stationary Sources. EPA Contract 68-02-4442. Prepared for 
Atmospheric Research and Environmental Assessment Laboratory, Office of 
Research and Development, U.S. Environmental Protection Agency, Research 
Triangle Park, NC 27711. January.
    3. Keith, L.H., W. Crummer, J. Deegan Jr., R.A. Libby, J.K. Taylor, 
and G. Wentler. 1983. Principles of Environmental Analysis. American 
Chemical Society, Washington, DC.
    4. Maxwell, E.A. 1974. Estimating variances from one or two 
measurements on each sample. Amer. Statistician 28:96-97.
    5. Midgett, M.R. 1977. How EPA Validates NSPS Methodology. Environ. 
Sci. & Technol. 11(7):655-659.
    6. Mitchell, W.J., and M.R. Midgett. 1976. Means to evaluate 
performance of stationary source test methods. Environ. Sci. & Technol. 
10:85-88.
    7. Plackett, R.L., and J.P. Burman. 1946. The design of optimum 
multifactorial experiments. Biometrika, 33:305.
    8. Taylor, J.K. 1987. Quality Assurance of Chemical Measurements. 
Lewis Publishers, Inc., pp. 79-81.
    9. U.S. Environmental Protection Agency. 1978. Quality Assurance 
Handbook for Air Pollution Measurement Systems: Volume III. Stationary 
Source Specific Methods. Publication No. EPA-600/4-77-027b. Office of 
Research and Development Publications, 26 West St. Clair St., 
Cincinnati, OH 45268.
    10. U.S. Environmental Protection Agency. 1981. A Procedure for 
Establishing Traceability of Gas Mixtures to Certain National Bureau of 
Standards Standard Reference Materials. Publication No. EPA-600/7-81-
010. Available from the U.S. EPA, Quality Assurance Division (MD-77), 
Research Triangle Park, NC 27711.
    11. U.S. Environmental Protection Agency. 1991. Protocol for The 
Field Validation of Emission Concentrations From Stationary Sources. 
Publication No. 450/4-90-015. Available from the U.S. EPA, Emission 
Measurement Technical Information Center, Technical Support Division 
(MD-14), Research Triangle Park, NC 27711.
    12. Youdon, W.J. Statistical techniques for collaborative tests. In: 
Statistical Manual of the Association of Official Analytical Chemists, 
Association of Official Analytical Chemists, Washington, DC, 1975, pp. 
33-36.

Method 303--Determination of Visible Emissions From By-Product Coke Oven 
                                Batteries

    Note: This method is not inclusive with respect to observer 
certification. Some material is incorporated by reference from other 
methods in appendix A to 40 CFR part 60.

[[Page 154]]

Therefore, to obtain reliable results, persons using this method should 
have a thorough knowledge of Method 9.

                        1.0 Scope and Application

    1.1 Applicability. This method is applicable for the determination 
of visible emissions (VE) from the following by-product coke oven 
battery sources: charging systems during charging; doors, topside port 
lids, and offtake systems on operating coke ovens; and collecting mains. 
This method is also applicable for qualifying observers for visually 
determining the presence of VE.

                          2.0 Summary of Method

    2.1 A certified observer visually determines the VE from coke oven 
battery sources. Certification procedures are presented. This method 
does not require that opacity of emissions be determined or that 
magnitude be differentiated.

                             3.0 Definitions

    3.1 Bench means the platform structure in front of the oven doors.
    3.2 By-product Coke Oven Battery means a source consisting of a 
group of ovens connected by common walls, where coal undergoes 
destructive distillation under positive pressure to produce coke and 
coke oven gas, from which by-products are recovered.
    3.3 Charge or charging period means the period of time that 
commences when coal begins to flow into an oven through a topside port 
and ends when the last charging port is recapped.
    3.4 Charging system means an apparatus used to charge coal to a coke 
oven (e.g., a larry car for wet coal charging systems).
    3.5 Coke oven door means each end enclosure on the push side and the 
coking side of an oven. The chuck, or leveler-bar, door is considered 
part of the push side door. The coke oven door area includes the entire 
area on the vertical face of a coke oven between the bench and the top 
of the battery between two adjacent buck stays.
    3.6 Coke side means the side of a battery from which the coke is 
discharged from ovens at the end of the coking cycle.
    3.7 Collecting main means any apparatus that is connected to one or 
more offtake systems and that provides a passage for conveying gases 
under positive pressure from the by-product coke oven battery to the by-
product recovery system.
    3.8 Consecutive charges means charges observed successively, 
excluding any charge during which the observer's view of the charging 
system or topside ports is obscured.
    3.9 Damper-off means to close off the gas passage between the coke 
oven and the collecting main, with no flow of raw coke oven gas from the 
collecting main into the oven or into the oven's offtake system(s).
    3.10 Decarbonization period means the period of time for combusting 
oven carbon that commences when the oven lids are removed from an empty 
oven or when standpipe caps of an oven are opened. The period ends with 
the initiation of the next charging period for that oven.
    3.11 Larry car means an apparatus used to charge coal to a coke oven 
with a wet coal charging system.
    3.12 Log average means logarithmic average as calculated in Section 
12.4.
    3.13 Offtake system means any individual oven apparatus that is 
stationary and provides a passage for gases from an oven to a coke oven 
battery collecting main or to another oven. Offtake system components 
include the standpipe and standpipe caps, goosenecks, stationary jumper 
pipes, mini-standpipes, and standpipe and gooseneck connections.
    3.14 Operating oven means any oven not out of operation for rebuild 
or maintenance work extensive enough to require the oven to be skipped 
in the charging sequence.
    3.15 Oven means a chamber in the coke oven battery in which coal 
undergoes destructive distillation to produce coke.
    3.16 Push side means the side of the battery from which the coke is 
pushed from ovens at the end of the coking cycle.
    3.17 Run means the observation of visible emissions from topside 
port lids, offtake systems, coke oven doors, or the charging of a single 
oven in accordance with this method.
    3.18 Shed means an enclosure that covers the side of the coke oven 
battery, captures emissions from pushing operations and from leaking 
coke oven doors on the coke side or push side of the coke oven battery, 
and routes the emissions to a control device or system.
    3.19 Standpipe cap means An apparatus used to cover the opening in 
the gooseneck of an offtake system.
    3.20 Topside port lid means a cover, removed during charging or 
decarbonizing, that is placed over the opening through which coal can be 
charged into the oven of a by-product coke oven battery.
    3.21 Traverse time means accumulated time for a traverse as measured 
by a stopwatch. Traverse time includes time to stop and write down oven 
numbers but excludes time waiting for obstructions of view to clear or 
for time to walk around obstacles.
    3.22 Visible Emissions or VE means any emission seen by the unaided 
(except for corrective lenses) eye, excluding steam or condensing water.

                      4.0 Interferences [Reserved]

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method may not address all

[[Page 155]]

of the safety problems associated with its use. It is the responsibility 
of the user of this test method to establish appropriate safety and 
health practices and determine the applicability of regulatory 
limitations prior to performing this test method.
    5.2 Safety Training. Because coke oven batteries have hazardous 
environments, the training materials and the field training (Section 
10.0) shall cover the precautions required by the company to address 
health and safety hazards. Special emphasis shall be given to the 
Occupational Safety and Health Administration (OSHA) regulations 
pertaining to exposure of coke oven workers (see Reference 3 in Section 
16.0). In general, the regulation requires that special fire-retardant 
clothing and respirators be worn in certain restricted areas of the coke 
oven battery. The OSHA regulation also prohibits certain activities, 
such as chewing gum, smoking, and eating in these areas.

                  6.0 Equipment and Supplies [Reserved]

                  7.0 Reagents and Standards [Reserved]

 8.0 Sample Collection, Preservation, Transport, and Storage [Reserved]

                     9.0 Quality Control [Reserved]

                  10.0 Calibration and Standardization

    Observer certification and training requirements are as follows:
    10.1 Certification Procedures. This method requires only the 
determination of whether VE occur and does not require the determination 
of opacity levels; therefore, observer certification according to Method 
9 in appendix A to part 60 of this chapter is not required to obtain 
certification under this method. However, in order to receive Method 303 
observer certification, the first-time observer (trainee) shall have 
attended the lecture portion of the Method 9 certification course. In 
addition, the trainee shall successfully complete the Method 303 
training course, satisfy the field observation requirement, and 
demonstrate adequate performance and sufficient knowledge of Method 303. 
The Method 303 training course shall be conducted by or under the 
sanction of the EPA and shall consist of classroom instruction and field 
observations, and a proficiency test.
    10.1.1 The classroom instruction shall familiarize the trainees with 
Method 303 through lecture, written training materials, and a Method 303 
demonstration video. A successful completion of the classroom portion of 
the Method 303 training course shall be demonstrated by a perfect score 
on a written test. If the trainee fails to answer all of the questions 
correctly, the trainee may review the appropriate portion of the 
training materials and retake the test.
    10.1.2 The field observations shall be a minimum of 12 hours and 
shall be completed before attending the Method 303 certification course. 
Trainees shall observe the operation of a coke oven battery as it 
pertains to Method 303, including topside operations, and shall also 
practice conducting Method 303 or similar methods. During the field 
observations, trainees unfamiliar with coke battery operations shall 
receive instruction from an experienced coke oven observer familiar with 
Method 303 or similar methods and with the operation of coke batteries. 
The trainee must verify completion of at least 12 hours of field 
observation prior to attending the Method 303 certification course.
    10.1.3 All trainees must demonstrate proficiency in the application 
of Method 303 to a panel of three certified Method 303 observers, 
including an ability to differentiate coke oven emissions from 
condensing water vapor and smoldering coal. Each panel member shall have 
at least 120 days experience in reading visible emissions from coke 
ovens. The visible emissions inspections that will satisfy the 
experience requirement must be inspections of coke oven battery fugitive 
emissions from the emission points subject to emission standards under 
subpart L of this part (i.e., coke oven doors, topside port lids, 
offtake system(s), and charging operations), using either Method 303 or 
predecessor State or local test methods. A ``day's experience'' for a 
particular inspection is a day on which one complete inspection was 
performed for that emission point under Method 303 or a predecessor 
State or local method. A ``day's experience'' does not mean 8 or 10 
hours performing inspections, or any particular time expressed in 
minutes or hours that may have been spent performing them. Thus, it 
would be possible for an individual to qualify as a Method 303 panel 
member for some emission points, but not others (e.g., an individual 
might satisfy the experience requirement for coke oven doors, but not 
topside port lids). Until November 15, 1994, the EPA may waive the 
certification requirement (but not the experience requirement) for panel 
members. The composition of the panel shall be approved by the EPA. The 
panel shall observe the trainee in a series of training runs and a 
series of certification runs. There shall be a minimum of 1 training run 
for doors, topside port lids, and offtake systems, and a minimum of 5 
training runs (i.e., 5 charges) for charging. During training runs, the 
panel can advise the trainee on proper procedures. There shall be a 
minimum of 3 certification runs for doors, topside port lids, and 
offtake systems, and a minimum of 15 certification runs for charging 
(i.e., 15 charges). The certifications runs shall be unassisted. 
Following the certification test runs, the panel shall approve or 
disapprove certification based on the trainee's performance during the 
certification

[[Page 156]]

runs. To obtain certification, the trainee shall demonstrate to the 
satisfaction of the panel a high degree of proficiency in performing 
Method 303. To aid in evaluating the trainee's performance, a checklist, 
provided by the EPA, will be used by the panel members.
    10.2 Observer Certification/Recertification. The coke oven observer 
certification is valid for 1 year from date of issue. The observer shall 
recertify annually by viewing the training video and answering all of 
the questions on the certification test correctly. Every 3 years, an 
observer shall be required to pass the proficiency test in Section 
10.1.3 in order to be certified.
    10.3 The EPA (or applicable enforcement agency) shall maintain 
records reflecting a certified observer's successful completion of the 
proficiency test, which shall include the completed proficiency test 
checklists for the certification runs.
    10.4 An owner or operator of a coke oven battery subject to subpart 
L of this part may observe a training and certification program under 
this section.

                             11.0 Procedure

    11.1 Procedure for Determining VE from Charging Systems During 
Charging.
    11.1.1 Number of Oven Charges. Refer to Sec. 63.309(c)(1) of this 
part for the number of oven charges to observe. The observer shall 
observe consecutive charges. Charges that are nonconsecutive can only be 
observed when necessary to replace observations terminated prior to the 
completion of a charge because of visual interferences. (See Section 
11.1.5).
    11.1.2 Data Records. Record all the information requested at the top 
of the charging system inspection sheet (Figure 303-1). For each charge, 
record the identification number of the oven being charged, the 
approximate beginning time of the charge, and the identification of the 
larry car used for the charge.
    11.1.3 Observer Position. Stand in an area or move to positions on 
the topside of the coke oven battery with an unobstructed view of the 
entire charging system. For wet coal charging systems or non-pipeline 
coal charging systems, the observer should have an unobstructed view of 
the emission points of the charging system, including larry car hoppers, 
drop sleeves, and the topside ports of the oven being charged. Some 
charging systems are configured so that all emission points can only be 
seen from a distance of five ovens. For other batteries, distances of 8 
to 12 ovens are adequate.
    11.1.4 Observation. The charging period begins when coal begins to 
flow into the oven and ends when the last charging port is recapped. 
During the charging period, observe all of the potential sources of VE 
from the entire charging system. For wet coal charging systems or non-
pipeline coal charging systems, sources of VE typically include the 
larry car hoppers, drop sleeves, slide gates, and topside ports on the 
oven being charged. Any VE from an open standpipe cap on the oven being 
charged is included as charging VE.
    11.1.4.1 Using an accumulative-type stopwatch with unit divisions of 
at least 0.5 seconds, determine the total time VE are observed as 
follows. Upon observing any VE emerging from any part of the charging 
system, start the stopwatch. Stop the watch when VE are no longer 
observed emerging, and restart the watch when VE reemerges.
    11.1.4.2 When VE occur simultaneously from several points during a 
charge, consider the sources as one. Time overlapping VE as continuous 
VE. Time single puffs of VE only for the time it takes for the puff to 
emerge from the charging system. Continue to time VE in this manner for 
the entire charging period. Record the accumulated time to the nearest 
0.5 second under ``Visible emissions, seconds'' on Figure 303-1.
    11.1.5 Visual Interference. If fugitive VE from other sources at the 
coke oven battery site (e.g., door leaks or condensing water vapor from 
the coke oven wharf) prevent a clear view of the charging system during 
a charge, stop the stopwatch and make an appropriate notation under 
``Comments'' on Figure 303-1. Label the observation an observation of an 
incomplete charge, and observe another charge to fulfill the 
requirements of Section 11.1.1.
    11.1.6 VE Exemptions. Do not time the following VE:
    11.1.6.1 The VE from burning or smoldering coal spilled on top of 
the oven, topside port lid, or larry car surfaces;
    Note: The VE from smoldering coal are generally white or gray. These 
VE generally have a plume of less than 1 meter long. If the observer 
cannot safely and with reasonable confidence determine that VE are from 
charging, do not count them as charging emissions.
    11.1.6.2 The VE from the coke oven doors or from the leveler bar; or
    11.1.6.3 The VE that drift from the top of a larry car hopper if the 
emissions had already been timed as VE from the drop sleeve.
    Note: When the slide gate on a larry car hopper closes after the 
coal has been added to the oven, the seal may not be airtight. On 
occasions, a puff of smoke observed at the drop sleeves is forced past 
the slide gate up into the larry car hopper and may drift from the top; 
time these VE either at the drop sleeves or the hopper. If the larry car 
hopper does not have a slide gate or the slide gate is left open or 
partially closed, VE may quickly pass through the larry car hopper 
without being observed at the drop sleeves and will appear as a strong 
surge of smoke; time these as charging VE.

[[Page 157]]

    11.1.7 Total Time Record. Record the total time that VE were 
observed for each charging operation in the appropriate column on the 
charging system inspection sheet.
    11.1.8 Determination of Validity of a Set of Observations. Five 
charging observations (runs) obtained in accordance with this method 
shall be considered a valid set of observations for that day. No 
observation of an incomplete charge shall be included in a daily set of 
observations that is lower than the lowest reading for a complete 
charge. If both complete and incomplete charges have been observed, the 
daily set of observations shall include the five highest values 
observed. Four or three charging observations (runs) obtained in 
accordance with this method shall be considered a valid set of charging 
observations only where it is not possible to obtain five charging 
observations, because visual interferences (see Section 11.1.5) or 
inclement weather prevent a clear view of the charging system during 
charging. However, observations from three or four charges that satisfy 
these requirements shall not be considered a valid set of charging 
observations if use of such set of observations in a calculation under 
Section 12.4 would cause the value of A to be less than 145.
    11.1.9 Log Average. For each day on which a valid daily set of 
observations is obtained, calculate the daily 30-day rolling log average 
of seconds of visible emissions from the charging operation for each 
battery using these data and the 29 previous valid daily sets of 
observations, in accordance with Section 12.4.
    11.2. Procedure for Determining VE from Coke Oven Door Areas. The 
intent of this procedure is to determine VE from coke oven door areas by 
carefully observing the door area from a standard distance while walking 
at a normal pace.
    11.2.1 Number of Runs. Refer to Sec. 63.309(c)(1) of this part for 
the appropriate number of runs.
    11.2.2 Battery Traverse. To conduct a battery traverse, walk the 
length of the battery on the outside of the pusher machine and quench 
car tracks at a steady, normal walking pace, pausing to make appropriate 
entries on the door area inspection sheet (Figure 303-2). A single test 
run consists of two timed traverses, one for the coke side and one for 
the push side. The walking pace shall be such that the duration of the 
traverse does not exceed an average of 4 seconds per oven door, 
excluding time spent moving around stationary obstructions or waiting 
for other obstructions to move from positions blocking the view of a 
series of doors. Extra time is allowed for each leak (a maximum of 10 
additional seconds for each leaking door) for the observer to make the 
proper notation. A walking pace of 3 seconds per oven door has been 
found to be typical. Record the actual traverse time with a stopwatch.
    11.2.2.1 Include in the traverse time only the time spent observing 
the doors and recording door leaks. To measure actual traverse time, use 
an accumulative-type stopwatch with unit divisions of 0.5 seconds or 
less. Exclude interruptions to the traverse and time required for the 
observer to move to positions where the view of the battery is 
unobstructed, or for obstructions, such as the door machine, to move 
from positions blocking the view of a series of doors.
    11.2.2.2 Various situations may arise that will prevent the observer 
from viewing a door or a series of doors. Prior to the door inspection, 
the owner or operator may elect to temporarily suspend charging 
operations for the duration of the inspection, so that all of the doors 
can be viewed by the observer. The observer has two options for dealing 
with obstructions to view: (a) Stop the stopwatch and wait for the 
equipment to move or the fugitive emissions to dissipate before 
completing the traverse; or (b) stop the stopwatch, skip the affected 
ovens, and move to an unobstructed position to continue the traverse. 
Restart the stopwatch and continue the traverse. After the completion of 
the traverse, if the equipment has moved or the fugitive emissions have 
dissipated, inspect the affected doors. If the equipment is still 
preventing the observer from viewing the doors, then the affected doors 
may be counted as not observed. If option (b) is used because of doors 
blocked by machines during charging operations, then, of the affected 
doors, exclude the door from the most recently charged oven from the 
inspection. Record the oven numbers and make an appropriate notation 
under ``Comments'' on the door area inspection sheet (Figure 303-2).
    11.2.2.3 When batteries have sheds to control emissions, conduct the 
inspection from outside the shed unless the doors cannot be adequately 
viewed. In this case, conduct the inspection from the bench. Be aware of 
special safety considerations pertinent to walking on the bench and 
follow the instructions of company personnel on the required equipment 
and procedures. If possible, conduct the bench traverse whenever the 
bench is clear of the door machine and hot coke guide.
    11.2.3 Observations. Record all the information requested at the top 
of the door area inspection sheet (Figure 303-2), including the number 
of non-operating ovens. Record the clock time at the start of the 
traverse on each side of the battery. Record which side is being 
inspected (i.e., coke side or push side). Other information may be 
recorded at the discretion of the observer, such as the location of the 
leak (e.g., top of the door, chuck door, etc.), the reason for any 
interruption of the traverse, or the position of the sun relative to the 
battery and sky conditions (e.g., overcast, partly sunny, etc.).

[[Page 158]]

    11.2.3.1 Begin the test run by starting the stopwatch and traversing 
either the coke side or the push side of the battery. After completing 
one side, stop the watch. Complete this procedure on the other side. If 
inspecting more than one battery, the observer may view the push sides 
and the coke sides sequentially.
    11.2.3.2 During the traverse, look around the entire perimeter of 
each oven door. The door is considered leaking if VE are detected in the 
coke oven door area. The coke oven door area includes the entire area on 
the vertical face of a coke oven between the bench and the top of the 
battery between two adjacent buck stays (e.g., the oven door, chuck 
door, between the masonry brick, buck stay or jamb, or other sources). 
Record the oven number and make the appropriate notation on the door 
area inspection sheet (Figure 303-2).

    Note: Multiple VE from the same door area (e.g., VE from both the 
chuck door and the push side door) are counted as only one emitting 
door, not as multiple emitting doors.

    11.2.3.3 Do not record the following sources as door area VE:
    11.2.3.3.1 VE from ovens with doors removed. Record the oven number 
and make an appropriate notation under ``Comments;''
    11.2.3.3.2 VE from ovens taken out of service. The owner or operator 
shall notify the observer as to which ovens are out of service. Record 
the oven number and make an appropriate notation under ``Comments;'' or
    11.2.3.3.3 VE from hot coke that has been spilled on the bench as a 
result of pushing.
    11.2.4 Criteria for Acceptance. After completing the run, calculate 
the maximum time allowed to observe the ovens using the equation in 
Section 12.2. If the total traverse time exceeds T, void the run, and 
conduct another run to satisfy the requirements of Sec. 63.309(c)(1) of 
this part.
    11.2.5 Percent Leaking Doors. For each day on which a valid 
observation is obtained, calculate the daily 30-day rolling average for 
each battery using these data and the 29 previous valid daily 
observations, in accordance with Section 12.5.
    11.3 Procedure for Determining VE from Topside Port Lids and Offtake 
Systems.
    11.3.1 Number of Runs. Refer to Sec. 63.309(c)(1) of this part for 
the number of runs to be conducted. Simultaneous runs or separate runs 
for the topside port lids and offtake systems may be conducted.
    11.3.2 Battery Traverse. To conduct a topside traverse of the 
battery, walk the length of the battery at a steady, normal walking 
pace, pausing only to make appropriate entries on the topside inspection 
sheet (Figure 303-3). The walking pace shall not exceed an average rate 
of 4 seconds per oven, excluding time spent moving around stationary 
obstructions or waiting for other obstructions to move from positions 
blocking the view. Extra time is allowed for each leak for the observer 
to make the proper notation. A walking pace of 3 seconds per oven is 
typical. Record the actual traverse time with a stopwatch.
    11.3.3 Topside Port Lid Observations. To observe lids of the ovens 
involved in the charging operation, the observer shall wait to view the 
lids until approximately 5 minutes after the completion of the charge. 
Record all the information requested on the topside inspection sheet 
(Figure 303-3). Record the clock time when traverses begin and end. If 
the observer's view is obstructed during the traverse (e.g., steam from 
the coke wharf, larry car, etc.), follow the guidelines given in Section 
11.2.2.2.
    11.3.3.1 To perform a test run, conduct a single traverse on the 
topside of the battery. The observer shall walk near the center of the 
battery but may deviate from this path to avoid safety hazards (such as 
open or closed charging ports, luting buckets, lid removal bars, and 
topside port lids that have been removed) and any other obstacles. Upon 
noting VE from the topside port lid(s) of an oven, record the oven 
number and port number, then resume the traverse. If any oven is 
dampered-off from the collecting main for decarbonization, note this 
under ``Comments'' for that particular oven.

    Note: Count the number of topside ports, not the number of points, 
exhibiting VE, i.e., if a topside port has several points of VE, count 
this as one port exhibiting VE.

    11.3.3.2 Do not count the following as topside port lid VE:
    11.3.3.2.1 VE from between the brickwork and oven lid casing or VE 
from cracks in the oven brickwork. Note these VE under ``Comments;''
    11.3.3.2.2 VE from topside ports involved in a charging operation. 
Record the oven number, and make an appropriate notation (e.g., not 
observed because ports open for charging) under ``Comments;''
    11.3.3.2.3 Topside ports having maintenance work done. Record the 
oven number and make an appropriate notation under ``Comments;'' or
    11.3.3.2.4 Condensing water from wet-sealing material. Ports with 
only visible condensing water from wet-sealing material are counted as 
observed but not as having VE.
    11.3.3.2.5 Visible emissions from the flue inspection ports and 
caps.
    11.3.4 Offtake Systems Observations. To perform a test run, traverse 
the battery as in Section 11.3.3.1. Look ahead and back two to four 
ovens to get a clear view of the entire offtake system for each oven. 
Consider visible emissions from the following points as offtake system 
VE: (a) the flange between the gooseneck and collecting main 
(``saddle''),

[[Page 159]]

(b) the junction point of the standpipe and oven (``standpipe base''), 
(c) the other parts of the offtake system (e.g., the standpipe cap), and 
(d) the junction points with ovens and flanges of jumper pipes.
    11.3.4.1 Do not stray from the traverse line in order to get a 
``closer look'' at any part of the offtake system unless it is to 
distinguish leaks from interferences from other sources or to avoid 
obstacles.
    11.3.4.2 If the centerline does not provide a clear view of the 
entire offtake system for each oven (e.g., when standpipes are longer 
than 15 feet), the observer may conduct the traverse farther from 
(rather than closer to) the offtake systems.
    11.3.4.3 Upon noting a leak from an offtake system during a 
traverse, record the oven number. Resume the traverse. If the oven is 
dampered-off from the collecting main for decarbonization and VE are 
observed, note this under ``Comments'' for that particular oven.
    11.3.4.4 If any part or parts of an offtake system have VE, count it 
as one emitting offtake system. Each stationary jumper pipe is 
considered a single offtake system.
    11.3.4.5 Do not count standpipe caps open for a decarbonization 
period or standpipes of an oven being charged as source of offtake 
system VE. Record the oven number and write ``Not observed'' and the 
reason (i.e., decarb or charging) under ``Comments.''

    Note: VE from open standpipes of an oven being charged count as 
charging emissions. All VE from closed standpipe caps count as offtake 
leaks.

    11.3.5 Criteria for Acceptance. After completing the run (allow 2 
traverses for batteries with double mains), calculate the maximum time 
allowed to observe the topside port lids and/or offtake systems using 
the equation in Section 12.3. If the total traverse time exceeds T, void 
the run and conduct another run to satisfy the requirements of Sec. 
63.309(c)(1) of this part.
    11.3.6 In determining the percent leaking topside port lids and 
percent leaking offtake systems, do not include topside port lids or 
offtake systems with VE from the following ovens:
    11.3.6.1 Empty ovens, including ovens undergoing maintenance, which 
are properly dampered off from the main.
    11.3.6.2 Ovens being charged or being pushed.
    11.3.6.3 Up to 3 full ovens that have been dampered off from the 
main prior to pushing.
    11.3.6.4 Up to 3 additional full ovens in the pushing sequence that 
have been dampered off from the main for offtake system cleaning, for 
decarbonization, for safety reasons, or when a charging/pushing schedule 
involves widely separated ovens (e.g., a Marquard system); or that have 
been dampered off from the main for maintenance near the end of the 
coking cycle. Examples of reasons that ovens are dampered off for safety 
reasons are to avoid exposing workers in areas with insufficient 
clearance between standpipes and the larry car, or in areas where 
workers could be exposed to flames or hot gases from open standpipes, 
and to avoid the potential for removing a door on an oven that is not 
dampered off from the main.
    11.3.7 Percent Leaking Topside Port Lids and Offtake Systems. For 
each day on which a valid observation is obtained, calculate the daily 
30-day rolling average for each battery using these data and the 29 
previous valid daily observations, in accordance with Sections 12.6 and 
12.7.
    11.4 Procedure for Determining VE from Collecting Mains.
    11.4.1 Traverse. To perform a test run, traverse both the collecting 
main catwalk and the battery topside along the side closest to the 
collecting main. If the battery has a double main, conduct two sets of 
traverses for each run, i.e., one set for each main.
    11.4.2 Data Recording. Upon noting VE from any portion of a 
collection main, identify the source and approximate location of the 
source of VE and record the time under ``Collecting main'' on Figure 
303-3; then resume the traverse.
    11.4.3 Collecting Main Pressure Check. After the completion of the 
door traverse, the topside port lids, and offtake systems, compare the 
collecting main pressure during the inspection to the collecting main 
pressure during the previous 8 to 24 hours. Record the following: (a) 
the pressure during inspection, (b) presence of pressure deviation from 
normal operations, and (c) the explanation for any pressure deviation 
from normal operations, if any, offered by the operators. The owner or 
operator of the coke battery shall maintain the pressure recording 
equipment and conduct the quality assurance/quality control (QA/QC) 
necessary to ensure reliable pressure readings and shall keep the QA/QC 
records for at least 6 months. The observer may periodically check the 
QA/QC records to determine their completeness. The owner or operator 
shall provide access to the records within 1 hour of an observer's 
request.

                   12.0 Data Analysis and Calculations

    12.1 Nomenclature.

A = 150 or the number of valid observations (runs). The value of A shall 
not be less than 145, except for purposes of determinations under Sec. 
63.306(c) (work practice plan implementation) or Sec. 63.306(d) (work 
practice plan revisions) of this part. No set of observations shall be 
considered valid for such a recalculation that otherwise would not be 
considered a valid set of observations for a calculation under this 
paragraph.

[[Page 160]]

Di = Number of doors on non-operating ovens.
Dno = Number of doors not observed.
Dob = Total number of doors observed on operating ovens.
Dt = Total number of oven doors on the battery.
e = 2.72
J = Number of stationary jumper pipes.
L = Number of doors with VE.
Lb = Yard-equivalent reading.
Ls = Number of doors with VE observed from the bench under 
sheds.
Ly = Number of doors with VE observed from the yard.
Ly = Number of doors with VE observed from the yard on the 
push side.
ln = Natural logarithm.
N = Total number of ovens in the battery.
Ni = Total number of inoperable ovens.
PNO = Number of ports not observed.
Povn = Number of ports per oven.
PVE = Number of topside port lids with VE.
PLD = Percent leaking coke oven doors for the test run.
PLL = Percent leaking topside port lids for the run.
PLO = Percent leaking offtake systems.
T = Total time allowed for traverse, seconds.
Tovn = Number of offtake systems (excluding jumper pipes) per 
oven.
TNO = Number of offtake systems not observed.
TVE = Number of offtake systems with VE.
Xi = Seconds of VE during the ith charge.
Z = Number of topside port lids or offtake systems with VE.

    12.2 Criteria for Acceptance for VE Determinations from Coke Oven 
Door Areas. After completing the run, calculate the maximum time allowed 
to observe the ovens using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.535

    12.3 Criteria for Acceptance for VE Determinations from Topside Port 
Lids and Offtake Systems. After completing the run (allow 2 traverses 
for batteries with double mains), calculate the maximum time allowed to 
observe the topside port lids and/or offtake systems by the following 
equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.536

    12.4 Average Duration of VE from Charging Operations. Use Equation 
303-3 to calculate the daily 30-day rolling log average of seconds of 
visible emissions from the charging operation for each battery using 
these current day's observations and the 29 previous valid daily sets of 
observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.537

    12.5 Percent Leaking Doors (PLD). Determine the total number of 
doors for which observations were made on the coke oven battery as 
follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.538

    12.5.1 For each test run (one run includes both the coke side and 
the push side traverses), sum the number of doors with door area VE. For 
batteries subject to an approved alternative standard under Sec. 63.305 
of this part, calculate the push side and the coke side PLD separately.
    12.5.2 Calculate percent leaking doors by using Equation 303-5:

[[Page 161]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.539

    12.5.3 When traverses are conducted from the bench under sheds, 
calculate the coke side and the push side separately. Use Equation 303-6 
to calculate a yard-equivalent reading:
[GRAPHIC] [TIFF OMITTED] TR17OC00.540

If Lb is less than zero, use zero for Lb in 
Equation 303-7 in the calculation of PLD.
    12.5.3.1 Use Equation 303-7 to calculate PLD:
    [GRAPHIC] [TIFF OMITTED] TR17OC00.541
    
Round off PLD to the nearest hundredth of 1 percent and record as the 
percent leaking coke oven doors for the run.
    12.5.3.2 Average Percent Leaking Doors. Use Equation 303-8 to 
calculate the daily 30-day rolling average percent leaking doors for 
each battery using these current day's observations and the 29 previous 
valid daily sets of observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.542

    12.6 Topside Port Lids. Determine the percent leaking topside port 
lids for each run as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.543

    12.6.1 Round off this percentage to the nearest hundredth of 1 
percent and record this percentage as the percent leaking topside port 
lids for the run.
    12.6.2 Average Percent Leaking Topside Port Lids. Use Equation 303-
10 to calculate the daily 30-day rolling average percent leaking topside 
port lids for each battery using these current day's observations and 
the 29 previous valid daily sets of observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.544


[[Page 162]]


    12.7 Offtake Systems. Determine the percent leaking offtake systems 
for the run as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.545

    12.7.1 Round off this percentage to the nearest hundredth of 1 
percent and record this percentage as the percent leaking offtake 
systems for the run.
    12.7.2 Average Percent Leaking Offtake Systems. Use Equation 303-12 
to calculate the daily 30-day rolling average percent leaking offtake 
systems for each battery using these current day's observations and the 
29 previous valid daily sets of observations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.546

                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                            16.0 References.

    1. Missan, R., and A. Stein. Guidelines for Evaluation of Visible 
Emissions Certification, Field Procedures, Legal Aspects, and Background 
Material. U.S. Environmental Protection Agency. EPA Publication No. EPA-
340/1-75-007. April 1975.
    2. Wohlschlegel, P., and D. E. Wagoner. Guideline for Development of 
a Quality Assurance Program: Volume IX--Visual Determination of Opacity 
Emission from Stationary Sources. U.S. Environmental Protection Agency. 
EPA Publication No. EPA-650/4-74-005i. November 1975.
    3. U.S. Occupational Safety and Health Administration. Code of 
Federal Regulations. Title 29, Chapter XVII, Section 1910.1029(g). 
Washington, D.C. Government Printing Office. July 1, 1990.
    4. U.S. Environmental Protection Agency. National Emission Standards 
for Hazardous Air Pollutants; Coke Oven Emissions from Wet-Coal Charged 
By-Product Coke Oven Batteries; Proposed Rule and Notice of Public 
Hearing. Washington, D.C. Federal Register. Vol. 52, No. 78 (13586). 
April 23, 1987.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data

Company name:___________________________________________________________
Battery no.: ------ Date: ------ Run no.: ------
City, State:____________________________________________________________
Observer name:__________________________________________________________
Company representative(s):______________________________________________

----------------------------------------------------------------------------------------------------------------
                                                                           Visible
           Charge No.                 Oven  No.        Clock time        emissions,              Comments
                                                                           seconds
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                Figure 303-1. Charging System Inspection

Company name:___________________________________________________________
Battery no.:____________________________________________________________
Date:___________________________________________________________________
City, State:____________________________________________________________
Total no. of ovens in battery:__________________________________________
Observer name:__________________________________________________________
Certification expiration date:__________________________________________
Inoperable ovens:_______________________________________________________
Company representative(s):______________________________________________
Traverse time CS:_______________________________________________________
Traverse time PS:_______________________________________________________
Valid run (Y or N):_____________________________________________________

----------------------------------------------------------------------------------------------------------------
                                                                          Comments  (No. of blocked doors,
      Time traverse started/completed         PS/CS      Door No.         interruptions to traverse, etc.)
----------------------------------------------------------------------------------------------------------------
 
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[[Page 164]]

                   Figure 303-2. Door Area Inspection.

Company name:___________________________________________________________
Battery no.:____________________________________________________________
Date:___________________________________________________________________
City, State:____________________________________________________________
Total no. of ovens in battery:__________________________________________
Observer name:__________________________________________________________
Certification expiration date:__________________________________________
Inoperable ovens:_______________________________________________________
Company representative(s):______________________________________________
Total no. of lids:______________________________________________________
Total no. of offtakes:__________________________________________________
Total no. of jumper pipes:______________________________________________
Ovens not observed:_____________________________________________________
Total traverse time:____________________________________________________
Valid run (Y or N):_____________________________________________________

----------------------------------------------------------------------------------------------------------------
                                    Type of Inspection
 Time traverse started/completed     (lids, offtakes,     Location of VE  (Oven /        Comments
                                     collecting main)             Port )
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                    Figure 303-3. Topside Inspection

 Method 303A--Determination of Visible Emissions From Nonrecovery Coke 
                             Oven Batteries

    Note: This method does not include all of the specifications 
pertaining to observer certification. Some material is incorporated by 
reference from other methods in this part and in appendix A to 40 CFR 
Part 60. Therefore, to obtain reliable results, persons using this 
method should have a thorough knowledge of Method 9 and Method 303.

                        1.0 Scope and Application

    1.1 Applicability. This method is applicable for the determination 
of visible emissions (VE) from leaking doors at nonrecovery coke oven 
batteries.

[[Page 165]]

                          2.0 Summary of Method

    2.1 A certified observer visually determines the VE from coke oven 
battery sources while walking at a normal pace. This method does not 
require that opacity of emissions be determined or that magnitude be 
differentiated.

                             3.0 Definitions

    3.1 Bench means the platform structure in front of the oven doors.
    3.2 Coke oven door means each end enclosure on the push side and the 
coking side of an oven.
    3.3 Coke side means the side of a battery from which the coke is 
discharged from ovens at the end of the coking cycle.
    3.4 Nonrecovery coke oven battery means a source consisting of a 
group of ovens connected by common walls and operated as a unit, where 
coal undergoes destructive distillation under negative pressure to 
produce coke, and which is designed for the combustion of coke oven gas 
from which by-products are not recovered.
    3.5 Operating oven means any oven not out of operation for rebuild 
or maintenance work extensive enough to require the oven to be skipped 
in the charging sequence.
    3.6 Oven means a chamber in the coke oven battery in which coal 
undergoes destructive distillation to produce coke.
    3.7 Push side means the side of the battery from which the coke is 
pushed from ovens at the end of the coking cycle.
    3.8 Run means the observation of visible emissions from coke oven 
doors in accordance with this method.
    3.9 Shed means an enclosure that covers the side of the coke oven 
battery, captures emissions from pushing operations and from leaking 
coke oven doors on the coke side or push side of the coke oven battery, 
and routes the emissions to a control device or system.
    3.10 Traverse time means accumulated time for a traverse as measured 
by a stopwatch. Traverse time includes time to stop and write down oven 
numbers but excludes time waiting for obstructions of view to clear or 
for time to walk around obstacles.
    3.11 Visible Emissions or VE means any emission seen by the unaided 
(except for corrective lenses) eye, excluding steam or condensing water.

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method may not address all of the 
safety problems associated with its use. It is the responsibility of the 
user of this test method to establish appropriate safety and health 
practices and determine the applicability of regulatory limitations 
prior to performing this test method.
    5.2 Safety Training. Because coke oven batteries have hazardous 
environments, the training materials and the field training (Section 
10.0) shall cover the precautions required by the company to address 
health and safety hazards. Special emphasis shall be given to the 
Occupational Safety and Health Administration (OSHA) regulations 
pertaining to exposure of coke oven workers (see Reference 3 in Section 
16.0). In general, the regulation requires that special fire-retardant 
clothing and respirators be worn in certain restricted areas of the coke 
oven battery. The OSHA regulation also prohibits certain activities, 
such as chewing gum, smoking, and eating in these areas.

                 6.0 Equipment and Supplies. [Reserved]

                 7.0 Reagents and Standards. [Reserved]

 8.0 Sample Collection, Preservation, Transport, and Storage. [Reserved]

                     9.0 Quality Control. [Reserved]

                  10.0 Calibration and Standardization.

    10.1 Training. This method requires only the determination of 
whether VE occur and does not require the determination of opacity 
levels; therefore, observer certification according to Method 9 in 
Appendix A to Part 60 is not required. However, the first-time observer 
(trainee) shall have attended the lecture portion of the Method 9 
certification course. Furthermore, before conducting any VE 
observations, an observer shall become familiar with nonrecovery coke 
oven battery operations and with this test method by observing for a 
minimum of 4 hours the operation of a nonrecovery coke oven battery in 
the presence of personnel experienced in performing Method 303 
assessments.

                             11.0 Procedure

    The intent of this procedure is to determine VE from coke oven door 
areas by carefully observing the door area while walking at a normal 
pace.
    11.1 Number of Runs. Refer to Sec. 63.309(c)(1) of this part for 
the appropriate number of runs.
    11.2 Battery Traverse. To conduct a battery traverse, walk the 
length of the battery on the outside of the pusher machine and quench 
car tracks at a steady, normal walking pace, pausing to make appropriate 
entries on the door area inspection sheet (Figure 303A-1). The walking 
pace shall be such that the duration of the traverse does not exceed an 
average of 4 seconds per oven door, excluding time spent moving around 
stationary obstructions or waiting for other obstructions to move from 
positions blocking the view of a series of doors. Extra time is

[[Page 166]]

allowed for each leak (a maximum of 10 additional seconds for each 
leaking door) for the observer to make the proper notation. A walking 
pace of 3 seconds per oven door has been found to be typical. Record the 
actual traverse time with a stopwatch. A single test run consists of two 
timed traverses, one for the coke side and one for the push side.
    11.2.1 Various situations may arise that will prevent the observer 
from viewing a door or a series of doors. The observer has two options 
for dealing with obstructions to view: (a) Wait for the equipment to 
move or the fugitive emissions to dissipate before completing the 
traverse; or (b) skip the affected ovens and move to an unobstructed 
position to continue the traverse. Continue the traverse. After the 
completion of the traverse, if the equipment has moved or the fugitive 
emissions have dissipated, complete the traverse by inspecting the 
affected doors. Record the oven numbers and make an appropriate notation 
under ``Comments'' on the door area inspection sheet (Figure 303A-1).

    Note: Extra time incurred for handling obstructions is not counted 
in the traverse time.

    11.2.2 When batteries have sheds to control pushing emissions, 
conduct the inspection from outside the shed, if the shed allows such 
observations, or from the bench. Be aware of special safety 
considerations pertinent to walking on the bench and follow the 
instructions of company personnel on the required equipment and 
operations procedures. If possible, conduct the bench traverse whenever 
the bench is clear of the door machine and hot coke guide.
    11.3 Observations. Record all the information requested at the top 
of the door area inspection sheet (Figure 303A-1), including the number 
of non-operating ovens. Record which side is being inspected, i.e., coke 
side or push side. Other information may be recorded at the discretion 
of the observer, such as the location of the leak (e.g., top of the 
door), the reason for any interruption of the traverse, or the position 
of the sun relative to the battery and sky conditions (e.g., overcast, 
partly sunny, etc.).
    11.3.1 Begin the test run by traversing either the coke side or the 
push side of the battery. After completing one side, traverse the other 
side.
    11.3.2 During the traverse, look around the entire perimeter of each 
oven door. The door is considered leaking if VE are detected in the coke 
oven door area. The coke oven door area includes the entire area on the 
vertical face of a coke oven between the bench and the top of the 
battery and the adjacent doors on both sides. Record the oven number and 
make the appropriate notation on the door area inspection sheet (Figure 
303A-1).
    11.3.3 Do not record the following sources as door area VE:
    11.3.3.1 VE from ovens with doors removed. Record the oven number 
and make an appropriate notation under ``Comments'';
    11.3.3.2 VE from ovens where maintenance work is being conducted. 
Record the oven number and make an appropriate notation under 
``Comments''; or
    11.3.3.3 VE from hot coke that has been spilled on the bench as a 
result of pushing.

                   12.0 Data Analysis and Calculations

    Same as Method 303, Section 12.1, 12.2, 12.3, 12.4, and 12.5.

                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                             16.0 References

    Same as Method 303, Section 16.0.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data

Company name:___________________________________________________________
Battery no.:____________________________________________________________
Date:___________________________________________________________________
City, State:____________________________________________________________
Total no. of ovens in battery:__________________________________________
Observer name:__________________________________________________________
Certification expiration date:__________________________________________
Inoperable ovens:_______________________________________________________
Company representative(s):______________________________________________
Traverse time CS:_______________________________________________________
Traverse time PS:_______________________________________________________
Valid run (Y or N):_____________________________________________________

----------------------------------------------------------------------------------------------------------------
                                                                          Comments  (No. of blocked doors,
      Time traverse started/completed         PS/CS      Door No.         interruptions to traverse, etc.)
----------------------------------------------------------------------------------------------------------------
 
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                   Figure 303A-1. Door Area Inspection

Method 304A: Determination of Biodegradation Rates of Organic Compounds 
                              (Vent Option)

                        1.0 Scope and Application

    1.1 Applicability. This method is applicable for the determination 
of biodegradation rates of organic compounds in an activated sludge 
process. The test method is designed to evaluate the ability of an 
aerobic biological reaction system to degrade or destroy specific 
components in waste streams. The method may also be used to determine 
the effects of changes in wastewater composition on operation. The 
biodegradation rates determined by utilizing this method are not 
representative of a full-scale system. The rates measured by this method 
shall be used in conjunction with the procedures listed in appendix C of 
this part to calculate the fraction emitted to the air versus the 
fraction biodegraded.

                          2.0 Summary of Method

    2.1 A self-contained benchtop bioreactor system is assembled in the 
laboratory. A sample of mixed liquor is added and the waste stream is 
then fed continuously. The benchtop bioreactor is operated under 
conditions nearly identical to the target full-scale activated sludge 
process. Bioreactor temperature, dissolved oxygen concentration, average 
residence time in the reactor, waste composition, biomass concentration, 
and biomass composition of the full-scale process are the parameters 
which are duplicated in the benchtop bioreactor. Biomass shall be 
removed from the target full-scale activated sludge unit and held for no 
more than 4 hours prior to use in the benchtop bioreactor. If 
antifoaming agents are used in the full-scale system, they shall also be 
used in the benchtop bioreactor. The feed flowing into and the effluent 
exiting the benchtop bioreactor are analyzed to determine the 
biodegradation rates of the target compounds. The flow rate of the exit 
vent is used to calculate the concentration of target compounds 
(utilizing Henry's law) in the exit gas stream. If Henry's law constants 
for the compounds of interest are not known, this method cannot be used 
in the determination of the biodegradation rate and Method 304B is the 
suggested method. The choice of analytical methodology for measuring the 
compounds of interest at the inlet and outlet to the benchtop bioreactor 
are left to the discretion of the source, except where validated methods 
are available.

[[Page 168]]

                       3.0 Definitions. [Reserved]

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 If explosive gases are produced as a byproduct of biodegradation 
and could realistically pose a hazard, closely monitor headspace 
concentration of these gases to ensure laboratory safety. Placement of 
the benchtop bioreactor system inside a laboratory hood is recommended 
regardless of byproducts produced.

                       6.0. Equipment and Supplies

    Note: Figure 304A-1 illustrates a typical laboratory apparatus used 
to measure biodegradation rates. While the following description refers 
to Figure 304A-1, the EPA recognizes that alternative reactor 
configurations, such as alternative reactor shapes and locations of 
probes and the feed inlet, will also meet the intent of this method. 
Ensure that the benchtop bioreactor system is self-contained and 
isolated from the atmosphere (except for the exit vent stream) by leak-
checking fittings, tubing, etc.

    6.1 Benchtop Bioreactor. The biological reaction is conducted in a 
biological oxidation reactor of at least 6 liters capacity. The benchtop 
bioreactor is sealed and equipped with internal probes for controlling 
and monitoring dissolved oxygen and internal temperature. The top of the 
reactor is equipped for aerators, gas flow ports, and instrumentation 
(while ensuring that no leaks to the atmosphere exist around the 
fittings).
    6.2 Aeration gas. Aeration gas is added to the benchtop bioreactor 
through three diffusers, which are glass tubes that extend to the bottom 
fifth of the reactor depth. A pure oxygen pressurized cylinder is 
recommended in order to maintain the specified oxygen concentration. 
Install a blower (e.g., Diaphragm Type, 15 SCFH capacity) to blow the 
aeration gas into the reactor diffusers. Measure the aeration gas flow 
rate with a rotameter (e.g., 0-15 SCFH recommended). The aeration gas 
will rise through the benchtop bioreactor, dissolving oxygen into the 
mixture in the process. The aeration gas must provide sufficient 
agitation to keep the solids in suspension. Provide an exit for the 
aeration gas from the top flange of the benchtop bioreactor through a 
water-cooled (e.g., Allihn-type) vertical condenser. Install the 
condenser through a gas-tight fitting in the benchtop bioreactor 
closure. Install a splitter which directs a portion of the gas to an 
exit vent and the rest of the gas through an air recycle pump back to 
the benchtop bioreactor. Monitor and record the flow rate through the 
exit vent at least 3 times per day throughout the day.
    6.3 Wastewater Feed. Supply the wastewater feed to the benchtop 
bioreactor in a collapsible low-density polyethylene container or 
collapsible liner in a container (e.g., 20 L) equipped with a spigot cap 
(collapsible containers or liners of other material may be required due 
to the permeability of some volatile compounds through polyethylene). 
Obtain the wastewater feed by sampling the wastewater feed in the target 
process. A representative sample of wastewater shall be obtained from 
the piping leading to the aeration tank. This sample may be obtained 
from existing sampling valves at the discharge of the wastewater feed 
pump, or collected from a pipe discharging to the aeration tank, or by 
pumping from a well-mixed equalization tank upstream from the aeration 
tank. Alternatively, wastewater can be pumped continuously to the 
laboratory apparatus from a bleed stream taken from the equalization 
tank of the full-scale treatment system.
    6.3.1 Refrigeration System. Keep the wastewater feed cool by ice or 
by refrigeration to 4 [deg]C. If using a bleed stream from the 
equalization tank, refrigeration is not required if the residence time 
in the bleed stream is less than five minutes.
    6.3.2 Wastewater Feed Pump. The wastewater is pumped from the 
refrigerated container using a variable-speed peristaltic pump drive 
equipped with a peristaltic pump head. Add the feed solution to the 
benchtop bioreactor through a fitting on the top flange. Determine the 
rate of feed addition to provide a retention time in the benchtop 
bioreactor that is numerically equivalent to the retention time in the 
full-scale system. The wastewater shall be fed at a rate sufficient to 
achieve 90 to 100 percent of the full-scale system residence time.
    6.3.3 Treated wastewater feed. The benchtop bioreactor effluent 
exits at the bottom of the reactor through a tube and proceeds to the 
clarifier.
    6.4 Clarifier. The effluent flows to a separate closed clarifier 
that allows separation of biomass and effluent (e.g., 2-liter pear-
shaped glass separatory funnel, modified by removing the stopcock and 
adding a 25-mm OD glass tube at the bottom). Benchtop bioreactor 
effluent enters the clarifier through a tube inserted to a depth of 0.08 
m (3 in.) through a stopper at the top of the clarifier. System effluent 
flows from a tube inserted through the stopper at the top of the 
clarifier to a drain (or sample bottle when sampling). The underflow 
from the clarifier leaves from the glass tube at the bottom of the 
clarifier. Flexible tubing connects this fitting to the sludge recycle 
pump. This pump is coupled to a variable speed pump drive. The discharge 
from this pump is returned through a tube inserted in a port on the side 
of the benchtop bioreactor. An additional port is provided near the 
bottom of the benchtop bioreactor for sampling the reactor contents. The 
mixed liquor from the

[[Page 169]]

benchtop bioreactor flows into the center of the clarifier. The 
clarified system effluent separates from the biomass and flows through 
an exit near the top of the clarifier. There shall be no headspace in 
the clarifier.
    6.5 Temperature Control Apparatus. Capable of maintaining the system 
at a temperature equal to the temperature of the full-scale system. The 
average temperature should be maintained within 2 
[deg]C of the set point.
    6.5.1 Temperature Monitoring Device. A resistance type temperature 
probe or a thermocouple connected to a temperature readout with a 
resolution of 0.1 [deg]C or better.
    6.5.2 Benchtop Bioreactor Heater. The heater is connected to the 
temperature control device.
    6.6 Oxygen Control System. Maintain the dissolved oxygen 
concentration at the levels present in the full-scale system. Target 
full-scale activated sludge systems with dissolved oxygen concentration 
below 2 mg/L are required to maintain the dissolved oxygen concentration 
in the benchtop ioreactor within 0.5 mg/L of the target dissolved oxygen 
level. Target full-scale activated sludge systems with dissolved oxygen 
concentration above 2 mg/L are required to maintain the dissolved oxygen 
concentration in the benchtop bioreactor within 1.5 mg/L of the target 
dissolved oxygen concentration; however, for target full-scale activated 
sludge systems with dissolved oxygen concentrations above 2 mg/L, the 
dissolved oxygen concentration in the benchtop bioreactor may not drop 
below 1.5 mg/L. If the benchtop bioreactor is outside the control range, 
the dissolved oxygen is noted and the reactor operation is adjusted.
    6.6.1 Dissolved Oxygen Monitor. Dissolved oxygen is monitored with a 
polarographic probe (gas permeable membrane) connected to a dissolved 
oxygen meter (e.g., 0 to 15 mg/L, 0 to 50 [deg]C).
    6.6.2 Benchtop Bioreactor Pressure Monitor. The benchtop bioreactor 
pressure is monitored through a port in the top flange of the reactor. 
This is connected to a gauge control with a span of 13-cm water vacuum 
to 13-cm water pressure or better. A relay is activated when the vacuum 
exceeds an adjustable setpoint which opens a solenoid valve (normally 
closed), admitting oxygen to the system. The vacuum setpoint controlling 
oxygen addition to the system shall be set at approximately 2.5  0.5 cm water and maintained at this setting except 
during brief periods when the dissolved oxygen concentration is 
adjusted.
    6.7 Connecting Tubing. All connecting tubing shall be Teflon or 
equivalent in impermeability. The only exception to this specification 
is the tubing directly inside the pump head of the wastewater feed pump, 
which may be Viton, Silicone or another type of flexible tubing.
    Note: Mention of trade names or products does not constitute 
endorsement by the U.S. Environmental Protection Agency.

                       7.0 Reagents and Standards

    7.1 Wastewater. Obtain a representative sample of wastewater at the 
inlet to the full-scale treatment plant if there is an existing full-
scale treatment plant (see section 6.3). If there is no existing full-
scale treatment plant, obtain the wastewater sample as close to the 
point of determination as possible. Collect the sample by pumping the 
wastewater into the 20-L collapsible container. The loss of volatiles 
shall be minimized from the wastewater by collapsing the container 
before filling, by minimizing the time of filling, and by avoiding a 
headspace in the container after filling. If the wastewater requires the 
addition of nutrients to support the biomass growth and maintain biomass 
characteristics, those nutrients are added and mixed with the container 
contents after the container is filled.
    7.2 Biomass. Obtain the biomass or activated sludge used for rate 
constant determination in the bench-scale process from the existing 
full-scale process or from a representative biomass culture (e.g., 
biomass that has been developed for a future full-scale process). This 
biomass is preferentially obtained from a thickened acclimated mixed 
liquor sample. Collect the sample either by bailing from the mixed 
liquor in the aeration tank with a weighted container, or by collecting 
aeration tank effluent at the effluent overflow weir. Transport the 
sample to the laboratory within no more than 4 hours of collection. 
Maintain the biomass concentration in the benchtop bioreactor at the 
level of the full-scale system +10 percent throughout the sampling 
period of the test method.

       8.0 Sample Collection, Preservation, Storage, and Transport

    8.1 Benchtop Bioreactor Operation. Charge the mixed liquor to the 
benchtop bioreactor, minimizing headspace over the liquid surface to 
minimize entrainment of mixed liquor in the circulating gas. Fasten the 
benchtop bioreactor headplate to the reactor over the liquid surface. 
Maintain the temperature of the contents of the benchtop bioreactor 
system at the temperature of the target full-scale system, 2 [deg]C, throughout the testing period. Monitor and 
record the temperature of the benchtop bioreactor contents at least to 
the nearest 0.1 [deg]C.
    8.1.1 Wastewater Storage. Collect the wastewater sample in the 20-L 
collapsible container. Store the container at 4 [deg]C throughout the 
testing period. Connect the container to the benchtop bioreactor feed 
pump.
    8.1.2 Wastewater Flow Rate.

[[Page 170]]

    8.1.2.1 The hydraulic residence time of the aeration tank is 
calculated as the ratio of the volume of the tank (L) to the flow rate 
(L/min). At the beginning of a test, the container shall be connected to 
the feed pump and solution shall be pumped to the benchtop bioreactor at 
the required flow rate to achieve the calculated hydraulic residence 
time of wastewater in the aeration tank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.547

Where:

Qtest = wastewater flow rate (L/min)
Qfs = average flow rate of full-scale process (L/min)
Vfs = volume of full-scale aeration tank (L)

    8.1.2.2 The target flow rate in the test apparatus is the same as 
the flow rate in the target full-scale process multiplied by the ratio 
of benchtop bioreactor volume (e.g., 6 L) to the volume of the full-
scale aeration tank. The hydraulic residence time shall be maintained at 
90 to 100 percent of the residence time maintained in the full-scale 
unit. A nominal flow rate is set on the pump based on a pump 
calibration. Changes in the elasticity of the tubing in the pump head 
and the accumulation of material in the tubing affect this calibration. 
The nominal pumping rate shall be changed as necessary based on 
volumetric flow measurements. Discharge the benchtop bioreactor effluent 
to a wastewater storage, treatment, or disposal facility, except during 
sampling or flow measurement periods.
    8.1.3 Sludge Recycle Rate. Set the sludge recycle rate at a rate 
sufficient to prevent accumulation in the bottom of the clarifier. Set 
the air circulation rate sufficient to maintain the biomass in 
suspension.
    8.1.4 Benchtop Bioreactor Operation and Maintenance. Temperature, 
dissolved oxygen concentration, exit vent flow rate, benchtop bioreactor 
effluent flow rate, and air circulation rate shall be measured and 
recorded three times throughout each day of benchtop bioreactor 
operation. If other parameters (such as pH) are measured and maintained 
in the target full-scale unit, these parameters, where appropriate, 
shall be monitored and maintained to target full-scale specifications in 
the benchtop bioreactor. At the beginning of each sampling period 
(Section 8.2), sample the benchtop bioreactor contents for suspended 
solids analysis. Take this sample by loosening a clamp on a length of 
tubing attached to the lower side port. Determine the suspended solids 
gravimetrically by the Gooch crucible/glass fiber filter method for 
total suspended solids, in accordance with Standard Methods\3\ or 
equivalent. When necessary, sludge shall be wasted from the lower side 
port of the benchtop bioreactor, and the volume that is wasted shall be 
replaced with an equal volume of the reactor effluent. Add thickened 
activated sludge mixed liquor as necessary to the benchtop bioreactor to 
increase the suspended solids concentration to the desired level. Pump 
this mixed liquor to the benchtop bioreactor through the upper side port 
(Item 24 in Figure 304A-1). Change the membrane on the dissolved oxygen 
probe before starting the test. Calibrate the oxygen probe immediately 
before the start of the test and each time the membrane is changed.
    8.1.5 Inspection and Correction Procedures. If the feed line tubing 
becomes clogged, replace with new tubing. If the feed flow rate is not 
within 5 percent of target flow any time the flow rate is measured, 
reset pump or check the flow measuring device and measure flow rate 
again until target flow rate is achieved.
    8.2 Test Sampling. At least two and one half hydraulic residence 
times after the system has reached the targeted specifications shall be 
permitted to elapse before the first sample is taken. Effluent samples 
of the clarifier discharge (Item 20 in Figure 304A-1) and the influent 
wastewater feed are collected in 40-mL septum vials to which two drops 
of 1:10 hydrochloric acid (HCl) in water have been added. Sample the 
clarifier discharge directly from the drain line. These samples will be 
composed of the entire flow from the system for a period of several 
minutes. Feed samples shall be taken from the feed pump suction line 
after temporarily stopping the benchtop bioreactor feed, removing a 
connector, and squeezing the collapsible feed container. Store both 
influent and effluent samples at 4 [deg]C immediately after collection 
and analyze within 8 hours of collection.
    8.2.1 Frequency of Sampling. During the test, sample and analyze the 
wastewater feed and the clarifier effluent at least six times. The 
sampling intervals shall be separated by at least 8 hours. During any 
individual sampling interval, sample the wastewater feed simultaneously 
with or immediately after the effluent sample. Calculate the relative 
standard deviation (RSD) of the amount removed (i.e., effluent 
concentration--wastewater feed concentration). The RSD values shall be < 
15 percent. If an RSD value is  15

[[Page 171]]

percent, continue sampling and analyzing influent and effluent sets of 
samples until the RSD values are within specifications.
    8.2.2 Sampling After Exposure of System to Atmosphere. If, after 
starting sampling procedures, the benchtop bioreactor system is exposed 
to the atmosphere (due to leaks, maintenance, etc.), allow at least one 
hydraulic residence time to elapse before resuming sampling.

                           9.0 Quality Control

    9.1 Dissolved Oxygen. Fluctuation in dissolved oxygen concentration 
may occur for numerous reasons, including undetected gas leaks, 
increases and decreases in mixed liquor suspended solids resulting from 
cell growth and solids loss in the effluent stream, changes in diffuser 
performance, cycling of effluent flow rate, and overcorrection due to 
faulty or sluggish dissolved oxygen probe response. Control the 
dissolved oxygen concentration in the benchtop bioreactor by changing 
the proportion of oxygen in the circulating aeration gas. Should the 
dissolved oxygen concentration drift below the designated experimental 
condition, bleed a small amount of aeration gas from the system on the 
pressure side (i.e., immediately upstream of one of the diffusers). This 
will create a vacuum in the system, triggering the pressure sensitive 
relay to open the solenoid valve and admit oxygen to the system. Should 
the dissolved oxygen concentration drift above the designated 
experimental condition, slow or stop the oxygen input to the system 
until the dissolved oxygen concentration approaches the correct level.
    9.2 Sludge Wasting.
    9.2.1 Determine the suspended solids concentration (section 8.1.4) 
at the beginning of a test, and once per day thereafter during the test. 
If the test is completed within a two day period, determine the 
suspended solids concentration after the final sample set is taken. If 
the suspended solids concentration exceeds the specified concentration, 
remove a fraction of the sludge from the benchtop bioreactor. The 
required volume of mixed liquor to remove is determined as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.548

Where:

Vw is the wasted volume (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sm is the measured solids (g/L), and
Ss is the specified solids (g/L).

    9.2.2 Remove the mixed liquor from the benchtop bioreactor by 
loosening a clamp on the mixed liquor sampling tube and allowing the 
required volume to drain to a graduated flask. Clamp the tube when the 
correct volume has been wasted. Replace the volume of the liquid wasted 
by pouring the same volume of effluent back into the benchtop 
bioreactor. Dispose of the waste sludge properly.
    9.3 Sludge Makeup. In the event that the suspended solids 
concentration is lower than the specifications, add makeup sludge back 
into the benchtop bioreactor. Determine the amount of sludge added by 
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.549

Where:

Vw is the volume of sludge to add (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sw is the solids in the makeup sludge (g/L),
Sm is the measured solids (g/L), and Ss is the 
specified solids (g/L).

                  10.0 Calibration and Standardization

    10.1 Wastewater Pump Calibration. Determine the wastewater flow rate 
by collecting the system effluent for a time period of at least one 
hour, and measuring the volume with a graduated cylinder. Record the 
collection time period and volume collected. Determine flow rate. Adjust 
the pump speed to deliver the specified flow rate.

[[Page 172]]

    10.2 Calibration Standards. Prepare calibration standards from pure 
certified standards in an aqueous medium. Prepare and analyze three 
concentrations of calibration standards for each target component (or 
for a mixture of components) in triplicate daily throughout the analyses 
of the test samples. At each concentration level, a single calibration 
shall be within 5 percent of the average of the three calibration 
results. The low and medium calibration standards shall bracket the 
expected concentration of the effluent (treated) wastewater. The medium 
and high standards shall bracket the expected influent concentration.

                       11.0 Analytical Procedures

    11.1 Analysis. If the identity of the compounds of interest in the 
wastewater is not known, a representative sample of the wastewater shall 
be analyzed in order to identify all of the compounds of interest 
present. A gas chromatography/mass spectrometry screening method is 
recommended.
    11.1.1 After identifying the compounds of interest in the 
wastewater, develop and/or use one or more analytical techniques capable 
of measuring each of those compounds (more than one analytical technique 
may be required, depending on the characteristics of the wastewater). 
Test Method 18, found in appendix A of 40 CFR 60, may be used as a 
guideline in developing the analytical technique. Purge and trap 
techniques may be used for analysis providing the target components are 
sufficiently volatile to make this technique appropriate. The limit of 
quantitation for each compound shall be determined (see reference 1). If 
the effluent concentration of any target compound is below the limit of 
quantitation determined for that compound, the operation of the Method 
304 unit may be altered to attempt to increase the effluent 
concentration above the limit of quantitation. Modifications to the 
method shall be approved prior to the test. The request should be 
addressed to Method 304 contact, Emissions Measurement Center, Mail Drop 
19, U.S. Environmental Protection Agency, Research Triangle Park, NC 
27711.

                   12.0 Data Analysis and Calculations

    12.1 Nomenclature. The following symbols are used in the 
calculations.

Ci = Average inlet feed concentration for a compound of 
interest, as analyzed (mg/L)
Co = Average outlet (effluent) concentration for a compound 
of interest, as analyzed (mg/L)
X = Biomass concentration, mixed liquor suspended solids (g/L)
t = Hydraulic residence time in the benchtop bioreactor (hours)
V = Volume of the benchtop bioreactor (L)
Q = Flow rate of wastewater into the benchtop bioreactor, average (L/
hour)

    12.2 Residence Time. The hydraulic residence time of the benchtop 
bioreactor is equal to the ratio of the volume of the benchtop 
bioreactor (L) to the flow rate (L/h):
[GRAPHIC] [TIFF OMITTED] TR17OC00.550

    12.3 Rate of Biodegradation. Calculate the rate of biodegradation 
for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.551

    12.4 First-Order Biorate Constant. Calculate the first-order biorate 
constant (K1) for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.552

    12.5 Relative Standard Deviation (RSD). Determine the standard 
deviation of both the influent and effluent sample concentrations (S) 
using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.553


[[Page 173]]


    12.6 Determination of Percent Air Emissions and Percent Biodegraded. 
Use the results from this test method and follow the applicable 
procedures in appendix C of 40 CFR part 63, entitled, ``Determination of 
the Fraction Biodegraded (Fbio) in a Biological Treatment 
Unit'' to determine Fbio.

                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                             16.0 References

    1. ``Guidelines for data acquisition and data quality evaluation in 
Environmental Chemistry,'' Daniel MacDoughal, Analytical Chemistry, 
Volume 52, p. 2242, 1980.
    2. Test Method 18, 40 CFR 60, appendix A.
    3. Standard Methods for the Examination of Water and Wastewater, 
16th Edition, Method 209C, Total Suspended Solids Dried at 103-105 
[deg]C, APHA, 1985.
    4. Water7, Hazardous Waste Treatment, Storage, and Disposal 
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection 
Agency, EPA-450/3-87-026, Review Draft, November 1989.
    5. Chemdat7, Hazardous Waste Treatment, Storage, and Disposal 
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection 
Agency, EPA-450/3-87-026, Review Draft, November 1989.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 174]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.554

Method 304B: Determination of Biodegradation Rates of Organic Compounds 
                            (Scrubber Option)

                        1.0 Scope and Application

    1.1 Applicability. This method is applicable for the determination 
of biodegradation rates of organic compounds in an activated sludge 
process. The test method is designed to evaluate the ability of an 
aerobic biological reaction system to degrade or destroy specific 
components in waste streams. The method may also be used to determine 
the effects of changes in wastewater composition on operation. The 
biodegradation rates determined by utilizing this method are not 
representative of a full-scale system. Full-scale systems embody 
biodegradation and air emissions in competing reactions. This method 
measures biodegradation in absence of air emissions. The rates measured 
by this method shall be used in conjunction with the procedures listed 
in appendix C of this part to calculate the fraction emitted to the air 
versus the fraction biodegraded.

[[Page 175]]

                          2.0 Summary of Method

    2.1 A self-contained benchtop bioreactor system is assembled in the 
laboratory. A sample of mixed liquor is added and the waste stream is 
then fed continuously. The benchtop bioreactor is operated under 
conditions nearly identical to the target full-scale activated sludge 
process, except that air emissions are not a factor. The benchtop 
bioreactor temperature, dissolved oxygen concentration, average 
residence time in the reactor, waste composition, biomass concentration, 
and biomass composition of the target full-scale process are the 
parameters which are duplicated in the laboratory system. Biomass shall 
be removed from the target full-scale activated sludge unit and held for 
no more than 4 hours prior to use in the benchtop bioreactor. If 
antifoaming agents are used in the full-scale system, they shall also be 
used in the benchtop bioreactor. The feed flowing into and the effluent 
exiting the benchtop bioreactor are analyzed to determine the 
biodegradation rates of the target compounds. The choice of analytical 
methodology for measuring the compounds of interest at the inlet and 
outlet to the benchtop bioreactor are left to the discretion of the 
source, except where validated methods are available.

                       3.0 Definitions. [Reserved]

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 If explosive gases are produced as a byproduct of biodegradation 
and could realistically pose a hazard, closely monitor headspace 
concentration of these gases to ensure laboratory safety. Placement of 
the benchtop bioreactor system inside a laboratory hood is recommended 
regardless of byproducts produced.

                       6.0 Equipment and Supplies

    Note: Figure 304B-1 illustrates a typical laboratory apparatus used 
to measure biodegradation rates. While the following description refers 
to Figure 304B-1, the EPA recognizes that alternative reactor 
configurations, such as alternative reactor shapes and locations of 
probes and the feed inlet, will also meet the intent of this method. 
Ensure that the benchtop bioreactor system is self-contained and 
isolated from the atmosphere by leak-checking fittings, tubing, etc.
    6.1 Benchtop Bioreactor. The biological reaction is conducted in a 
biological oxidation reactor of at least 6-liters capacity. The benchtop 
bioreactor is sealed and equipped with internal probes for controlling 
and monitoring dissolved oxygen and internal temperature. The top of the 
benchtop bioreactor is equipped for aerators, gas flow ports, and 
instrumentation (while ensuring that no leaks to the atmosphere exist 
around the fittings).
    6.2 Aeration gas. Aeration gas is added to the benchtop bioreactor 
through three diffusers, which are glass tubes that extend to the bottom 
fifth of the reactor depth. A pure oxygen pressurized cylinder is 
recommended in order to maintain the specified oxygen concentration. 
Install a blower (e.g., Diaphragm Type, 15 SCFH capacity) to blow the 
aeration gas into the benchtop bioreactor diffusers. Measure the 
aeration gas flow rate with a rotameter (e.g., 0-15 SCFH recommended). 
The aeration gas will rise through the benchtop bioreactor, dissolving 
oxygen into the mixture in the process. The aeration gas must provide 
sufficient agitation to keep the solids in suspension. Provide an exit 
for the aeration gas from the top flange of the benchtop bioreactor 
through a water-cooled (e.g., Allihn-type) vertical condenser. Install 
the condenser through a gas-tight fitting in the benchtop bioreactor 
closure. Design the system so that at least 10 percent of the gas flows 
through an alkaline scrubber containing 175 mL of 45 percent by weight 
solution of potassium hydroxide (KOH) and 5 drops of 0.2 percent 
alizarin yellow dye. Route the balance of the gas through an adjustable 
scrubber bypass. Route all of the gas through a 1-L knock-out flask to 
remove entrained moisture and then to the intake of the blower. The 
blower recirculates the gas to the benchtop bioreactor.
    6.3 Wastewater Feed. Supply the wastewater feed to the benchtop 
bioreactor in a collapsible low-density polyethylene container or 
collapsible liner in a container (e.g., 20 L) equipped with a spigot cap 
(collapsible containers or liners of other material may be required due 
to the permeability of some volatile compounds through polyethylene). 
Obtain the wastewater feed by sampling the wastewater feed in the target 
process. A representative sample of wastewater shall be obtained from 
the piping leading to the aeration tank. This sample may be obtained 
from existing sampling valves at the discharge of the wastewater feed 
pump, or collected from a pipe discharging to the aeration tank, or by 
pumping from a well-mixed equalization tank upstream from the aeration 
tank. Alternatively, wastewater can be pumped continuously to the 
laboratory apparatus from a bleed stream taken from the equalization 
tank of the full-scale treatment system.
    6.3.1 Refrigeration System. Keep the wastewater feed cool by ice or 
by refrigeration to 4 [deg]C. If using a bleed stream from the 
equalization tank, refrigeration is not required if the residence time 
in the bleed stream is less than five minutes.
    6.3.2 Wastewater Feed Pump. The wastewater is pumped from the 
refrigerated container using a variable-speed peristaltic pump drive 
equipped with a peristaltic pump

[[Page 176]]

head. Add the feed solution to the benchtop bioreactor through a fitting 
on the top flange. Determine the rate of feed addition to provide a 
retention time in the benchtop bioreactor that is numerically equivalent 
to the retention time in the target full-scale system. The wastewater 
shall be fed at a rate sufficient to achieve 90 to 100 percent of the 
target full-scale system residence time.
    6.3.3 Treated wastewater feed. The benchtop bioreactor effluent 
exits at the bottom of the reactor through a tube and proceeds to the 
clarifier.
    6.4 Clarifier. The effluent flows to a separate closed clarifier 
that allows separation of biomass and effluent (e.g., 2-liter pear-
shaped glass separatory funnel, modified by removing the stopcock and 
adding a 25-mm OD glass tube at the bottom). Benchtop bioreactor 
effluent enters the clarifier through a tube inserted to a depth of 0.08 
m (3 in.) through a stopper at the top of the clarifier. System effluent 
flows from a tube inserted through the stopper at the top of the 
clarifier to a drain (or sample bottle when sampling). The underflow 
from the clarifier leaves from the glass tube at the bottom of the 
clarifier. Flexible tubing connects this fitting to the sludge recycle 
pump. This pump is coupled to a variable speed pump drive. The discharge 
from this pump is returned through a tube inserted in a port on the side 
of the benchtop bioreactor. An additional port is provided near the 
bottom of the benchtop bioreactor for sampling the reactor contents. The 
mixed liquor from the benchtop bioreactor flows into the center of the 
clarifier. The clarified system effluent separates from the biomass and 
flows through an exit near the top of the clarifier. There shall be no 
headspace in the clarifier.
    6.5 Temperature Control Apparatus. Capable of maintaining the system 
at a temperature equal to the temperature of the full-scale system. The 
average temperature should be maintained within 2 
[deg]C of the set point.
    6.5.1 Temperature Monitoring Device. A resistance type temperature 
probe or a thermocouple connected to a temperature readout with a 
resolution of 0.1 [deg]C or better.
    6.5.2 Benchtop Bioreactor Heater. The heater is connected to the 
temperature control device.
    6.6 Oxygen Control System. Maintain the dissolved oxygen 
concentration at the levels present in the full-scale system. Target 
full-scale activated sludge systems with dissolved oxygen concentration 
below 2 mg/L are required to maintain the dissolved oxygen concentration 
in the benchtop bioreactor within 0.5 mg/L of the target dissolved 
oxygen level. Target full-scale activated sludge systems with dissolved 
oxygen concentration above 2 mg/L are required to maintain the dissolved 
oxygen concentration in the benchtop bioreactor within 1.5 mg/L of the 
target dissolved oxygen concentration; however, for target full-scale 
activated sludge systems with dissolved oxygen concentrations above 2 
mg/L, the dissolved oxygen concentration in the benchtop bioreactor may 
not drop below 1.5 mg/L. If the benchtop bioreactor is outside the 
control range, the dissolved oxygen is noted and the reactor operation 
is adjusted.
    6.6.1 Dissolved Oxygen Monitor. Dissolved oxygen is monitored with a 
polarographic probe (gas permeable membrane) connected to a dissolved 
oxygen meter (e.g., 0 to 15 mg/L, 0 to 50 [deg]C).
    6.6.2 Benchtop Bioreactor Pressure Monitor. The benchtop bioreactor 
pressure is monitored through a port in the top flange of the reactor. 
This is connected to a gauge control with a span of 13-cm water vacuum 
to 13-cm water pressure or better. A relay is activated when the vacuum 
exceeds an adjustable setpoint which opens a solenoid valve (normally 
closed), admitting oxygen to the system. The vacuum setpoint controlling 
oxygen addition to the system shall be set at approximately 2.5  0.5 cm water and maintained at this setting except 
during brief periods when the dissolved oxygen concentration is 
adjusted.
    6.7 Connecting Tubing. All connecting tubing shall be Teflon or 
equivalent in impermeability. The only exception to this specification 
is the tubing directly inside the pump head of the wastewater feed pump, 
which may be Viton, Silicone or another type of flexible tubing.
    Note: Mention of trade names or products does not constitute 
endorsement by the U.S. Environmental Protection Agency.

                       7.0. Reagents and Standards

    7.1 Wastewater. Obtain a representative sample of wastewater at the 
inlet to the full-scale treatment plant if there is an existing full-
scale treatment plant (See Section 6.3). If there is no existing full-
scale treatment plant, obtain the wastewater sample as close to the 
point of determination as possible. Collect the sample by pumping the 
wastewater into the 20-L collapsible container. The loss of volatiles 
shall be minimized from the wastewater by collapsing the container 
before filling, by minimizing the time of filling, and by avoiding a 
headspace in the container after filling. If the wastewater requires the 
addition of nutrients to support the biomass growth and maintain biomass 
characteristics, those nutrients are added and mixed with the container 
contents after the container is filled.
    7.2 Biomass. Obtain the biomass or activated sludge used for rate 
constant determination in the bench-scale process from the existing 
full-scale process or from a representative biomass culture (e.g., 
biomass that has been developed for a future full-scale process). This 
biomass is preferentially

[[Page 177]]

obtained from a thickened acclimated mixed liquor sample. Collect the 
sample either by bailing from the mixed liquor in the aeration tank with 
a weighted container, or by collecting aeration tank effluent at the 
effluent overflow weir. Transport the sample to the laboratory within no 
more than 4 hours of collection. Maintain the biomass concentration in 
the benchtop bioreactor at the level of the target full-scale system +10 
percent throughout the sampling period of the test method.

       8.0 Sample Collection, Preservation, Storage, and Transport

    8.1 Benchtop Bioreactor Operation. Charge the mixed liquor to the 
benchtop bioreactor, minimizing headspace over the liquid surface to 
minimize entrainment of mixed liquor in the circulating gas. Fasten the 
benchtop bioreactor headplate to the reactor over the liquid surface. 
Maintain the temperature of the contents of the benchtop bioreactor 
system at the temperature of the target full-scale system, 2 [deg]C, throughout the testing period. Monitor and 
record the temperature of the reactor contents at least to the nearest 
0.1 [deg]C.
    8.1.1 Wastewater Storage. Collect the wastewater sample in the 20-L 
collapsible container. Store the container at 4 [deg]C throughout the 
testing period. Connect the container to the benchtop bioreactor feed 
pump.
    8.1.2 Wastewater Flow Rate.
    8.1.2.1 The hydraulic residence time of the aeration tank is 
calculated as the ratio of the volume of the tank (L) to the flow rate 
(L/min). At the beginning of a test, the container shall be connected to 
the feed pump and solution shall be pumped to the benchtop bioreactor at 
the required flow rate to achieve the calculated hydraulic residence 
time of wastewater in the aeration tank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.555

Where:

Qtest = wastewater flow rate (L/min)
Qfs = average flow rate of full-scale process (L/min)
Vfs = volume of full-scale aeration tank (L)

    8.1.2.2 The target flow rate in the test apparatus is the same as 
the flow rate in the target full-scale process multiplied by the ratio 
of benchtop bioreactor volume (e.g., 6 L) to the volume of the full-
scale aeration tank. The hydraulic residence time shall be maintained at 
90 to 100 percent of the residence time maintained in the target full-
scale unit. A nominal flow rate is set on the pump based on a pump 
calibration. Changes in the elasticity of the tubing in the pump head 
and the accumulation of material in the tubing affect this calibration. 
The nominal pumping rate shall be changed as necessary based on 
volumetric flow measurements. Discharge the benchtop bioreactor effluent 
to a wastewater storage, treatment, or disposal facility, except during 
sampling or flow measurement periods.
    8.1.3 Sludge Recycle Rate. Set the sludge recycle rate at a rate 
sufficient to prevent accumulation in the bottom of the clarifier. Set 
the air circulation rate sufficient to maintain the biomass in 
suspension.
    8.1.4 Benchtop Bioreactor Operation and Maintenance. Temperature, 
dissolved oxygen concentration, flow rate, and air circulation rate 
shall be measured and recorded three times throughout each day of 
testing. If other parameters (such as pH) are measured and maintained in 
the target full-scale unit, these parameters shall, where appropriate, 
be monitored and maintained to full-scale specifications in the benchtop 
bioreactor. At the beginning of each sampling period (section 8.2), 
sample the benchtop bioreactor contents for suspended solids analysis. 
Take this sample by loosening a clamp on a length of tubing attached to 
the lower side port. Determine the suspended solids gravimetrically by 
the Gooch crucible/glass fiber filter method for total suspended solids, 
in accordance with Standard Methods3 or equivalent. When 
necessary, sludge shall be wasted from the lower side port of the 
benchtop bioreactor, and the volume that is wasted shall be replaced 
with an equal volume of the benchtop bioreactor effluent. Add thickened 
activated sludge mixed liquor as necessary to the benchtop bioreactor to 
increase the suspended solids concentration to the desired level. Pump 
this mixed liquor to the benchtop bioreactor through the upper side port 
(Item 24 in Figure 304B-1). Change the membrane on the dissolved oxygen 
probe before starting the test. Calibrate the oxygen probe immediately 
before the start of the test and each time the membrane is changed. The 
scrubber solution shall be replaced each weekday with 175 mL 45 percent 
W/W KOH solution to which five drops of 0.2 percent alizarin yellow 
indicator in water have been added. The potassium hydroxide solution in 
the alkaline scrubber shall be changed if the alizarin yellow dye color 
changes.

[[Page 178]]

    8.1.5 Inspection and Correction Procedures. If the feed line tubing 
becomes clogged, replace with new tubing. If the feed flow rate is not 
within 5 percent of target flow any time the flow rate is measured, 
reset pump or check the flow measuring device and measure flow rate 
again until target flow rate is achieved.
    8.2 Test Sampling. At least two and one half hydraulic residence 
times after the system has reached the targeted specifications shall be 
permitted to elapse before the first sample is taken. Effluent samples 
of the clarifier discharge (Item 20 in Figure 304B-1) and the influent 
wastewater feed are collected in 40-mL septum vials to which two drops 
of 1:10 hydrochloric acid (HCl) in water have been added. Sample the 
clarifier discharge directly from the drain line. These samples will be 
composed of the entire flow from the system for a period of several 
minutes. Feed samples shall be taken from the feed pump suction line 
after temporarily stopping the benchtop bioreactor feed, removing a 
connector, and squeezing the collapsible feed container. Store both 
influent and effluent samples at 4 [deg]C immediately after collection 
and analyze within 8 hours of collection.
    8.2.1 Frequency of Sampling. During the test, sample and analyze the 
wastewater feed and the clarifier effluent at least six times. The 
sampling intervals shall be separated by at least 8 hours. During any 
individual sampling interval, sample the wastewater feed simultaneously 
with or immediately after the effluent sample. Calculate the RSD of the 
amount removed (i.e., effluent concentration--wastewater feed 
concentration). The RSD values shall be <15 percent. If an RSD value is 
15 percent, continue sampling and analyzing influent and 
effluent sets of samples until the RSD values are within specifications.
    8.2.2 Sampling After Exposure of System to Atmosphere. If, after 
starting sampling procedures, the benchtop bioreactor system is exposed 
to the atmosphere (due to leaks, maintenance, etc.), allow at least one 
hydraulic residence time to elapse before resuming sampling.

                           9.0 Quality Control

    9.1 Dissolved Oxygen. Fluctuation in dissolved oxygen concentration 
may occur for numerous reasons, including undetected gas leaks, 
increases and decreases in mixed liquor suspended solids resulting from 
cell growth and solids loss in the effluent stream, changes in diffuser 
performance, cycling of effluent flow rate, and overcorrection due to 
faulty or sluggish dissolved oxygen probe response. Control the 
dissolved oxygen concentration in the benchtop bioreactor by changing 
the proportion of oxygen in the circulating aeration gas. Should the 
dissolved oxygen concentration drift below the designated experimental 
condition, bleed a small amount of aeration gas from the system on the 
pressure side (i.e., immediately upstream of one of the diffusers). This 
will create a vacuum in the system, triggering the pressure sensitive 
relay to open the solenoid valve and admit oxygen to the system. Should 
the dissolved oxygen concentration drift above the designated 
experimental condition, slow or stop the oxygen input to the system 
until the dissolved oxygen concentration approaches the correct level.
    9.2 Sludge Wasting.
    9.2.1 Determine the suspended solids concentration (section 8.1.4) 
at the beginning of a test, and once per day thereafter during the test. 
If the test is completed within a two day period, determine the 
suspended solids concentration after the final sample set is taken. If 
the suspended solids concentration exceeds the specified concentration, 
remove a fraction of the sludge from the benchtop bioreactor. The 
required volume of mixed liquor to remove is determined as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.556

Where:

Vw is the wasted volume (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sm is the measured solids (g/L), and
Ss is the specified solids (g/L).

    9.2.2 Remove the mixed liquor from the benchtop bioreactor by 
loosening a clamp on the mixed liquor sampling tube and allowing the 
required volume to drain to a graduated flask. Clamp the tube when the 
correct volume has been wasted. Replace the volume of the liquid wasted 
by pouring the same volume of effluent back into the benchtop 
bioreactor. Dispose of the waste sludge properly.
    9.3 Sludge Makeup. In the event that the suspended solids 
concentration is lower than the specifications, add makeup sludge back 
into the benchtop bioreactor. Determine the

[[Page 179]]

amount of sludge added by the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.557

Where:

Vw is the volume of sludge to add (Liters),
Vr is the volume of the benchtop bioreactor (Liters),
Sw is the solids in the makeup sludge (g/L),
Sm is the measured solids (g/L), and
Ss is the specified solids (g/L).

                  10.0 Calibration and Standardizations

    10.1 Wastewater Pump Calibration. Determine the wastewater flow rate 
by collecting the system effluent for a time period of at least one 
hour, and measuring the volume with a graduated cylinder. Record the 
collection time period and volume collected. Determine flow rate. Adjust 
the pump speed to deliver the specified flow rate.
    10.2 Calibration Standards. Prepare calibration standards from pure 
certified standards in an aqueous medium. Prepare and analyze three 
concentrations of calibration standards for each target component (or 
for a mixture of components) in triplicate daily throughout the analyses 
of the test samples. At each concentration level, a single calibration 
shall be within 5 percent of the average of the three calibration 
results. The low and medium calibration standards shall bracket the 
expected concentration of the effluent (treated) wastewater. The medium 
and high standards shall bracket the expected influent concentration.

                     11.0 Analytical Test Procedures

    11.1 Analysis. If the identity of the compounds of interest in the 
wastewater is not known, a representative sample of the wastewater shall 
be analyzed in order to identify all of the compounds of interest 
present. A gas chromatography/mass spectrometry screening method is 
recommended.
    11.1.1 After identifying the compounds of interest in the 
wastewater, develop and/or use one or more analytical technique capable 
of measuring each of those compounds (more than one analytical technique 
may be required, depending on the characteristics of the wastewater). 
Method 18, found in appendix A of 40 CFR 60, may be used as a guideline 
in developing the analytical technique. Purge and trap techniques may be 
used for analysis providing the target components are sufficiently 
volatile to make this technique appropriate. The limit of quantitation 
for each compound shall be determined.\1\ If the effluent concentration 
of any target compound is below the limit of quantitation determined for 
that compound, the operation of the Method 304 unit may be altered to 
attempt to increase the effluent concentration above the limit of 
quantitation. Modifications to the method shall be approved prior to the 
test. The request should be addressed to Method 304 contact, Emissions 
Measurement Center, Mail Drop 19, U.S. Environmental Protection Agency, 
Research Triangle Park, NC 27711.

                   12.0 Data Analysis and Calculations

    12.1 Nomenclature. The following symbols are used in the 
calculations.

Ci = Average inlet feed concentration for a compound of 
interest, as analyzed (mg/L)
Co = Average outlet (effluent) concentration for a compound 
of interest, as analyzed (mg/L)
X = Biomass concentration, mixed liquor suspended solids (g/L)
t = Hydraulic residence time in the benchtop bioreactor (hours)
V = Volume of the benchtop bioreactor (L)
Q = Flow rate of wastewater into the benchtop bioreactor, average (L/
hour)

    12.2 Residence Time. The hydraulic residence time of the benchtop 
bioreactor is equal to the ratio of the volume of the benchtop 
bioreactor (L) to the flow rate (L/h)
[GRAPHIC] [TIFF OMITTED] TR17OC00.558


[[Page 180]]


    12.3 Rate of Biodegradation. Calculate the rate of biodegradation 
for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.559

    12.4 First-Order Biorate Constant. Calculate the first-order biorate 
constant (K1) for each component with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.560

    12.5 Relative Standard Deviation (RSD). Determine the standard 
deviation of both the influent and effluent sample concentrations (S) 
using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.561

    12.6 Determination of Percent Air Emissions and Percent Biodegraded. 
Use the results from this test method and follow the applicable 
procedures in appendix C of 40 CFR Part 63, entitled, ``Determination of 
the Fraction Biodegraded (Fbio) in a Biological Treatment 
Unit'' to determine Fbio.

                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                             16.0 References

    1. ``Guidelines for data acquisition and data quality evaluation in 
Environmental Chemistry'', Daniel MacDoughal, Analytical Chemistry, 
Volume 52, p. 2242, 1980.
    2. Test Method 18, 40 CFR 60, Appendix A.
    3. Standard Methods for the Examination of Water and Wastewater, 
16th Edition, Method 209C, Total Suspended Solids Dried at 103-105 
[deg]C, APHA, 1985.
    4. Water--7, Hazardous Waste Treatment, Storage, and Disposal 
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection 
Agency, EPA-450/3-87-026, Review Draft, November 1989.
    5. Chemdat7, Hazardous Waste Treatment, Storage, and Disposal 
Facilities (TSDF)--Air Emission Models, U.S. Environmental Protection 
Agency, EPA-450/3-87-026, Review Draft, November 1989.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 181]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.562

  Method 305: Measurement of Emission Potential of Individual Volatile 
                       Organic Compounds in Waste

    Note: This method does not include all of the specifications (e.g., 
equipment and supplies) and procedures (e.g., sampling and analytical) 
essential to its performance. Some material is incorporated by reference 
from other methods in 40 CFR Part 60, Appendix A. Therefore, to obtain 
reliable results, persons using this method should have a thorough 
knowledge of at least Method 25D.

                        1.0 Scope and Application

    1.1 Analyte. Volatile Organics. No CAS No. assigned.
    1.2 Applicability. This procedure is used to determine the emission 
potential of individual volatile organics (VOs) in waste.
    1.3 Data Quality Objectives. Adherence to the requirements of this 
method will enhance the quality of the data obtained from air pollutant 
sampling methods.

[[Page 182]]

                          2.0 Summary of Method

    2.1 The heated purge conditions established by Method 25D (40 CFR 
Part 60, Appendix A) are used to remove VOs from a 10 gram sample of 
waste suspended in a 50/50 solution of polyethylene glycol (PEG) and 
water. The purged VOs are quantified by using the sample collection and 
analytical techniques (e.g. gas chromatography) appropriate for the VOs 
present in the waste. The recovery efficiency of the sample collection 
and analytical technique is determined for each waste matrix. A 
correction factor is determined for each compound (if acceptable 
recovery criteria requirements are met of 70 to 130 percent recovery for 
every target compound), and the measured waste concentration is 
corrected with the correction factor for each compound. A minimum of 
three replicate waste samples shall be analyzed.

                       3.0 Definitions. [Reserved]

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method may not address all of the 
safety problems associated with its use. It is the responsibility of the 
user of this test method to establish appropriate safety and health 
practices and to determine the applicability of regulatory limitations 
prior to performing this test method.

                       6.0 Equipment and Supplies

    6.1 Method 25D Purge Apparatus.
    6.1.1 Purge Chamber. The purge chamber shall accommodate the 10 gram 
sample of waste suspended in a matrix of 50 mL of PEG and 50 mL of 
deionized, hydrocarbon-free water. Three fittings are used on the glass 
chamber top. Two 7 Ace-threads are used for the purge gas inlet 
and outlet connections. A 50 Ace-thread is used to connect the 
top of the chamber to the base (see Figure 305-1). The base of the 
chamber has a side-arm equipped with a 22 Sovirel fitting to 
allow for easy sample introductions into the chamber. The dimensions of 
the chamber are shown in Figure 305-1.
    6.1.2 Flow Distribution Device (FDD). The FDD enhances the gas-to-
liquid contact for improved purging efficiency. The FDD is a 6 mm OD 
(0.2 in) by 30 cm (12 in) long glass tube equipped with four arm 
bubblers as shown in Figure 305-1. Each arm shall have an opening of 1 
mm (0.04 in) in diameter.
    6.1.3 Coalescing Filter. The coalescing filter serves to discourage 
aerosol formation of sample gas once it leaves the purge chamber. The 
glass filter has a fritted disc mounted 10 cm (3.9 in) from the bottom. 
Two 7 Ace-threads are used for the inlet and outlet 
connections. The dimensions of the chamber are shown in Figure 305-2.
    6.1.4 Oven. A forced convection airflow oven capable of maintaining 
the purge chamber and coalescing filter at 75  2 
[deg]C (167  3.6 [deg]F).
    6.1.5 Toggle Valve. An on/off valve constructed from brass or 
stainless steel rated to 100 psig. This valve is placed in line between 
the purge nitrogen source and the flow controller.
    6.1.6 Flow Controller. High-quality stainless steel flow controller 
capable of restricting a flow of nitrogen to 6  
0.06 L/min (0.2  0.002 ft3/min) at 40 
psig.
    6.1.7 Polyethylene Glycol Cleaning System.
    6.1.7.1 Round-Bottom Flask. One liter, three-neck glass round-bottom 
flask for cleaning PEG. Standard taper 24/40 joints are mounted on each 
neck.
    6.1.7.2 Heating Mantle. Capable of heating contents of the 1-L flask 
to 120 [deg]C (248 [deg]F).
    6.1.7.3 Nitrogen Bubbler. Teflon[reg] or glass tube, 0.25 in OD 
(6.35 mm).
    6.1.7.4 Temperature Sensor. Partial immersion glass thermometer.
    6.1.7.5 Hose Adapter. Glass with 24/40 standard tapered joint.
    6.2 Volatile Organic Recovery System.
    6.2.1 Splitter Valve (Optional). Stainless steel cross-pattern valve 
capable of splitting nominal flow rates from the purge flow of 6 L/min 
(0.2 ft3/min). The valve shall be maintained at 75 + 2 [deg]C 
(167  3.6 [deg]F) in the heated zone and shall be 
placed downstream of the coalescing filter. It is recommended that 0.125 
in OD (3.175 mm) tubing be used to direct the split vent flow from the 
heated zone. The back pressure caused by the 0.125 in OD (3.175 mm) 
tubing is critical for maintaining proper split valve operation.
    Note: The splitter valve design is optional; it may be used in cases 
where the concentration of a pollutant would saturate the adsorbents.
    6.2.2 Injection Port. Stainless steel 1/4 in OD (6.35 mm) 
compression fitting tee with a 6 mm (0.2 in) septum fixed on the top 
port. The injection port is the point of entry for the recovery study 
solution. If using a gaseous standard to determine recovery efficiency, 
connect the gaseous standard to the injection port of the tee.
    6.2.3 Knockout Trap (Optional but Recommended). A 25 mL capacity 
glass reservoir body with a full-stem impinger (to avoid leaks, a 
modified midget glass impinger with a screw cap and ball/socket clamps 
on the inlet and outlet is recommended). The empty impinger is placed in 
an ice water bath between the injection port and the sorbent cartridge. 
Its purpose is to reduce the water content of the purge gas (saturated 
at 75 [deg]C (167 [deg]F)) before the sorbent cartridge.
    6.2.4 Insulated Ice Bath. A 350 mL dewar or other type of insulated 
bath is used to

[[Page 183]]

maintain ice water around the knockout trap.
    6.2.5 Sorbent Cartridges. Commercially available glass or stainless 
steel cartridge packed with one or more appropriate sorbents. The amount 
of adsorbent packed in the cartridge depends on the breakthrough volume 
of the test compounds but is limited by back pressure caused by the 
packing (not to exceed 7 psig). More than one sorbent cartridge placed 
in series may be necessary depending upon the mixture of the measured 
components.
    6.2.6 Volumetric Glassware. Type A glass 10 mL volumetric flasks for 
measuring a final volume from the water catch in the knockout trap.
    6.2.7 Thermal Desorption Unit. A clam-shell type oven, used for the 
desorption of direct thermal desorption sorbent tubes. The oven shall be 
capable of increasing the temperature of the desorption tubes rapidly to 
recommended desorption temperature.
    6.2.8 Ultrasonic Bath. Small bath used to agitate sorbent material 
and desorption solvent. Ice water shall be used in the bath because of 
heat transfer caused by operation of the bath.
    6.2.9 Desorption Vials. Four-dram (15 mL) capacity borosilicate 
glass vials with Teflon-lined caps.
    6.3 Analytical System. A gas chromatograph (GC) is commonly used to 
separate and quantify compounds from the sample collection and recovery 
procedure. Method 18 (40 CFR Part 60, Appendix A) may be used as a 
guideline for determining the appropriate GC column and GC detector 
based on the test compounds to be determined. Other types of analytical 
instrumentation may be used (HPLC) in lieu of GC systems as long as the 
recovery efficiency criteria of this method are met.
    6.3.1 Gas Chromatograph (GC). The GC shall be equipped with a 
constant-temperature liquid injection port or a heated sampling loop/
valve system, as appropriate. The GC oven shall be temperature-
programmable over the useful range of the GC column. The choice of 
detectors is based on the test compounds to be determined.
    6.3.2 GC Column. Select the appropriate GC column based on (1) 
literature review or previous experience, (2) polarity of the analytes, 
(3) capacity of the column, or (4) resolving power (e.g., length, 
diameter, film thickness) required.
    6.3.3 Data System. A programmable electronic integrator for 
recording, analyzing, and storing the signal generated by the detector.

                       7.0 Reagents and Standards

    7.1 Method 25D Purge Apparatus.
    7.1.1 Polyethylene Glycol (PEG). Ninety-eight percent pure organic 
polymer with an average molecular weight of 400 g/mol. Volatile organics 
are removed from the PEG prior to use by heating to 120  5 [deg]C (248  9 [deg]F) and 
purging with pure nitrogen at 1 L/min (0.04 ft3/min) for 2 
hours. After purging and heating, the PEG is maintained at room 
temperature under a nitrogen purge maintained at 1 L/min (0.04 
ft3/min) until used. A typical apparatus used to clean the 
PEG is shown in Figure 305-3.
    7.1.2 Water. Organic-free deionized water is required.
    7.1.3 Nitrogen. High-purity nitrogen (less than 0.5 ppm total 
hydrocarbons) is used to remove test compounds from the purge matrix. 
The source of nitrogen shall be regulated continuously to 40 psig before 
the on/off toggle valve.
    7.2 Volatile Organic Recovery System.
    7.2.1 Water. Organic-free deionized water is required.
    7.2.2 Desorption Solvent (when used). Appropriate high-purity (99.99 
percent) solvent for desorption shall be used. Analysis shall be 
performed (utilizing the same analytical technique as that used in the 
analysis of the waste samples) on each lot to determine purity.
    7.3 Analytical System. The gases required for GC operation shall be 
of the highest obtainable purity (hydrocarbon free). Consult the 
operating manual for recommended settings.

       8.0 Sample Collection, Preservation, Storage, and Transport

    8.1 Assemble the glassware and associated fittings (see Figures 305-
3 and 305-4, as appropriate) and leak-check the system (approximately 7 
psig is the target pressure). After an initial leak check, mark the 
pressure gauge and use the initial checkpoint to monitor for leaks 
throughout subsequent analyses. If the pressure in the system drops 
below the target pressure at any time during analysis, that analysis 
shall be considered invalid.
    8.2 Recovery Efficiency Determination. Determine the individual 
recovery efficiency (RE) for each of the target compounds in duplicate 
before the waste samples are analyzed. To determine the RE, generate a 
water blank (Section 11.1) and use the injection port to introduce a 
known volume of spike solution (or certified gaseous standard) 
containing all of the target compounds at the levels expected in the 
waste sample. Introduce the spike solution immediately after the 
nitrogen purge has been started (Section 8.3.2). Follow the procedures 
outlined in Section 8.3.3. Analyze the recovery efficiency samples using 
the techniques described in Section 11.2. Determine the recovery 
efficiency (Equation 305-1, Section 12.2) by comparing the amount of 
compound recovered to the theoretical amount spiked. Determine the RE 
twice for each compound; the relative

[[Page 184]]

standard deviation, (RSD) shall be <= 10 percent for each compound. If 
the RSD for any compound is not <= 10 percent, modify the sampling/
analytical procedure and complete an RE study in duplicate, or continue 
determining RE until the RSD meets the acceptable criteria. The average 
RE shall be 0.70 <= RE <= 1.30 for each compound. If the average RE does 
not meet these criteria, an alternative sample collection and/or 
analysis technique shall be developed and the recovery efficiency 
determination shall be repeated for that compound until the criteria are 
met for every target compound. Example modifications of the sampling/
analytical system include changing the adsorbent material, changing the 
desorption solvent, utilizing direct thermal desorption of test 
compounds from the sorbent tubes, utilizing another analytical 
technique.
    8.3 Sample Collection and Recovery.
    8.3.1 The sample collection procedure in Method 25D shall be used to 
collect (into a preweighed vial) 10 g of waste into PEG, cool, and ship 
to the laboratory. Remove the sample container from the cooler and wipe 
the exterior to remove any ice or water. Weigh the container and sample 
to the nearest 0.01 g and record the weight. Pour the sample from the 
container into the purge flask. Rinse the sample container three times 
with approximately 6 mL of PEG (or the volume needed to total 50 mL of 
PEG in the purge flask), transferring the rinses to the purge flask. Add 
50 mL of organic-free deionized water to the purge flask. Cap the purge 
flask tightly in between each rinse and after adding all the components 
into the flask.
    8.3.2 Allow the oven to equilibrate to 75  2 
[deg]C (167  3.6 [deg]F). Begin the sample 
recovery process by turning the toggle valve on, thus allowing a 6 L/min 
flow of pure nitrogen through the purge chamber.
    8.3.3 Stop the purge after 30 min. Immediately remove the sorbent 
tube(s) from the apparatus and cap both ends. Remove the knockout trap 
and transfer the water catch to a 10 mL volumetric flask. Rinse the trap 
with organic-free deionized water and transfer the rinse to the 
volumetric flask. Dilute to the 10 mL mark with water. Transfer the 
water sample to a sample vial and store at 4 [deg]C (39.2 [deg]F) with 
zero headspace. The analysis of the contents of the water knockout trap 
is optional for this method. If the target compounds are water soluble, 
analysis of the water is recommended; meeting the recovery efficiency 
criteria in these cases would be difficult without adding the amount 
captured in the knockout trap.

                           9.0 Quality Control

    9.1 Miscellaneous Quality Control Measures.

------------------------------------------------------------------------
                                 Quality control
            Section                  measure               Effect
------------------------------------------------------------------------
8.1...........................  Sampling           Ensures accurate
                                 equipment leak-    measurement of
                                 check.             sample volume.
8.2...........................  Recovery           Ensures accurate
                                 efficiency (RE)    sample collection
                                 determination      and analysis.
                                 for each
                                 measured
                                 compound..
8.3...........................  Calibration of     Ensures linear
                                 analytical         measurement of
                                 instrument with    compounds over the
                                 at least 3         instrument span.
                                 calibration
                                 standards..
------------------------------------------------------------------------

                  10.0 Calibration and Standardization

    10.1 The analytical instrument shall be calibrated with a minimum of 
three levels of standards for each compound whose concentrations bracket 
the concentration of test compounds from the sorbent tubes. Liquid 
calibration standards shall be used for calibration in the analysis of 
the solvent extracts. The liquid calibration standards shall be prepared 
in the desorption solvent matrix. The calibration standards may be 
prepared and injected individually or as a mixture. If thermal 
desorption and focusing (onto another sorbent or cryogen focusing) are 
used, a certified gaseous mixture or a series of gaseous standards shall 
be used for calibration of the instrument. The gaseous standards shall 
be focused and analyzed in the same manner as the samples.
    10.2 The analytical system shall be certified free from contaminants 
before a calibration is performed (see Section 11.1). The calibration 
standards are used to determine the linearity of the analytical system. 
Perform an initial calibration and linearity check by analyzing the 
three calibration standards for each target compound in triplicate 
starting with the lowest level and continuing to the highest level. If 
the triplicate analyses do not agree within 5 percent of their average, 
additional analyses will be needed until the 5 percent criteria is met. 
Calculate the response factor (Equation 305-3, Section 12.4) from the 
average area counts of the injections for each concentration level. 
Average the response factors of the standards for each compound. The 
linearity of the detector is acceptable if the response factor of each 
compound at a particular concentration is within 10 percent of the 
overall mean response factor for that compound. Analyze daily a mid-
level calibration standard in duplicate and calculate a new response 
factor. Compare the daily response factor average to the average 
response factor calculated for the mid-level calibration during the 
initial linearity check; repeat the three-

[[Page 185]]

level calibration procedure if the daily average response factor differs 
from the initial linearity check mid-level response factor by more than 
10 percent. Otherwise, proceed with the sample analysis.

                        11.0 Analytical Procedure

    11.1 Water Blank Analysis. A water blank shall be analyzed daily to 
determine the cleanliness of the purge and recovery system. A water 
blank is generated by adding 60 mL of organic-free deionized water to 50 
mL of PEG in the purge chamber. Treat the blank as described in Sections 
8.3.2 and 8.3.3. The purpose of the water blank is to insure that no 
contaminants exist in the sampling and analytical apparatus which would 
interfere with the quantitation of the target compounds. If contaminants 
are present, locate the source of contamination, remove it, and repeat 
the water blank analysis.
    11.2 Sample Analysis. Sample analysis in the context of this method 
refers to techniques to remove the target compounds from the sorbent 
tubes, separate them using a chromatography technique, and quantify them 
with an appropriate detector. Two types of sample extraction techniques 
typically used for sorbents include solvent desorption or direct thermal 
desorption of test compounds to a secondary focusing unit (either 
sorbent or cryogen based). The test compounds are then typically 
transferred to a GC system for analysis. Other analytical systems may be 
used (e.g., HPLC) in lieu of GC systems as long as the recovery 
efficiency criteria of this method are met.
    11.2.1 Recover the test compounds from the sorbent tubes that 
require solvent desorption by transferring the adsorbent material to a 
sample vial containing the desorption solvent. The desorption solvent 
shall be the same as the solvent used to prepare calibration standards. 
The volume of solvent depends on the amount of adsorbed material to be 
desorbed (1.0 mL per 100 mg of adsorbent material) and also on the 
amount of test compounds present. Final volume adjustment and or 
dilution can be made so that the concentration of test compounds in the 
desorption solvent is bracketed by the concentration of the calibration 
solutions. Ultrasonicate the desorption solvent for 15 min in an ice 
bath. Allow the sample to sit for a period of time so that the adsorbent 
material can settle to the bottom of the vial. Transfer the solvent with 
a pasteur pipet (minimizing the amount of adsorbent material taken) to 
another vial and store at 4 [deg]C (39.2 [deg]F).
    11.2.2 Analyze the desorption solvent or direct thermal desorption 
tubes from each sample using the same analytical parameters used for the 
calibration standard. Calculate the total weight detected for each 
compound (Equation 305-4, Section 12.5). The slope (area/amount) and y-
intercept are calculated from the line bracketed between the two closest 
calibration points. Correct the concentration of each waste sample with 
the appropriate recovery efficiency factor and the split flow ratio (if 
used). The final concentration of each individual test compound is 
calculated by dividing the corrected measured weight for that compound 
by the weight of the original sample determined in Section 8.3.1 
(Equation 305-5, Section 12.6).
    11.2.3 Repeat the analysis for the three samples collected in 
Section 8.3. Report the corrected concentration of each of the waste 
samples, average waste concentration, and relative standard deviation 
(Equation 305-6, Section 12.7).

                  12.0 Data Analysis and Calculations.

    12.1 Nomenclature.

AS = Mean area counts of test compound in standard.
AU = Mean area counts of test compound in sample desorption 
solvent.
b = Y-intercept of the line formed between the two closest calibration 
standards that bracket the concentration of the sample.
CT = Amount of test compound ([mu]g) in calibration standard.
CF = Correction for adjusting final amount of sample detected 
for losses during individual sample runs.
FP = Nitrogen flow through the purge chamber (6 L/min).
FS = Nitrogen split flow directed to the sample recovery 
system (use 6 L/min if split flow design was not used).
PPM = Final concentration of test compound in waste sample [[mu]g/g 
(which is equivalent to parts per million by weight (ppmw))].
RE = Recovery efficiency for adjusting final amount of sample detected 
for losses due to inefficient trapping and desorption techniques.
R.F. = Response factor for test compound, calculated from a calibration 
standard.
S = Slope of the line (area counts/CT) formed between two 
closest calibration points that bracket the concentration of the sample.
WC = Weight of test compound expected to be recovered in 
spike solution based on theoretical amount ([mu]g).
WE = Weight of vial and PEG (g).
WF = Weight of vial, PEG and waste sample (g).
WS = Weight of original waste sample (g).
WT = Corrected weight of test compound measured ([mu]g) in 
sample.
WX = Weight of test compound measured during analysis of 
recovery efficiency spike samples ([mu]g).

    12.2 Recovery efficiency for determining trapping/desorption 
efficiency of individual test compounds in the spike solution, decimal 
value.

[[Page 186]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.563

    12.3 Weight of waste sample (g).
    [GRAPHIC] [TIFF OMITTED] TR17OC00.564
    
    12.4 Response factor for individual test compounds.
    [GRAPHIC] [TIFF OMITTED] TR17OC00.565
    
    12.5 Corrected weight of a test compound in the sample, in [mu]g.
    [GRAPHIC] [TIFF OMITTED] TR17OC00.566
    
    12.6 Final concentration of a test compound in the sample in ppmw.
    [GRAPHIC] [TIFF OMITTED] TR17OC00.567
    
    12.7 Relative standard deviation (RSD) calculation.
    [GRAPHIC] [TIFF OMITTED] TR17OC00.568
    
                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                       16.0 References. [Reserved]

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         17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.569


[[Page 188]]


[GRAPHIC] [TIFF OMITTED] TR17OC00.570


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[GRAPHIC] [TIFF OMITTED] TR17OC00.571


[[Page 190]]


[GRAPHIC] [TIFF OMITTED] TR17OC00.572

Method 306--Determination of Chromium Emissions From Decorative and Hard 
 Chromium Electroplating and Chromium Anodizing Operations--Isokinetic 
                                 Method

    Note: This method does not include all of the specifications (e.g., 
equipment and supplies) and procedures (e.g., sampling and analytical) 
essential to its performance. Some material is incorporated by reference 
from other methods in 40 CFR Part 60, Appendix A. Therefore, to obtain 
reliable results, persons using this method should have a thorough 
knowledge of at least Method 5.

                        1.0 Scope and Application

    1.1 Analytes.

------------------------------------------------------------------------
            Analyte                  CAS No.            Sensitivity
------------------------------------------------------------------------
Chromium......................  7440-47-3........  See Sec. 13.2.
------------------------------------------------------------------------

    1.2 Applicability. This method applies to the determination of 
chromium (Cr) in emissions from decorative and hard chrome 
electroplating facilities, chromium anodizing operations, and continuous 
chromium plating operations at iron and steel facilities.
    1.3 Data Quality Objectives. [Reserved]

                          2.0 Summary of Method

    2.1 Sampling. An emission sample is extracted isokinetically from 
the source using an unheated Method 5 sampling train (40 CFR Part 60, 
Appendix A), with a glass nozzle and probe liner, but with the filter 
omitted. The sample time shall be at least two hours. The Cr emissions 
are collected in an alkaline solution containing 0.1 N sodium hydroxide 
(NaOH) or 0.1 N sodium bicarbonate (NaHCO3). The collected 
samples are recovered using an alkaline solution and are then 
transported to the laboratory for analysis.
    2.2 Analysis.
    2.2.1 Total chromium samples with high chromium concentrations 
(=35 [mu]g/L) may be analyzed using inductively coupled 
plasma emission spectrometry (ICP) at 267.72 nm.
    Note: The ICP analysis is applicable for this method only when the 
solution analyzed has a Cr concentration greater than or equal

[[Page 191]]

to 35 [mu]g/L or five times the method detection limit as determined 
according to Appendix B in 40 CFR Part 136.
    2.2.2 Alternatively, when lower total chromium concentrations (<35 
[mu]g/L) are encountered, a portion of the alkaline sample solution may 
be digested with nitric acid and analyzed by graphite furnace atomic 
absorption spectroscopy (GFAAS) at 357.9 nm.
    2.2.3 If it is desirable to determine hexavalent chromium 
(Cr+6) emissions, the samples may be analyzed using an ion 
chromatograph equipped with a post-column reactor (IC/PCR) and a visible 
wavelength detector. To increase sensitivity for trace levels of 
Cr+6, a preconcentration system may be used in conjunction 
with the IC/PCR.

                             3.0 Definitions

    3.1 Total Chromium--measured chromium content that includes both 
major chromium oxidation states (Cr+3, Cr+3).
    3.2 May--Implies an optional operation.
    3.3 Digestion--The analytical operation involving the complete (or 
nearly complete) dissolution of the sample in order to ensure the 
complete solubilization of the element (analyte) to be measured.
    3.4 Interferences--Physical, chemical, or spectral phenomena that 
may produce a high or low bias in the analytical result.
    3.5 Analytical System--All components of the analytical process 
including the sample digestion and measurement apparatus.
    3.6 Sample Recovery--The quantitative transfer of sample from the 
collection apparatus to the sample preparation (digestion, etc.) 
apparatus. This term should not be confused with analytical recovery.
    3.7 Matrix Modifier--A chemical modification to the sample during 
GFAAS determinations to ensure that the analyte is not lost during the 
measurement process (prior to the atomization stage)
    3.8 Calibration Reference Standards--Quality control standards used 
to check the accuracy of the instrument calibration curve prior to 
sample analysis.
    3.9 Continuing Check Standard--Quality control standards used to 
verify that unacceptable drift in the measurement system has not 
occurred.
    3.10 Calibration Blank--A blank used to verify that there has been 
no unacceptable shift in the baseline either immediately following 
calibration or during the course of the analytical measurement.
    3.11 Interference Check--An analytical/measurement operation that 
ascertains whether a measurable interference in the sample exists.
    3.12 Interelement Correction Factors--Factors used to correct for 
interfering elements that produce a false signal (high bias).
    3.13 Duplicate Sample Analysis--Either the repeat measurement of a 
single solution or the measurement of duplicate preparations of the same 
sample. It is important to be aware of which approach is required for a 
particular type of measurement. For example, no digestion is required 
for the ICP determination and the duplicate instrument measurement is 
therefore adequate whereas duplicate digestion/instrument measurements 
are required for GFAAS.
    3.14 Matrix Spiking--Analytical spikes that have been added to the 
actual sample matrix either before (Section 9.2.5.2) or after (Section 
9.1.6). Spikes added to the sample prior to a preparation technique 
(e.g., digestion) allow for the assessment of an overall method accuracy 
while those added after only provide for the measurement accuracy 
determination.

                            4.0 Interferences

    4.1 ICP Interferences.
    4.1.1 ICP Spectral Interferences. Spectral interferences are caused 
by: overlap of a spectral line from another element; unresolved overlap 
of molecular band spectra; background contribution from continuous or 
recombination phenomena; and, stray light from the line emission of 
high-concentrated elements. Spectral overlap may be compensated for by 
correcting the raw data with a computer and measuring the interfering 
element. At the 267.72 nm Cr analytical wavelength, iron, manganese, and 
uranium are potential interfering elements. Background and stray light 
interferences can usually be compensated for by a background correction 
adjacent to the analytical line. Unresolved overlap requires the 
selection of an alternative chromium wavelength. Consult the instrument 
manufacturer's operation manual for interference correction procedures.
    4.1.2 ICP Physical Interferences. High levels of dissolved solids in 
the samples may cause significant inaccuracies due to salt buildup at 
the nebulizer and torch tips. This problem can be controlled by diluting 
the sample or by extending the rinse times between sample analyses. 
Standards shall be prepared in the same solution matrix as the samples 
(i.e., 0.1 N NaOH or 0.1 N NaHCO3).
    4.1.3 ICP Chemical Interferences. These include molecular compound 
formation, ionization effects and solute vaporization effects, and are 
usually not significant in the ICP procedure, especially if the 
standards and samples are matrix matched.
    4.2 GFAAS Interferences.
    4.2.1 GFAAS Chemical Interferences. Low concentrations of calcium 
and/or phosphate may cause interferences; at concentrations above 200 
[mu]g/L, calcium's effect is constant and eliminates the effect of 
phosphate. Calcium nitrate is therefore added to the concentrated 
analyte to ensure a known constant effect. Other matrix modifiers 
recommended by the instrument manufacturer may also be considered.

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    4.2.2 GFAAS Cyanide Band Interferences. Nitrogen should not be used 
as the purge gas due to cyanide band interference.
    4.2.3 GFAAS Spectral Interferences. Background correction may be 
required because of possible significant levels of nonspecific 
absorption and scattering at the 357.9 nm analytical wavelength.
    4.2.4 GFAAS Background Interferences. Zeeman or Smith-Hieftje 
background correction is recommended for interferences resulting from 
high levels of dissolved solids in the alkaline impinger solutions.
    4.3 IC/PCR Interferences.
    4.3.1 IC/PCR Chemical Interferences. Components in the sample matrix 
may cause Cr+6 to convert to trivalent chromium 
(Cr+3) or cause Cr+3 to convert to 
Cr+6. The chromatographic separation of Cr+6 using 
ion chromatography reduces the potential for other metals to interfere 
with the post column reaction. For the IC/PCR analysis, only compounds 
that coelute with Cr+6 and affect the diphenylcarbazide 
reaction will cause interference.
    4.3.2 IC/PCR Background Interferences. Periodic analyses of reagent 
water blanks are used to demonstrate that the analytical system is 
essentially free of contamination. Sample cross-contamination can occur 
when high-level and low-level samples or standards are analyzed 
alternately and can be eliminated by thorough purging of the sample 
loop. Purging of the sample can easily be achieved by increasing the 
injection volume to ten times the size of the sample loop.

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method may not address all of the 
safety problems associated with its use. It is the responsibility of the 
user to establish appropriate safety and health practices and to 
determine the applicability of regulatory limitations prior to 
performing this test method.
    5.2 Hexavalent chromium compounds have been listed as carcinogens 
although chromium (III) compounds show little or no toxicity. Chromium 
can be a skin and respiratory irritant.

                       6.0 Equipment and Supplies

    6.1 Sampling Train.
    6.1.1 A schematic of the sampling train used in this method is shown 
in Figure 306-1. The train is the same as shown in Method 5, Section 6.0 
(40 CFR Part 60, Appendix A) except that the probe liner is unheated, 
the particulate filter is omitted, and quartz or borosilicate glass must 
be used for the probe nozzle and liner in place of stainless steel.
    6.1.2 Probe fittings of plastic such as Teflon, polypropylene, etc. 
are recommended over metal fittings to prevent contamination. If 
desired, a single combined probe nozzle and liner may be used, but such 
a single glass assembly is not a requirement of this methodology.
    6.1.3 Use 0.1 N NaOH or 0.1 N NaHCO3 in the impingers in 
place of water.
    6.1.4 Operating and maintenance procedures for the sampling train 
are described in APTD-0576 of Method 5. Users should read the APTD-0576 
document and adopt the outlined procedures.
    6.1.5 Similar collection systems which have been approved by the 
Administrator may be used.
    6.2 Sample Recovery. Same as Method 5, [40 CFR Part 60, Appendix A], 
with the following exceptions:
    6.2.1 Probe-Liner and Probe-Nozzle Brushes. Brushes are not 
necessary for sample recovery. If a probe brush is used, it must be non-
metallic.
    6.2.2 Sample Recovery Solution. Use 0.1 N NaOH or 0.1 N 
NaHCO3, whichever is used as the impinger absorbing solution, 
in place of acetone to recover the sample.
    6.2.3 Sample Storage Containers. Polyethylene, with leak-free screw 
cap, 250 mL, 500 mL or 1,000 mL.
    6.3 Analysis.
    6.3.1 General. For analysis, the following equipment is needed.
    6.3.1.1 Phillips Beakers. (Phillips beakers are preferred, but 
regular beakers may also be used.)
    6.3.1.2 Hot Plate.
    6.3.1.3 Volumetric Flasks. Class A, various sizes as appropriate.
    6.3.1.4 Assorted Pipettes.
    6.3.2 Analysis by ICP.
    6.3.2.1 ICP Spectrometer. Computer-controlled emission spectrometer 
with background correction and radio frequency generator.
    6.3.2.2 Argon Gas Supply. Welding grade or better.
    6.3.3 Analysis by GFAAS.
    6.3.3.1 Chromium Hollow Cathode Lamp or Electrodeless Discharge 
Lamp.
    6.3.3.2 Graphite Furnace Atomic Absorption Spectrophotometer.
    6.3.3.3 Furnace Autosampler.
    6.3.4 Analysis by IC/PCR.
    6.3.4.1 IC/PCR System. High performance liquid chromatograph pump, 
sample injection valve, post-column reagent delivery and mixing system, 
and a visible detector, capable of operating at 520 nm-540 nm, all with 
a non-metallic (or inert) flow path. An electronic peak area mode is 
recommended, but other recording devices and integration techniques are 
acceptable provided the repeatability criteria and the linearity 
criteria for the calibration curve described in Section 10.4 can be 
satisfied. A sample loading system is required if preconcentration is 
employed.

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    6.3.4.2 Analytical Column. A high performance ion chromatograph 
(HPIC) non-metallic column with anion separation characteristics and a 
high loading capacity designed for separation of metal chelating 
compounds to prevent metal interference. Resolution described in Section 
11.6 must be obtained. A non-metallic guard column with the same ion-
exchange material is recommended.
    6.3.4.3 Preconcentration Column (for older instruments). An HPIC 
non-metallic column with acceptable anion retention characteristics and 
sample loading rates must be used as described in Section 11.6.
    6.3.4.4 Filtration Apparatus for IC/PCR.
    6.3.4.4.1 Teflon, or equivalent, filter holder to accommodate 0.45-
[mu]m acetate, or equivalent, filter, if needed to remove insoluble 
particulate matter.
    6.3.4.4.2 0.45-[mu]m Filter Cartridge. For the removal of insoluble 
material. To be used just prior to sample injection/analysis.

                       7.0 Reagents and Standards

    Note: Unless otherwise indicated, all reagents should conform to the 
specifications established by the Committee on Analytical Reagents of 
the American Chemical Society (ACS reagent grade). Where such 
specifications are not available, use the best available grade. Reagents 
should be checked by the appropriate analysis prior to field use to 
assure that contamination is below the analytical detection limit for 
the ICP or GFAAS total chromium analysis; and that contamination is 
below the analytical detection limit for Cr+6 using IC/PCR 
for direct injection or, if selected, preconcentration.
    7.1 Sampling.
    7.1.1 Water. Reagent water that conforms to ASTM Specification 
D1193-77 or 91 Type II (incorporated by reference see Sec. 63.14). All 
references to water in the method refer to reagent water unless 
otherwise specified. It is recommended that water blanks be checked 
prior to preparing the sampling reagents to ensure that the Cr content 
is less than three (3) times the anticipated detection limit of the 
analytical method.
    7.1.2 Sodium Hydroxide (NaOH) Absorbing Solution, 0.1 N. Dissolve 
4.0 g of sodium hydroxide in 1 liter of water to obtain a pH of 
approximately 8.5.
    7.1.3 Sodium Bicarbonate (NaHCO3) Absorbing Solution, 0.1 
N. Dissolve approximately 8.5 g of sodium bicarbonate in 1 liter of 
water to obtain a pH of approximately 8.3.
    7.1.4 Chromium Contamination.
    7.1.4.1 The absorbing solution shall not exceed the QC criteria 
noted in Section 7.1.1 (<= 3 times the instrument detection limit).
    7.1.4.2 When the Cr+6 content in the field samples 
exceeds the blank concentration by at least a factor of ten (10), 
Cr+6 blank concentrations = 10 times the detection 
limit will be allowed.
    Note: At sources with high concentrations of acids and/or 
SO2, the concentration of NaOH or NaHCO3 should be 
= 0.5 N to insure that the pH of the solution remains at or 
above 8.5 for NaOH and 8.0 for NaHCO3 during and after 
sampling.
    7.1.5 Silica Gel. Same as in Method 5.
    7.2 Sample Recovery.
    7.2.1 0.1 N NaOH or 0.1 N NaHCO3. Use the same solution 
for the sample recovery that is used for the impinger absorbing 
solution.
    7.2.2 pH Indicator Strip, for IC/PCR. pH indicator capable of 
determining the pH of solutions between the pH range of 7 and 12, at 0.5 
pH increments.
    7.3 Sample Preparation and Analysis.
    7.3.1 Nitric Acid (HNO3), Concentrated, for GFAAS. Trace 
metals grade or better HNO3 must be used for reagent 
preparation. The ACS reagent grade HNO3 is acceptable for 
cleaning glassware.
    7.3.2 HNO3, 1.0% (v/v), for GFAAS. Prepare, by slowly 
stirring, 10 mL of concentrated HNO3) into 800 mL of reagent 
water. Dilute to 1,000 mL with reagent water. The solution shall contain 
less than 0.001 mg Cr/L.
    7.3.3 Calcium Nitrate Ca(NO3)2 Solution (10 
[mu]g Ca/mL) for GFAAS analysis. Prepare the solution by weighing 40.9 
mg of Ca(NO3)2 into a 1 liter volumetric flask. 
Dilute with reagent water to 1 liter.
    7.3.4 Matrix Modifier, for GFAAS. See instrument manufacturer's 
manual for suggested matrix modifier.
    7.3.5 Chromatographic Eluent, for IC/PCR. The eluent used in the 
analytical system is ammonium sulfate based.
    7.3.5.1 Prepare by adding 6.5 mL of 29 percent ammonium hydroxide 
(NH4OH) and 33 g of ammonium sulfate 
((NH4)2SO4) to 500 mL of reagent water. 
Dilute to 1 liter with reagent water and mix well.
    7.3.5.2 Other combinations of eluents and/or columns may be employed 
provided peak resolution, repeatability, linearity, and analytical 
sensitivity as described in Sections 9.3 and 11.6 are acceptable.
    7.3.6 Post-Column Reagent, for IC/PCR. An effective post-column 
reagent for use with the chromatographic eluent described in Section 
7.3.5 is a diphenylcarbazide (DPC)-based system. Dissolve 0.5 g of 1,5-
diphenylcarbazide in 100 mL of ACS grade methanol. Add 500 mL of reagent 
water containing 50 mL of 96 percent spectrophotometric grade sulfuric 
acid. Dilute to 1 liter with reagent water.
    7.3.7 Chromium Standard Stock Solution (1000 mg/L). Procure a 
certified aqueous standard or dissolve 2.829 g of potassium dichromate 
(K2Cr2O7), in reagent water and dilute 
to 1 liter.
    7.3.8 Calibration Standards for ICP or IC/PCR. Prepare calibration 
standards for ICP or IC/PCR by diluting the Cr standard stock solution 
(Section 7.3.7) with 0.1 N NaOH or

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0.1 N NaHCO3, whichever is used as the impinger absorbing 
solution, to achieve a matrix similar to the actual field samples. 
Suggested levels are 0, 50, 100, and 200 [mu]g Cr/L for ICP, and 0, 1, 
5, and 10 [mu]g Cr+6/L for IC/PCR.
    7.3.9 Calibration Standards for GFAAS. Chromium solutions for GFAAS 
calibration shall contain 1.0 percent (v/v) HNO3. The zero 
standard shall be 1.0 percent (v/v) HNO3. Calibration 
standards should be prepared daily by diluting the Cr standard stock 
solution (Section 7.3.7) with 1.0 percent HNO3. Use at least 
four standards to make the calibration curve. Suggested levels are 0, 
10, 50, and 100 [mu]g Cr/L.
    7.4 Glassware Cleaning Reagents.
    7.4.1 HNO3, Concentrated. ACS reagent grade or 
equivalent.
    7.4.2 Water. Reagent water that conforms to ASTM Specification 
D1193-77 or 91 Type II.
    7.4.3 HNO3, 10 percent (v/v). Add by stirring 500 mL of 
concentrated HNO3 into a flask containing approximately 4,000 
mL of reagent water. Dilute to 5,000 mL with reagent water. Mix well. 
The reagent shall contain less than 2 [mu]g Cr/L.
    7.5 Quality Assurance Audit Samples.
    7.5.1 When making compliance determinations, and upon availability, 
audit samples shall be obtained from the appropriate EPA regional Office 
or from the responsible enforcement authority and analyzed in 
conjunction with the field samples.
    7.5.2 If EPA or National Institute of Standards and Technology 
(NIST) reference audit sample are not available, a mid-range standard, 
prepared from an independent commercial source, may be used.
    Note: To order audit samples, contact the responsible enforcement 
authority at least 30 days prior to the test date to allow sufficient 
time for the audit sample to be delivered.

    8.0 Sample Collection, Preservation, Holding Times, Storage, and 
                                Transport

    Note: Prior to sample collection, consideration should be given to 
the type of analysis (Cr+\6\ or total Cr) that will be 
performed. Which analysis option(s) will be performed will determine 
which sample recovery and storage procedures will be required to process 
the sample (See Figures 306-3 and 306-4).
    8.1 Sample Collection. Same as Method 5 (40 CFR part 60, Appendix 
A), with the following exceptions.
    8.1.1 Omit the particulate filter and filter holder from the 
sampling train. Use a glass nozzle and probe liner instead of stainless 
steel. Do not heat the probe. Place 100 mL of 0.1 N NaOH or 0.1 N 
NaHCO3 in each of the first two impingers, and record the 
data for each run on a data sheet such as shown in Figure 306-2.
    8.1.2 Clean all glassware prior to sampling in hot soapy water 
designed for laboratory cleaning of glassware. Next, rinse the glassware 
three times with tap water, followed by three additional rinses with 
reagent water. Then soak the glassware in 10% (v/v) HNO3 
solution for a minimum of 4 hours, rinse three times with reagent water, 
and allow to air dry. Cover all glassware openings where contamination 
can occur with Parafilm, or equivalent, until the sampling train is 
assembled for sampling.
    8.1.3 Train Operation. Follow the basic procedures outlined in 
Method 5 in conjunction with the following instructions. Train sampling 
rate shall not exceed 0.030 m\3\/min (1.0 cfm) during a run.
    8.2 Sample Recovery. Follow the basic procedures of Method 5, with 
the exceptions noted.
    8.2.1 A particulate filter is not recovered from this train.
    8.2.2 Tester shall select either the total Cr or Cr+\6\ 
sample recovery option.
    8.2.3 Samples to be analyzed for both total Cr and 
Cr+\6\, shall be recovered using the Cr+\6\ sample 
option (Section 8.2.6).
    8.2.4 A field reagent blank shall be collected for either of the Cr 
or the Cr+\6\ analysis. If both analyses (Cr and 
Cr+\6\) are to be conducted on the samples, collect separate 
reagent blanks for each analysis.
    Note: Since particulate matter is not usually present at chromium 
electroplating and/or chromium anodizing operations, it is not necessary 
to filter the Cr+\6\ samples unless there is observed 
sediment in the collected solutions. If it is necessary to filter the 
Cr+\6\ solutions, please refer to Method 0061, Determination 
of Hexavalent Chromium Emissions From Stationary Sources, Section 7.4, 
Sample Preparation in SW-846 (see Reference 1).
    8.2.5 Total Cr Sample Option.
    8.2.5.1 Container No. 1. Measure the volume of the liquid in the 
first, second, and third impingers and quantitatively transfer into a 
labeled sample container.
    8.2.5.2 Use approximately 200 to 300 mL of the 0.1 N NaOH or 0.1 N 
NaHCO3 absorbing solution to rinse the probe nozzle, probe 
liner, three impingers, and connecting glassware; add this rinse to 
Container No. 1.
    8.2.6 Cr+\6\ Sample Option.
    8.2.6.1 Container No. 1. Measure and record the pH of the absorbing 
solution contained in the first impinger at the end of the sampling run 
using a pH indicator strip. The pH of the solution must be 
=8.5 for NaOH and =8.0 for NaHCO3. If 
it is not, discard the collected sample, increase the normality of the 
NaOH or NaHCO3 impinger absorbing solution to 0.5 N or to a 
solution normality approved by the Administrator and collect another air 
emission sample.
    8.2.6.2 After determining the pH of the first impinger solution, 
combine and measure the volume of the liquid in the first, second, and 
third impingers and quantitatively transfer into the labeled sample 
container.

[[Page 195]]

Use approximately 200 to 300 mL of the 0.1 N NaOH or 0.1 N 
NaHCO3 absorbing solution to rinse the probe nozzle, probe 
liner, three impingers, and connecting glassware; add this rinse to 
Container No. 1.
    8.2.7 Field Reagent Blank.
    8.2.7.1 Container No. 2.
    8.2.7.2 Place approximately 500 mL of the 0.1 N NaOH or 0.1 N 
NaHCO3 absorbing solution into a labeled sample container.
    8.3 Sample Preservation, Storage, and Transport.
    8.3.1 Total Cr Sample Option. Samples to be analyzed for total Cr 
need not be refrigerated.
    8.3.2 Cr+\6\ Sample Option. Samples to be analyzed for 
Cr+\6\ must be shipped and stored at 4 [deg]C. Allow 
Cr+\6\ samples to return to ambient temperature prior to 
analysis.
    8.4 Sample Holding Times.
    8.4.1 Total Cr Sample Option. Samples to be analyzed for total Cr 
shall be analyzed within 60 days of collection.
    8.4.2 Cr+\6\ Sample Option. Samples to be analyzed for 
Cr+\6\ shall be analyzed within 14 days of collection.

                           9.0 Quality Control

    9.1 ICP Quality Control.
    9.1.1 ICP Calibration Reference Standards. Prepare a calibration 
reference standard using the same alkaline matrix as the calibration 
standards; it should be at least 10 times the instrumental detection 
limit.
    9.1.1.1 This reference standard must be prepared from a different Cr 
stock solution source than that used for preparation of the calibration 
curve standards.
    9.1.1.2 Prior to sample analysis, analyze at least one reference 
standard.
    9.1.1.3 The calibration reference standard must be measured within 
10 percent of it's true value for the curve to be considered valid.
    9.1.1.4 The curve must be validated before sample analyses are 
performed.
    9.1.2 ICP Continuing Check Standard.
    9.1.2.1 Perform analysis of the check standard with the field 
samples as described in Section 11.2 (at least after every 10 samples, 
and at the end of the analytical run).
    9.1.2.2 The check standard can either be the mid-range calibration 
standard or the reference standard. The results of the check standard 
shall agree within 10 percent of the expected value; if not, terminate 
the analyses, correct the problem, recalibrate the instrument, and rerun 
all samples analyzed subsequent to the last acceptable check standard 
analysis.
    9.1.3 ICP Calibration Blank.
    9.1.3.1 Perform analysis of the calibration blank with the field 
samples as described in Section 11.2 (at least after every 10 samples, 
and at the end of the analytical run).
    9.1.3.2 The results of the calibration blank shall agree within 
three standard deviations of the mean blank value. If not, analyze the 
calibration blank two more times and average the results. If the average 
is not within three standard deviations of the background mean, 
terminate the analyses, correct the problem, recalibrate, and reanalyze 
all samples analyzed subsequent to the last acceptable calibration blank 
analysis.
    9.1.4 ICP Interference Check. Prepare an interference check solution 
that contains known concentrations of interfering elements that will 
provide an adequate test of the correction factors in the event of 
potential spectral interferences.
    9.1.4.1 Two potential interferences, iron and manganese, may be 
prepared as 1000 [mu]g/mL and 200 [mu]g/mL solutions, respectively. The 
solutions should be prepared in dilute HNO3 (1-5 percent). 
Particular care must be used to ensure that the solutions and/or salts 
used to prepare the solutions are of ICP grade purity (i.e., that no 
measurable Cr contamination exists in the salts/solutions). Commercially 
prepared interfering element check standards are available.
    9.1.4.2 Verify the interelement correction factors every three 
months by analyzing the interference check solution. The correction 
factors are calculated according to the instrument manufacturer's 
directions. If the interelement correction factors are used properly, no 
false Cr should be detected.
    9.1.4.3 Negative results with an absolute value greater than three 
(3) times the detection limit are usually the results of the background 
correction position being set incorrectly. Scan the spectral region to 
ensure that the correction position has not been placed on an 
interfering peak.
    9.1.5 ICP Duplicate Sample Analysis. Perform one duplicate sample 
analysis for each compliance sample batch (3 runs).
    9.1.5.1 As there is no sample preparation required for the ICP 
analysis, a duplicate analysis is defined as a repeat analysis of one of 
the field samples. The selected sample shall be analyzed using the same 
procedures that were used to analyze the original sample.
    9.1.5.2 Duplicate sample analyses shall agree within 10 percent of 
the original measurement value.
    9.1.5.3 Report the original analysis value for the sample and report 
the duplicate analysis value as the QC check value. If agreement is not 
achieved, perform the duplicate analysis again. If agreement is not 
achieved the second time, perform corrective action to identify and 
correct the problem before analyzing the sample for a third time.
    9.1.6 ICP Matrix Spiking. Spiked samples shall be prepared and 
analyzed daily to ensure that there are no matrix effects, that samples 
and standards have been matrix-matched, and that the laboratory 
equipment is operating properly.

[[Page 196]]

    9.1.6.1 Spiked sample recovery analyses should indicate a recovery 
for the Cr spike of between 75 and 125 percent.
    9.1.6.2 Cr levels in the spiked sample should provide final solution 
concentrations that are within the linear portion of the calibration 
curve, as well as, at a concentration level at least: equal to that of 
the original sample; and, ten (10) times the detection limit.
    9.1.6.3 If the spiked sample concentration meets the stated criteria 
but exceeds the linear calibration range, the spiked sample must be 
diluted with the field absorbing solution.
    9.1.6.4 If the recoveries for the Cr spiked samples do not meet the 
specified criteria, perform corrective action to identify and correct 
the problem prior to reanalyzing the samples.
    9.1.7 ICP Field Reagent Blank.
    9.1.7.1 Analyze a minimum of one matrix-matched field reagent blank 
(Section 8.2.4) per sample batch to determine if contamination or memory 
effects are occurring.
    9.1.7.2 If contamination or memory effects are observed, perform 
corrective action to identify and correct the problem before reanalyzing 
the samples.
    9.1.8 Audit Sample Analysis.
    9.1.8.1 When the method is used to analyze samples to demonstrate 
compliance with a source emission regulation, an audit sample must be 
analyzed, subject to availability.
    9.1.8.2 Concurrently analyze the audit sample and the compliance 
samples in the same manner to evaluate the technique of the analyst and 
the standards preparation.
    9.1.8.3 The same analyst, analytical reagents, and analytical system 
shall be used for the compliance samples and the audit sample. If this 
condition is met, duplicate auditing of subsequent compliance analyses 
for the same enforcement agency within a 30-day period is waived. An 
audit sample set may not be used to validate different sets of 
compliance samples under the jurisdiction of separate enforcement 
agencies, unless prior arrangements have been made with both enforcement 
agencies.
    9.1.9 Audit Sample Results.
    9.1.9.1 Calculate the audit sample concentrations and submit results 
using the instructions provided with the audit samples.
    9.1.9.2 Report the results of the audit samples and the compliance 
determination samples along with their identification numbers, and the 
analyst's name to the responsible enforcement authority. Include this 
information with reports of any subsequent compliance analyses for the 
same enforcement authority during the 30-day period.
    9.1.9.3 The concentrations of the audit samples obtained by the 
analyst shall agree within the values specified by the compliance 
auditor. If the specified range is not met, reanalyze the compliance and 
audit samples, and include initial and reanalysis values in the test 
report.
    9.1.9.4 Failure to meet the specified range may require retests 
unless the audit problems are resolved. However, if the audit results do 
not affect the compliance or noncompliance status of the affected 
facility, the Administrator may waive the reanalysis requirement, 
further audits, or retests and accept the results of the compliance 
test. While steps are being taken to resolve audit analysis problems, 
the Administrator may also choose to use the data to determine the 
compliance or noncompliance status of the affected facility.
    9.2 GFAAS Quality Control.
    9.2.1 GFAAS Calibration Reference Standards. The calibration curve 
must be verified by using at least one calibration reference standard 
(made from a reference material or other independent standard material) 
at or near the mid-range of the calibration curve.
    9.2.1.1 The calibration curve must be validated before sample 
analyses are performed.
    9.2.1.2 The calibration reference standard must be measured within 
10 percent of its true value for the curve to be considered valid.
    9.2.2 GFAAS Continuing Check Standard.
    9.2.2.1 Perform analysis of the check standard with the field 
samples as described in Section 11.4 (at least after every 10 samples, 
and at the end of the analytical run).
    9.2.2.2 These standards are analyzed, in part, to monitor the life 
and performance of the graphite tube. Lack of reproducibility or a 
significant change in the signal for the check standard may indicate 
that the graphite tube should be replaced.
    9.2.2.3 The check standard may be either the mid-range calibration 
standard or the reference standard.
    9.2.2.4 The results of the check standard shall agree within 10 
percent of the expected value.
    9.2.2.5 If not, terminate the analyses, correct the problem, 
recalibrate the instrument, and reanalyze all samples analyzed 
subsequent to the last acceptable check standard analysis.
    9.2.3 GFAAS Calibration Blank.
    9.2.3.1 Perform analysis of the calibration blank with the field 
samples as described in Section 11.4 (at least after every 10 samples, 
and at the end of the analytical run).
    9.2.3.2 The calibration blank is analyzed to monitor the life and 
performance of the graphite tube as well as the existence of any memory 
effects. Lack of reproducibility or a significant change in the signal, 
may indicate that the graphite tube should be replaced.
    9.2.3.3 The results of the calibration blank shall agree within 
three standard deviations of the mean blank value.

[[Page 197]]

    9.2.3.4 If not, analyze the calibration blank two more times and 
average the results. If the average is not within three standard 
deviations of the background mean, terminate the analyses, correct the 
problem, recalibrate, and reanalyze all samples analyzed subsequent to 
the last acceptable calibration blank analysis.
    9.2.4 GFAAS Duplicate Sample Analysis. Perform one duplicate sample 
analysis for each compliance sample batch (3 runs).
    9.2.4.1 A digested aliquot of the selected sample is processed and 
analyzed using the identical procedures that were used for the whole 
sample preparation and analytical efforts.
    9.2.4.2 Duplicate sample analyses results incorporating duplicate 
digestions shall agree within 20 percent for sample results exceeding 
ten (10) times the detection limit.
    9.2.4.3 Report the original analysis value for the sample and report 
the duplicate analysis value as the QC check value.
    9.2.4.4 If agreement is not achieved, perform the duplicate analysis 
again. If agreement is not achieved the second time, perform corrective 
action to identify and correct the problem before analyzing the sample 
for a third time.
    9.2.5 GFAAS Matrix Spiking.
    9.2.5.1 Spiked samples shall be prepared and analyzed daily to 
ensure that (1) correct procedures are being followed, (2) there are no 
matrix effects and (3) all equipment is operating properly.
    9.2.5.2 Cr spikes are added prior to any sample preparation.
    9.2.5.3 Cr levels in the spiked sample should provide final solution 
concentrations that are within the linear portion of the calibration 
curve, as well as, at a concentration level at least: equal to that of 
the original sample; and, ten (10) times the detection limit.
    9.2.5.4 Spiked sample recovery analyses should indicate a recovery 
for the Cr spike of between 75 and 125 percent.
    9.2.5.5 If the recoveries for the Cr spiked samples do not meet the 
specified criteria, perform corrective action to identify and correct 
the problem prior to reanalyzing the samples.
    9.2.6 GFAAS Method of Standard Additions.
    9.2.6.1 Method of Standard Additions. Perform procedures in Section 
5.4 of Method 12 (40 CFR Part 60, Appendix A)
    9.2.6.2 Whenever sample matrix problems are suspected and standard/
sample matrix matching is not possible or whenever a new sample matrix 
is being analyzed, perform referenced procedures to determine if the 
method of standard additions is necessary.
    9.2.7 GFAAS Field Reagent Blank.
    9.2.7.1 Analyze a minimum of one matrix-matched field reagent blank 
(Section 8.2.4) per sample batch to determine if contamination or memory 
effects are occurring.
    9.2.7.2 If contamination or memory effects are observed, perform 
corrective action to identify and correct the problem before reanalyzing 
the samples.
    9.2.8 Audit Sample Analysis.
    9.2.8.1 When the method is used to analyze samples to demonstrate 
compliance with a source emission regulation, an audit sample must be 
analyzed, subject to availability.
    9.2.8.2 Concurrently analyze the audit sample and the compliance 
samples in the same manner to evaluate the technique of the analyst and 
the standards preparation.
    9.2.8.3 The same analyst, analytical reagents, and analytical system 
shall be used for the compliance samples and the audit sample. If this 
condition is met, duplicate auditing of subsequent compliance analyses 
for the same enforcement agency within a 30-day period is waived. An 
audit sample set may not be used to validate different sets of 
compliance samples under the jurisdiction of separate enforcement 
agencies, unless prior arrangements have been made with both enforcement 
agencies.
    9.2.9 Audit Sample Results.
    9.2.9.1 Calculate the audit sample concentrations and submit results 
using the instructions provided with the audit samples.
    9.2.9.2 Report the results of the audit samples and the compliance 
determination samples along with their identification numbers, and the 
analyst's name to the responsible enforcement authority. Include this 
information with reports of any subsequent compliance analyses for the 
same enforcement authority during the 30-day period.
    9.2.9.3 The concentrations of the audit samples obtained by the 
analyst shall agree within the values specified by the compliance 
auditor. If the specified range is not met, reanalyze the compliance and 
audit samples, and include initial and reanalysis values in the test 
report.
    9.2.9.4 Failure to meet the specified range may require retests 
unless the audit problems are resolved. However, if the audit results do 
not affect the compliance or noncompliance status of the affected 
facility, the Administrator may waive the reanalysis requirement, 
further audits, or retests and accept the results of the compliance 
test. While steps are being taken to resolve audit analysis problems, 
the Administrator may also choose to use the data to determine the 
compliance or noncompliance status of the affected facility.
    9.3 IC/PCR Quality Control.
    9.3.1 IC/PCR Calibration Reference Standards.
    9.3.1.1 Prepare a calibration reference standard at a concentration 
that is at or near the mid-point of the calibration curve using the same 
alkaline matrix as the calibration standards. This reference standard

[[Page 198]]

should be prepared from a different Cr stock solution than that used to 
prepare the calibration curve standards. The reference standard is used 
to verify the accuracy of the calibration curve.
    9.3.1.2 The curve must be validated before sample analyses are 
performed. Prior to sample analysis, analyze at least one reference 
standard with an expected value within the calibration range.
    9.3.1.3 The results of this reference standard analysis must be 
within 10 percent of the true value of the reference standard for the 
calibration curve to be considered valid.
    9.3.2 IC/PCR Continuing Check Standard and Calibration Blank.
    9.3.2.1 Perform analysis of the check standard and the calibration 
blank with the field samples as described in Section 11.6 (at least 
after every 10 samples, and at the end of the analytical run).
    9.3.2.2 The result from the check standard must be within 10 percent 
of the expected value.
    9.3.2.3 If the 10 percent criteria is exceeded, excessive drift and/
or instrument degradation may have occurred, and must be corrected 
before further analyses can be performed.
    9.3.2.4 The results of the calibration blank analyses must agree 
within three standard deviations of the mean blank value.
    9.3.2.5 If not, analyze the calibration blank two more times and 
average the results.
    9.3.2.6 If the average is not within three standard deviations of 
the background mean, terminate the analyses, correct the problem, 
recalibrate, and reanalyze all samples analyzed subsequent to the last 
acceptable calibration blank analysis.
    9.3.3 IC/PCR Duplicate Sample Analysis.
    9.3.3.1 Perform one duplicate sample analysis for each compliance 
sample batch (3 runs).
    9.3.3.2 An aliquot of the selected sample is prepared and analyzed 
using procedures identical to those used for the emission samples (for 
example, filtration and/or, if necessary, preconcentration).
    9.3.3.3 Duplicate sample injection results shall agree within 10 
percent for sample results exceeding ten (10) times the detection limit.
    9.3.3.4 Report the original analysis value for the sample and report 
the duplicate analysis value as the QC check value.
    9.3.3.5 If agreement is not achieved, perform the duplicate analysis 
again.
    9.3.3.6 If agreement is not achieved the second time, perform 
corrective action to identify and correct the problem prior to analyzing 
the sample for a third time.
    9.3.4 ICP/PCR Matrix Spiking. Spiked samples shall be prepared and 
analyzed with each sample set to ensure that there are no matrix 
effects, that samples and standards have been matrix-matched, and that 
the equipment is operating properly.
    9.3.4.1 Spiked sample recovery analysis should indicate a recovery 
of the Cr+\6\ spike between 75 and 125 percent.
    9.3.4.2 The spiked sample concentration should be within the linear 
portion of the calibration curve and should be equal to or greater than 
the concentration of the original sample. In addition, the spiked sample 
concentration should be at least ten (10) times the detection limit.
    9.3.4.3 If the recoveries for the Cr+\6\ spiked samples 
do not meet the specified criteria, perform corrective action to 
identify and correct the problem prior to reanalyzing the samples.
    9.3.5 IC/PCR Field Reagent Blank.
    9.3.5.1 Analyze a minimum of one matrix-matched field reagent blank 
(Section 8.2.4) per sample batch to determine if contamination or memory 
effects are occurring.
    9.3.5.2 If contamination or memory effects are observed, perform 
corrective action to identify and correct the problem before reanalyzing 
the samples.
    9.3.6 Audit Sample Analysis.
    9.3.6.1 When the method is used to analyze samples to demonstrate 
compliance with source emission regulation, an audit sample must be 
analyzed, subject to availability.
    9.3.6.2 Concurrently analyze the audit sample and the compliance 
samples in the same manner to evaluate the technique of the analyst and 
the standards preparation.
    9.3.6.3 The same analyst, analytical reagents, and analytical system 
shall be used for the compliance samples and the audit sample. If this 
condition is met, duplicate auditing of subsequent compliance analyses 
for the same enforcement agency within a 30-day period is waived. An 
audit sample set may not be used to validate different sets of 
compliance samples under the jurisdiction of separate enforcement 
agencies, unless prior arrangements have been made with both enforcement 
agencies.
    9.3.7 Audit Sample Results.
    9.3.7.1 Calculate the audit sample concentrations and submit results 
using the instructions provided with the audit samples.
    9.3.7.2 Report the results of the audit samples and the compliance 
determination samples along with their identification numbers, and the 
analyst's name to the responsible enforcement authority. Include this 
information with reports of any subsequent compliance analyses for the 
same enforcement authority during the 30-day period.
    9.3.7.3 The concentrations of the audit samples obtained by the 
analyst shall agree within the values specified by the compliance 
auditor. If the specified range is not met, reanalyze the compliance and 
audit samples, and include initial and reanalysis values in the test 
report.

[[Page 199]]

    9.3.7.4 Failure to meet the specified range may require retests 
unless the audit problems are resolved. However, if the audit results do 
not affect the compliance or noncompliance status of the affected 
facility, the Administrator may waive the reanalysis requirement, 
further audits, or retests and accept the results of the compliance 
test. While steps are being taken to resolve audit analysis problems, 
the Administrator may also choose to use the data to determine the 
compliance or noncompliance status of the affected facility.

                  10.0 Calibration and Standardization

    10.1 Sampling Train Calibration. Perform calibrations described in 
Method 5, (40 CFR Part 60, Appendix A). The alternate calibration 
procedures described in Method 5, may also be used.
    10.2 ICP Calibration.
    10.2.1 Calibrate the instrument according to the instrument 
manufacturer's recommended procedures, using a calibration blank and 
three standards for the initial calibration.
    10.2.2 Calibration standards should be prepared fresh daily, as 
described in Section 7.3.8. Be sure that samples and calibration 
standards are matrix matched. Flush the system with the calibration 
blank between each standard.
    10.2.3 Use the average intensity of multiple exposures (3 or more) 
for both standardization and sample analysis to reduce random error.
    10.2.4 Employing linear regression, calculate the correlation 
coefficient .
    10.2.5 The correlation coefficient must equal or exceed 0.995.
    10.2.6 If linearity is not acceptable, prepare and rerun another set 
of calibration standards or reduce the range of the calibration 
standards, as necessary.
    10.3 GFAAS Calibration.
    10.3.1 For instruments that measure directly in concentration, set 
the instrument software to display the correct concentration, if 
applicable.
    10.3.2 Curve must be linear in order to correctly perform the method 
of standard additions which is customarily performed automatically with 
most instrument computer-based data systems.
    10.3.3 The calibration curve (direct calibration or standard 
additions) must be prepared daily with a minimum of a calibration blank 
and three standards that are prepared fresh daily.
    10.3.4 The calibration curve acceptance criteria must equal or 
exceed 0.995.
    10.3.5 If linearity is not acceptable, prepare and rerun another set 
of calibration standards or reduce the range of calibration standards, 
as necessary.
    10.4 IC/PCR Calibration.
    10.4.1 Prepare a calibration curve using the calibration blank and 
three calibration standards prepared fresh daily as described in Section 
7.3.8.
    10.4.2 The calibration curve acceptance criteria must equal or 
exceed 0.995.
    10.4.3 If linearity is not acceptable, remake and/or rerun the 
calibration standards. If the calibration curve is still unacceptable, 
reduce the range of the curve.
    10.4.4 Analyze the standards with the field samples as described in 
Section 11.6.

                       11.0 Analytical Procedures

    Note: The method determines the chromium concentration in [mu]g Cr/
mL. It is important that the analyst measure the field sample volume 
prior to analyzing the sample. This will allow for conversion of [mu]g 
Cr/mL to [mu]g Cr/sample.

    11.1 ICP Sample Preparation.
    11.1.1 The ICP analysis is performed directly on the alkaline 
impinger solution; acid digestion is not necessary, provided the samples 
and standards are matrix matched.
    11.1.2 The ICP analysis should only be employed when the solution 
analyzed has a Cr concentration greater than 35 [mu]g/L or five times 
the method detection limit as determined according to Appendix B in 40 
CFR Part 136 or by other commonly accepted analytical procedures.
    11.2 ICP Sample Analysis.
    11.2.1 The ICP analysis is applicable for the determination of total 
chromium only.
    11.2.2 ICP Blanks. Two types of blanks are required for the ICP 
analysis.
    11.2.2.1 Calibration Blank. The calibration blank is used in 
establishing the calibration curve. For the calibration blank, use 
either 0.1 N NaOH or 0.1 N NaHCO3, whichever is used for the 
impinger absorbing solution. The calibration blank can be prepared fresh 
in the laboratory; it does not have to be prepared from the same batch 
of solution that was used in the field. A sufficient quantity should be 
prepared to flush the system between standards and samples.
    11.2.2.2 Field Reagent Blank. The field reagent blank is collected 
in the field during the testing program. The field reagent blank 
(Section 8.2.4) is an aliquot of the absorbing solution prepared in 
Section 7.1.2. The reagent blank is used to assess possible 
contamination resulting from sample processing.
    11.2.3 ICP Instrument Adjustment.
    11.2.3.1 Adjust the ICP instrument for proper operating parameters 
including wavelength, background correction settings (if necessary), and 
interfering element correction settings (if necessary).
    11.2.3.2 The instrument must be allowed to become thermally stable 
before beginning measurements (usually requiring at least 30

[[Page 200]]

min of operation prior to calibration). During this warmup period, the 
optical calibration and torch position optimization may be performed 
(consult the operator's manual).
    11.2.4 ICP Instrument Calibration.
    11.2.4.1 Calibrate the instrument according to the instrument 
manufacturer's recommended procedures, and the procedures specified in 
Section 10.2.
    11.2.4.2 Prior to analyzing the field samples, reanalyze the highest 
calibration standard as if it were a sample.
    11.2.4.3 Concentration values obtained should not deviate from the 
actual values or from the established control limits by more than 5 
percent, whichever is lower (see Sections 9.1 and 10.2).
    11.2.4.4 If they do, follow the recommendations of the instrument 
manufacturer to correct the problem.
    11.2.5 ICP Operational Quality Control Procedures.
    11.2.5.1 Flush the system with the calibration blank solution for at 
least 1 min before the analysis of each sample or standard.
    11.2.5.2 Analyze the continuing check standard and the calibration 
blank after each batch of 10 samples.
    11.2.5.3 Use the average intensity of multiple exposures for both 
standardization and sample analysis to reduce random error.
    11.2.6 ICP Sample Dilution.
    11.2.6.1 Dilute and reanalyze samples that are more concentrated 
than the linear calibration limit or use an alternate, less sensitive Cr 
wavelength for which quality control data have already been established.
    11.2.6.2 When dilutions are performed, the appropriate factors must 
be applied to sample measurement results.
    11.2.7 Reporting Analytical Results. All analytical results should 
be reported in [mu]g Cr/mL using three significant figures. Field sample 
volumes (mL) must be reported also.
    11.3 GFAAS Sample Preparation.
    11.3.1 GFAAS Acid Digestion. An acid digestion of the alkaline 
impinger solution is required for the GFAAS analysis.
    11.3.1.1 In a beaker, add 10 mL of concentrated HNO3 to a 
100 mL sample aliquot that has been well mixed. Cover the beaker with a 
watch glass. Place the beaker on a hot plate and reflux the sample to 
near dryness. Add another 5 mL of concentrated HNO3 to 
complete the digestion. Again, carefully reflux the sample volume to 
near dryness. Rinse the beaker walls and watch glass with reagent water.
    11.3.1.2 The final concentration of HNO3 in the solution 
should be 1 percent (v/v).
    11.3.1.3 Transfer the digested sample to a 50-mL volumetric flask. 
Add 0.5 mL of concentrated HNO3 and 1 mL of the 10 [mu]g/mL 
of Ca(NO3)2. Dilute to 50 mL with reagent water.
    11.3.2 HNO3 Concentration. A different final volume may 
be used based on the expected Cr concentration, but the HNO3 
concentration must be maintained at 1 percent (v/v).
    11.4 GFAAS Sample Analysis.
    11.4.1 The GFAAS analysis is applicable for the determination of 
total chromium only.
    11.4.2 GFAAS Blanks. Two types of blanks are required for the GFAAS 
analysis.
    11.4.2.1 Calibration Blank. The 1.0 percent HNO3 is the 
calibration blank which is used in establishing the calibration curve.
    11.4.2.2 Field Reagent Blank. An aliquot of the 0.1 N NaOH solution 
or the 0.1 N NaHCO3 prepared in Section 7.1.2 is collected 
for the field reagent blank. The field reagent blank is used to assess 
possible contamination resulting from processing the sample.
    11.4.2.2.1 The reagent blank must be subjected to the entire series 
of sample preparation and analytical procedures, including the acid 
digestion.
    11.4.2.2.2 The reagent blank's final solution must contain the same 
acid concentration as the sample solutions.
    11.4.3 GFAAS Instrument Adjustment.
    11.4.3.1 The 357.9 nm wavelength line shall be used.
    11.4.3.2 Follow the manufacturer's instructions for all other 
spectrophotometer operating parameters.
    11.4.4 Furnace Operational Parameters. Parameters suggested by the 
manufacturer should be employed as guidelines.
    11.4.4.1 Temperature-sensing mechanisms and temperature controllers 
can vary between instruments and/or with time; the validity of the 
furnace operating parameters must be periodically confirmed by 
systematically altering the furnace parameters while analyzing a 
standard. In this manner, losses of analyte due to higher-than-necessary 
temperature settings or losses in sensitivity due to less than optimum 
settings can be minimized.
    11.4.4.2 Similar verification of furnace operating parameters may be 
required for complex sample matrices (consult instrument manual for 
additional information). Calibrate the GFAAS system following the 
procedures specified in Section 10.3.
    11.4.5 GFAAS Operational Quality Control Procedures.
    11.4.5.1 Introduce a measured aliquot of digested sample into the 
furnace and atomize.
    11.4.5.2 If the measured concentration exceeds the calibration 
range, the sample should be diluted with the calibration blank solution 
(1.0 percent HNO3) and reanalyzed.
    11.4.5.3 Consult the operator's manual for suggested injection 
volumes. The use of multiple injections can improve accuracy and assist 
in detecting furnace pipetting errors.
    11.4.5.4 Analyze a minimum of one matrix-matched reagent blank per 
sample batch

[[Page 201]]

to determine if contamination or any memory effects are occurring.
    11.4.5.5 Analyze a calibration blank and a continuing check standard 
after approximately every batch of 10 sample injections.
    11.4.6 GFAAS Sample Dilution.
    11.4.6.1 Dilute and reanalyze samples that are more concentrated 
than the instrument calibration range.
    11.4.6.2 If dilutions are performed, the appropriate factors must be 
applied to sample measurement results.
    11.4.7 Reporting Analytical Results.
    11.4.7.1 Calculate the Cr concentrations by the method of standard 
additions (see operator's manual) or, from direct calibration. All 
dilution and/or concentration factors must be used when calculating the 
results.
    11.4.7.2 Analytical results should be reported in [mu]g Cr/mL using 
three significant figures. Field sample volumes (mL) must be reported 
also.
    11.5 IC/PCR Sample Preparation.
    11.5.1 Sample pH. Measure and record the sample pH prior to 
analysis.
    11.5.2 Sample Filtration. Prior to preconcentration and/or analysis, 
filter all field samples through a 0.45-[mu]m filter. The filtration 
step should be conducted just prior to sample injection/analysis.
    11.5.2.1 Use a portion of the sample to rinse the syringe filtration 
unit and acetate filter and then collect the required volume of 
filtrate.
    11.5.2.2 Retain the filter if total Cr is to be determined also.
    11.5.3 Sample Preconcentration (older instruments).
    11.5.3.1 For older instruments, a preconcentration system may be 
used in conjunction with the IC/PCR to increase sensitivity for trace 
levels of Cr+6.
    11.5.3.2 The preconcentration is accomplished by selectively 
retaining the analyte on a solid absorbent, followed by removal of the 
analyte from the absorbent (consult instrument manual).
    11.5.3.3 For a manual system, position the injection valve so that 
the eluent displaces the concentrated Cr+\6\ sample, 
transferring it from the preconcentration column and onto the IC anion 
separation column.
    11.6 IC/PCR Sample Analyses.
    11.6.1 The IC/PCR analysis is applicable for hexavalent chromium 
measurements only.
    11.6.2 IC/PCR Blanks. Two types of blanks are required for the IC/
PCR analysis.
    11.6.2.1 Calibration Blank. The calibration blank is used in 
establishing the analytical curve. For the calibration blank, use either 
0.1 N NaOH or 0.1 N NaHCO3, whichever is used for the 
impinger solution. The calibration blank can be prepared fresh in the 
laboratory; it does not have to be prepared from the same batch of 
absorbing solution that is used in the field.
    11.6.2.2 Field Reagent Blank. An aliquot of the 0.1 N NaOH solution 
or the 0.1 N NaHCO3 solution prepared in Section 7.1.2 is 
collected for the field reagent blank. The field reagent blank is used 
to assess possible contamination resulting from processing the sample.
    11.6.3 Stabilized Baseline. Prior to sample analysis, establish a 
stable baseline with the detector set at the required attenuation by 
setting the eluent and post-column reagent flow rates according to the 
manufacturers recommendations.
    Note: As long as the ratio of eluent flow rate to PCR flow rate 
remains constant, the standard curve should remain linear. Inject a 
sample of reagent water to ensure that no Cr+6 appears in the 
water blank.
    11.6.4 Sample Injection Loop. Size of injection loop is based on 
standard/sample concentrations and the selected attenuator setting.
    11.6.4.1 A 50-[mu]L loop is normally sufficient for most higher 
concentrations.
    11.6.4.2 The sample volume used to load the injection loop should be 
at least 10 times the loop size so that all tubing in contact with the 
sample is thoroughly flushed with the new sample to prevent cross 
contamination.
    11.6.5 IC/PCR Instrument Calibration.
    11.6.5.1 First, inject the calibration standards prepared, as 
described in Section 7.3.8 to correspond to the appropriate 
concentration range, starting with the lowest standard first.
    11.6.5.2 Check the performance of the instrument and verify the 
calibration using data gathered from analyses of laboratory blanks, 
calibration standards, and a quality control sample.
    11.6.5.3 Verify the calibration by analyzing a calibration reference 
standard. If the measured concentration exceeds the established value by 
more than 10 percent, perform a second analysis. If the measured 
concentration still exceeds the established value by more than 10 
percent, terminate the analysis until the problem can be identified and 
corrected.
    11.6.6 IC/PCR Instrument Operation.
    11.6.6.1 Inject the calibration reference standard (as described in 
Section 9.3.1), followed by the field reagent blank (Section 8.2.4), and 
the field samples.
    11.6.6.1.1 Standards (and QC standards) and samples are injected 
into the sample loop of the desired size (use a larger size loop for 
greater sensitivity). The Cr+6 is collected on the resin bed 
of the column.
    11.6.6.1.2 After separation from other sample components, the 
Cr+6 forms a specific complex in the post-column reactor with 
the DPC reaction solution, and the complex is detected by visible 
absorbance at a maximum wavelength of 540 nm.

[[Page 202]]

    11.6.6.1.3 The amount of absorbance measured is proportional to the 
concentration of the Cr+6 complex formed.
    11.6.6.1.4 The IC retention time and the absorbance of the 
Cr+6 complex with known Cr+6 standards analyzed 
under identical conditions must be compared to provide both qualitative 
and quantitative analyses.
    11.6.6.1.5 If a sample peak appears near the expected retention time 
of the Cr+6 ion, spike the sample according to Section 9.3.4 
to verify peak identity.
    11.6.7 IC/PCR Operational Quality Control Procedures.
    11.6.7.1 Samples should be at a pH =8.5 for NaOH and 
=8.0 if using NaHCO3; document any discrepancies.
    11.6.7.2 Refrigerated samples should be allowed to equilibrate to 
ambient temperature prior to preparation and analysis.
    11.6.7.3 Repeat the injection of the calibration standards at the 
end of the analytical run to assess instrument drift. Measure areas or 
heights of the Cr+6/DPC complex chromatogram peaks.
    11.6.7.4 To ensure the precision of the sample injection (manual or 
autosampler), the response for the second set of injected standards must 
be within 10 percent of the average response.
    11.6.7.5 If the 10 percent criteria duplicate injection cannot be 
achieved, identify the source of the problem and rerun the calibration 
standards.
    11.6.7.6 Use peak areas or peak heights from the injections of 
calibration standards to generate a linear calibration curve. From the 
calibration curve, determine the concentrations of the field samples.
    11.6.8 IC/PCR Sample Dilution.
    11.6.8.1 Samples having concentrations higher than the established 
calibration range must be diluted into the calibration range and re-
analyzed.
    11.6.8.2 If dilutions are performed, the appropriate factors must be 
applied to sample measurement results.
    11.6.9 Reporting Analytical Results. Results should be reported in 
[mu]g Cr+6/mL using three significant figures. Field sample 
volumes (mL) must be reported also.

                   12.0 Data Analysis and Calculations

    12.1 Pretest Calculations.
    12.1.1 Pretest Protocol (Site Test Plan).
    12.1.1.1 The pretest protocol should define and address the test 
data quality objectives (DQOs), with all assumptions, that will be 
required by the end user (enforcement authority); what data are needed? 
why are the data needed? how will the data be used? what are method 
detection limits? and what are estimated target analyte levels for the 
following test parameters.
    12.1.1.1.1 Estimated source concentration for total chromium and/or 
Cr+6.
    12.1.1.1.2 Estimated minimum sampling time and/or volume required to 
meet method detection limit requirements (Appendix B 40 CFR Part 136) 
for measurement of total chromium and/or Cr+6.
    12.1.1.1.3 Demonstrate that planned sampling parameters will meet 
DQOs. The protocol must demonstrate that the planned sampling parameters 
calculated by the tester will meet the needs of the source and the 
enforcement authority.
    12.1.1.2 The pre-test protocol should include information on 
equipment, logistics, personnel, process operation, and other resources 
necessary for an efficient and coordinated test.
    12.1.1.3 At a minimum, the pre-test protocol should identify and be 
approved by the source, the tester, the analytical laboratory, and the 
regulatory enforcement authority. The tester should not proceed with the 
compliance testing before obtaining approval from the enforcement 
authority.
    12.1.2 Post Test Calculations.
    12.1.2.1 Perform the calculations, retaining one extra decimal 
figure beyond that of the acquired data. Round off figures after final 
calculations.
    12.1.2.2 Nomenclature.

CS = Concentration of Cr in sample solution, [mu]g Cr/mL.
Ccr = Concentration of Cr in stack gas, dry basis, corrected 
to standard conditions, mg/dscm.
D = Digestion factor, dimension less.
F = Dilution factor, dimension less.
MCr = Total Cr in each sample, [mu]g.
Vad = Volume of sample aliquot after digestion, mL.
Vaf = Volume of sample aliquot after dilution, mL.
Vbd = Volume of sample aliquot submitted to digestion, mL.
Vbf = Volume of sample aliquot before dilution, mL.
VmL = Volume of impinger contents plus rinses, mL.
Vm(std) = Volume of gas sample measured by the dry gas meter, 
corrected to standard conditions, dscm.

    12.1.2.3 Dilution Factor. The dilution factor is the ratio of the 
volume of sample aliquot after dilution to the volume before dilution. 
This ratio is given by the following equation:

[[Page 203]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.573

    12.1.2.4 Digestion Factor. The digestion factor is the ratio of the 
volume of sample aliquot after digestion to the volume before digestion. 
This ratio is given by Equation 306-2.
[GRAPHIC] [TIFF OMITTED] TR17OC00.574

    12.1.2.5 Total Cr in Sample. Calculate MCr, the total [mu]g Cr in 
each sample, using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.575

    12.1.2.6 Average Dry Gas Meter Temperature and Average Orifice 
Pressure Drop. Same as Method 5.
    12.1.2.7 Dry Gas Volume, Volume of Water Vapor, Moisture Content. 
Same as Method 5.
    12.1.2.8 Cr Emission Concentration (CCr). Calculate 
CCr, the Cr concentration in the stack gas, in mg/dscm on a 
dry basis, corrected to standard conditions using the following 
equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.576

    12.1.2.9 Isokinetic Variation, Acceptable Results. Same as Method 5.

                         13.0 Method Performance

    13.1 Range. The recommended working range for all of the three 
analytical techniques starts at five times the analytical detection 
limit (see also Section 13.2.2). The upper limit of all three techniques 
can be extended indefinitely by appropriate dilution.
    13.2 Sensitivity.
    13.2.1 Analytical Sensitivity. The estimated instrumental detection 
limits listed are provided as a guide for an instrumental limit. The 
actual method detection limits are sample and instrument dependent and 
may vary as the sample matrix varies.
    13.2.1.2 ICP Analytical Sensitivity. The minimum estimated detection 
limits for ICP, as reported in Method 6010A and the recently revised 
Method 6010B of SW-846 (Reference 1), are 7.0 [mu]g Cr/L and 4.7 [mu]g 
Cr/L, respectively.
    13.2.1.3 GFAAS Analytical Sensitivity. The minimum estimated 
detection limit for GFAAS, as reported in Methods 7000A and 7191 of SW-
846 (Reference 1), is 1 [mu]g Cr/L.
    13.2.1.4 IC/PCR Analytical Sensitivity. The minimum detection limit 
for IC/PCR with a preconcentrator, as reported in Methods 0061 and 7199 
of SW-846 (Reference 1), is 0.05 [mu]g Cr\+6\/L.
    1.3.2.1.5 Determination of Detection Limits. The laboratory 
performing the Cr\+6\ measurements must determine the method detection 
limit on a quarterly basis using a suitable procedure such as that found 
in 40 CFR, Part 136, Appendix B. The determination should be made on 
samples in the appropriate alkaline matrix. Normally this involves the 
preparation (if applicable) and consecutive measurement of seven (7) 
separate aliquots of a sample with a concentration <5 times the expected 
detection limit. The detection limit is 3.14 times the standard 
deviation of these results.

[[Page 204]]

    13.2.2 In-stack Sensitivity. The in-stack sensitivity depends upon 
the analytical detection limit, the volume of stack gas sampled, the 
total volume of the impinger absorbing solution plus the rinses, and, in 
some cases, dilution or concentration factors from sample preparation. 
Using the analytical detection limits given in Sections 13.2.1.1, 
13.2.1.2, and 13.2.1.3; a stack gas sample volume of 1.7 dscm; a total 
liquid sample volume of 500 mL; and the digestion concentration factor 
of 1/2 for the GFAAS analysis; the corresponding in-stack detection 
limits are 0.0014 mg Cr/dscm to 0.0021 mg Cr/dscm for ICP, 0.00015 mg 
Cr/dscm for GFAAS, and 0.000015 mg Cr\+6\/dscm for IC/PCR with 
preconcentration.

    Note: It is recommended that the concentration of Cr in the 
analytical solutions be at least five times the analytical detection 
limit to optimize sensitivity in the analyses. Using this guideline and 
the same assumptions for impinger sample volume, stack gas sample 
volume, and the digestion concentration factor for the GFAAS analysis 
(500 mL,1.7 dscm, and 1/2, respectively), the recommended minimum stack 
concentrations for optimum sensitivity are 0.0068 mg Cr/dscm to 0.0103 
mg Cr/dscm for ICP, 0.00074 mg Cr/dscm for GFAAS, and 0.000074 mg 
Cr\+6\/dscm for IC/PCR with preconcentration. If required, the in-stack 
detection limits can be improved by either increasing the stack gas 
sample volume, further reducing the volume of the digested sample for 
GFAAS, improving the analytical detection limits, or any combination of 
the three.

    13.3 Precision.
    13.3.1 The following precision data have been reported for the three 
analytical methods. In each case, when the sampling precision is 
combined with the reported analytical precision, the resulting overall 
precision may decrease.
    13.3.2 Bias data is also reported for GFAAS.
    13.4 ICP Precision.
    13.4.1 As reported in Method 6010B of SW-846 (Reference 1), in an 
EPA round-robin Phase 1 study, seven laboratories applied the ICP 
technique to acid/distilled water matrices that had been spiked with 
various metal concentrates. For true values of 10, 50, and 150 [mu]g Cr/
L; the mean reported values were 10, 50, and 149 [mu]g Cr/L; and the 
mean percent relative standard deviations were 18, 3.3, and 3.8 percent, 
respectively.
    13.4.2 In another multi laboratory study cited in Method 6010B, a 
mean relative standard of 8.2 percent was reported for an aqueous sample 
concentration of approximately 3750 [mu]g Cr/L.
    13.5 GFAAS Precision. As reported in Method 7191 of SW-846 
(Reference 1), in a single laboratory (EMSL), using Cincinnati, Ohio tap 
water spiked at concentrations of 19, 48, and 77 [mu]g Cr/L, the 
standard deviations were 0.1, 0.2, and 0.8, respectively. 
Recoveries at these levels were 97 percent, 101 percent, and 102 
percent, respectively.
    13.6 IC/PCR Precision. As reported in Methods 0061 and 7199 of SW-
846 (Reference 1), the precision of IC/PCR with sample preconcentration 
is 5 to 10 percent. The overall precision for sewage sludge incinerators 
emitting 120 ng/dscm of Cr+\6\ and 3.5 [mu]g/dscm of total Cr 
was 25 percent and 9 percent, respectively; and for hazardous waste 
incinerators emitting 300 ng/dscm of C+\6\ the precision was 
20 percent.

                        14.0 Pollution Prevention

    14.1 The only materials used in this method that could be considered 
pollutants are the chromium standards used for instrument calibration 
and acids used in the cleaning of the collection and measurement 
containers/labware, in the preparation of standards, and in the acid 
digestion of samples. Both reagents can be stored in the same waste 
container.
    14.2 Cleaning solutions containing acids should be prepared in 
volumes consistent with use to minimize the disposal of excessive 
volumes of acid.
    14.3 To the extent possible, the containers/vessels used to collect 
and prepare samples should be cleaned and reused to minimize the 
generation of solid waste.

                          15.0 Waste Management

    15.1 It is the responsibility of the laboratory and the sampling 
team to comply with all federal, state, and local regulations governing 
waste management, particularly the discharge regulations, hazardous 
waste identification rules, and land disposal restrictions; and to 
protect the air, water, and land by minimizing and controlling all 
releases from field operations.
    15.2 For further information on waste management, consult The Waste 
Management Manual for Laboratory Personnel and Less is Better--
Laboratory Chemical Management for Waste Reduction, available from the 
American Chemical Society's Department of Government Relations and 
Science Policy, 1155 16th Street NW, Washington, DC 20036.

                             16.0 References

    1. ``Test Methods for Evaluating Solid Waste, Physical/Chemical 
Methods, SW-846, Third Edition,'' as amended by Updates I, II, IIA, IIB, 
and III. Document No. 955-001-000001. Available from Superintendent of 
Documents, U.S. Government Printing Office, Washington, DC, November 
1986.
    2. Cox, X.B., R.W. Linton, and F.E. Butler. Determination of 
Chromium Speciation in Environmental Particles--A Multi-technique

[[Page 205]]

Study of Ferrochrome Smelter Dust. Accepted for publication in 
Environmental Science and Technology.
    3. Same as Section 17.0 of Method 5, References 2, 3, 4, 5, and 7.
    4. California Air Resources Board, ``Determination of Total Chromium 
and Hexavalent Chromium Emissions from Stationary Sources.'' Method 425, 
September 12, 1990.
    5. The Merck Index. Eleventh Edition. Merck & Co., Inc., 1989.
    6. Walpole, R.E., and R.H. Myers. ``Probability and Statistics for 
Scientists and Engineering.'' 3rd Edition. MacMillan Publishing Co., 
NewYork, N.Y., 1985.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.577


[[Page 206]]


[GRAPHIC] [TIFF OMITTED] TR17OC00.578

  Method 306A--Determination of Chromium Emissions From Decorative and 
     Hard Chromium Electroplating and Chromium Anodizing Operations

    Note: This method does not include all of the specifications (e.g., 
equipment and supplies) and procedures (e.g., sampling and analytical) 
essential to its performance. Some material is incorporated by reference 
from other methods in 40 CFR Part 60, Appendix A and in this part. 
Therefore, to obtain reliable results, persons using this method should 
have a thorough knowledge of at least Methods 5 and 306.

                        1.0 Scope and Application

    1.1 Analyte. Chromium. CAS Number (7440-47-3).
    1.2 Applicability.
    1.2.1 This method applies to the determination of chromium (Cr) in 
emissions

[[Page 207]]

from decorative and hard chromium electroplating facilities, chromium 
anodizing operations, and continuous chromium plating at iron and steel 
facilities. The method is less expensive and less complex to conduct 
than Method 306. Correctly applied, the precision and bias of the sample 
results should be comparable to those obtained with the isokinetic 
Method 306. This method is applicable for the determination of air 
emissions under nominal ambient moisture, temperature, and pressure 
conditions.
    1.2.2 The method is also applicable to electroplating and anodizing 
sources controlled by wet scrubbers.
    1.3 Data Quality Objectives.
    1.3.1 Pretest Protocol.
    1.3.1.1 The pretest protocol should define and address the test data 
quality objectives (DQOs), with all assumptions, that will be required 
by the end user (enforcement authority); what data are needed? why are 
the data needed? how will data be used? what are method detection 
limits? and what are estimated target analyte levels for the following 
test parameters.
    1.3.1.1.1 Estimated source concentration for total chromium and/or 
Cr\+6\.
    1.3.1.1.2 Estimated minimum sampling time and/or volume required to 
meet method detection limit requirements (Appendix B 40 CFR Part 136) 
for measurement of total chromium and/or Cr\+6\.
    1.3.1.1.3 Demonstrate that planned sampling parameters will meet 
DQOs. The protocol must demonstrate that the planned sampling parameters 
calculated by the tester will meet the needs of the source and the 
enforcement authority.
    1.3.1.2 The pre-test protocol should include information on 
equipment, logistics, personnel, process operation, and other resources 
necessary for an efficient and coordinated performance test.
    1.3.1.3 At a minimum, the pre-test protocol should identify and be 
approved by the source, the tester, the analytical laboratory, and the 
regulatory enforcement authority. The tester should not proceed with the 
compliance testing before obtaining approval from the enforcement 
authority.

                          2.0 Summary of Method

    2.1 Sampling.
    2.1.1 An emission sample is extracted from the source at a constant 
sampling rate determined by a critical orifice and collected in a 
sampling train composed of a probe and impingers. The proportional 
sampling time at the cross sectional traverse points is varied according 
to the stack gas velocity at each point. The total sample time must be 
at least two hours.
    2.1.2 The chromium emission concentration is determined by the same 
analytical procedures described in Method 306: inductively-coupled 
plasma emission spectrometry (ICP), graphite furnace atomic absorption 
spectrometry (GFAAS), or ion chromatography with a post-column reactor 
(IC/PCR).
    2.1.2.1 Total chromium samples with high chromium concentrations 
(=35 [mu]g/L) may be analyzed using inductively coupled 
plasma emission spectrometry (ICP) at 267.72 nm.
    Note: The ICP analysis is applicable for this method only when the 
solution analyzed has a Cr concentration greater than or equal to 35 
[mu]g/L or five times the method detection limit as determined according 
to Appendix B in 40 CFR Part 136.
    2.1.2.2 Alternatively, when lower total chromium concentrations (<35 
[mu]g/L) are encountered, a portion of the alkaline sample solution may 
be digested with nitric acid and analyzed by graphite furnace atomic 
absorption spectroscopy (GFAAS) at 357.9 nm.
    2.1.2.3 If it is desirable to determine hexavalent chromium (Cr\+6\) 
emissions, the samples may be analyzed using an ion chromatograph 
equipped with a post-column reactor (IC/PCR) and a visible wavelength 
detector. To increase sensitivity for trace levels of Cr\+6\, a 
preconcentration system may be used in conjunction with the IC/PCR.

                             3.0 Definitions

    3.1 Total Chromium--measured chromium content that includes both 
major chromium oxidation states (Cr+3, Cr+6).
    3.2 May--Implies an optional operation.
    3.3 Digestion--The analytical operation involving the complete (or 
nearly complete) dissolution of the sample in order to ensure the 
complete solubilization of the element (analyte) to be measured.
    3.4 Interferences--Physical, chemical, or spectral phenomena that 
may produce a high or low bias in the analytical result.
    3.5 Analytical System--All components of the analytical process 
including the sample digestion and measurement apparatus.
    3.6 Sample Recovery--The quantitative transfer of sample from the 
collection apparatus to the sample preparation (digestion, etc.) 
apparatus. This term should not be confused with analytical recovery.

                            4.0 Interferences

    4.1 Same as in Method 306, Section 4.0.

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method does not purport to address 
all of the safety issues associated with its use. It is the 
responsibility of the user to establish appropriate safety and health 
practices and to determine the applicability of regulatory limitations 
prior to performing this test method.

[[Page 208]]

    5.2 Chromium and some chromium compounds have been listed as 
carcinogens although Chromium (III) compounds show little or no 
toxicity. Chromium is a skin and respiratory irritant.

                       6.0 Equipment and Supplies

    Note: Mention of trade names or specific products does not 
constitute endorsement by the Environmental Protection Agency.
    6.1 Sampling Train. A schematic of the sampling train is shown in 
Figure 306A-1. The individual components of the train are available 
commercially, however, some fabrication and assembly are required.
    6.1.1 Probe Nozzle/Tubing and Sheath.
    6.1.1.1 Use approximately 6.4-mm (\1/4\-in.) inside diameter (ID) 
glass or rigid plastic tubing approximately 20 cm (8 in.) in length with 
a short 90 degree bend at one end to form the sampling nozzle. Grind a 
slight taper on the nozzle end before making the bend. Attach the nozzle 
to flexible tubing of sufficient length to enable collection of a sample 
from the stack.
    6.1.1.2 Use a straight piece of larger diameter rigid tubing (such 
as metal conduit or plastic water pipe) to form a sheath that begins 
about 2.5 cm (1 in.) from the 90 [deg] bend on the nozzle and encases 
and supports the flexible tubing.
    6.1.2 Type S Pitot Tube. Same as Method 2, Section 6.1 (40 CFR Part 
60, Appendix A).
    6.1.3 Temperature Sensor.
    6.1.3.1 A thermocouple, liquid-filled bulb thermometer, bimetallic 
thermometer, mercury-in-glass thermometer, or other sensor capable of 
measuring temperature to within 1.5 percent of the minimum absolute 
stack temperature.
    6.1.3.2 The temperature sensor shall either be positioned near the 
center of the stack, or be attached to the pitot tube as directed in 
Section 6.3 of Method 2.
    6.1.4 Sample Train Connectors.
    6.1.4.1 Use thick wall flexible plastic tubing (polyethylene, 
polypropylene, or polyvinyl chloride)  6.4-mm (\1/4\-in.) to 9.5-mm (\3/
8\-in.) ID to connect the train components.
    6.1.4.2 A combination of rigid plastic tubing and thin wall flexible 
tubing may be used as long as tubing walls do not collapse when leak-
checking the train. Metal tubing cannot be used.
    6.1.5 Impingers. Three, one-quart capacity, glass canning jars with 
vacuum seal lids, or three Greenburg-Smith (GS) design impingers 
connected in series, or equivalent, may be used.
    6.1.5.1 One-quart glass canning jar. Three separate jar containers 
are required: (1) the first jar contains the absorbing solution; (2) the 
second is empty and is used to collect any reagent carried over from the 
first container; and (3) the third contains the desiccant drying agent.
    6.1.5.2 Canning Jar Connectors. The jar containers are connected by 
leak-tight inlet and outlet tubes installed in the lids of each 
container for assembly with the train. The tubes may be made of  6.4 mm 
(\1/4\-in.) ID glass or rigid plastic tubing. For the inlet tube of the 
first impinger, heat the glass or plastic tubing and draw until the 
tubing separates. Fabricate the necked tip to form an orifice tip that 
is approximately 2.4 mm (\3/32\-in.) ID.
    6.1.5.2.1 When assembling the first container, place the orifice tip 
end of the tube approximately 4.8 mm (\3/16\-in.) above the inside 
bottom of the jar.
    6.1.5.2.2 For the second container, the inlet tube need not be drawn 
and sized, but the tip should be approximately 25 mm (1 in.) above the 
bottom of the jar.
    6.1.5.2.3 The inlet tube of the third container should extend to 
approximately 12.7 mm (\1/2\-in.) above the bottom of the jar.
    6.1.5.2.4 Extend the outlet tube for each container approximately 50 
mm (2 in.) above the jar lid and downward through the lid, approximately 
12.7 mm (\1/2\-in.) beneath the bottom of the lid.
    6.1.5.3 Greenburg-Smith Impingers. Three separate impingers of the 
Greenburg-Smith (GS) design as described in Section 6.0 of Method 5 are 
required. The first GS impinger shall have a standard tip (orifice/
plate), and the second and third GS impingers shall be modified by 
replacing the orifice/plate tube with a 13 mm (\1/2\-in.) ID glass tube, 
having an unrestricted opening located 13 mm (\1/2\-in.) from the bottom 
of the outer flask.
    6.1.5.4 Greenburg-Smith Connectors. The GS impingers shall be 
connected by leak-free ground glass ``U'' tube connectors or by leak-
free non-contaminating flexible tubing. The first impinger shall contain 
the absorbing solution, the second is empty and the third contains the 
desiccant drying agent.
    6.1.6 Manometer. Inclined/vertical type, or equivalent device, as 
described in Section 6.2 of Method 2 (40 CFR Part 60, Appendix A).
    6.1.7 Critical Orifice. The critical orifice is a small restriction 
in the sample line that is located upstream of the vacuum pump. The 
orifice produces a constant sampling flow rate that is approximately 
0.021 cubic meters per minute (m3/min) or 0.75 cubic feet per minute 
(cfm).
    6.1.7.1 The critical orifice can be constructed by sealing a 2.4-mm 
(\3/32\-in.) ID brass tube approximately 14.3 mm (\9/16\-in.) in length 
inside a second brass tube that is approximately 8 mm (\5/16\-in.) ID 
and 14.3-mm (\9/16\-in.) in length .
    6.1.7.2 Materials other than brass can be used to construct the 
critical orifice as long as the flow through the sampling train can be 
maintained at approximately 0.021 cubic meter per minute (0.75) cfm.
    6.1.8 Connecting Hardware. Standard pipe and fittings, 9.5-mm (\3/
8\-in.), 6.4-mm (\1/4\-in.)

[[Page 209]]

or 3.2-mm (\1/8\-in.) ID, may be used to assemble the vacuum pump, dry 
gas meter and other sampling train components.
    6.1.9 Vacuum Gauge. Capable of measuring approximately 760 mm 
Hg (30 in. Hg) vacuum in 25.4 mm HG (1 
in. Hg) increments. Locate vacuum gauge between the critical 
orifice and the vacuum pump.
    6.1.10 Pump Oiler. A glass oil reservoir with a wick mounted at the 
vacuum pump inlet that lubricates the pump vanes. The oiler should be an 
in-line type and not vented to the atmosphere. See EMTIC Guideline 
Document No. GD-041.WPD for additional information.
    6.1.11 Vacuum Pump. Gast Model 0522-V103-G18DX, or equivalent, 
capable of delivering at least 1.5 cfm at 15 in. Hg vacuum.
    6.1.12 Oil Trap/Muffler. An empty glass oil reservoir without wick 
mounted at the pump outlet to control the pump noise and prevent oil 
from reaching the dry gas meter.
    6.1.13 By-pass Fine Adjust Valve (Optional). Needle valve assembly 
6.4-mm (\1/4\-in.), Whitey 1 RF 4-A, or equivalent, that allows for 
adjustment of the train vacuum.
    6.1.13.1 A fine-adjustment valve is positioned in the optional pump 
by-pass system that allows the gas flow to recirculate through the pump. 
This by-pass system allows the tester to control/reduce the maximum 
leak-check vacuum pressure produced by the pump.
    6.1.13.1.1 The tester must conduct the post test leak check at a 
vacuum equal to or greater than the maximum vacuum encountered during 
the sampling run.
    6.1.13.1.2 The pump by-pass assembly is not required, but is 
recommended if the tester intends to leak-check the 306A train at the 
vacuum experienced during a run.
    6.1.14 Dry Gas Meter. An Equimeter Model 110 test meter or, 
equivalent with temperature sensor(s) installed (inlet/outlet) to 
monitor the meter temperature. If only one temperature sensor is 
installed, locate the sensor at the outlet side of the meter. The dry 
gas meter must be capable of measuring the gaseous volume to within 
2% of the true volume.
    Note: The Method 306 sampling train is also commercially available 
and may be used to perform the Method 306A tests. The sampling train may 
be assembled as specified in Method 306A with the sampling rate being 
operated at the delta H@ specified for the calibrated orifice 
located in the meter box. The Method 306 train is then operated as 
described in Method 306A.
    6.2 Barometer. Mercury aneroid barometer, or other barometer 
equivalent, capable of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
    6.2.1 A preliminary check of the barometer shall be made against a 
mercury-in-glass reference barometer or its equivalent.
    6.2.2 Tester may elect to obtain the absolute barometric pressure 
from a nearby National Weather Service station.
    6.2.2.1 The station value (which is the absolute barometric 
pressure) must be adjusted for elevation differences between the weather 
station and the sampling location. Either subtract 2.5 mm Hg 
(0.1 in. Hg) from the station value per 30 m (100 ft) of 
elevation increase or add the same for an elevation decrease.
    6.2.2.2 If the field barometer cannot be adjusted to agree within 
0.1 in. Hg of the reference barometric, repair or discard the 
unit. The barometer pressure measurement shall be recorded on the 
sampling data sheet.
    6.3 Sample Recovery. Same as Method 5, Section 6.2 (40 CFR Part 60, 
Appendix A), with the following exceptions:
    6.3.1 Probe-Liner and Probe-Nozzle Brushes. Brushes are not 
necessary for sample recovery. If a probe brush is used, it must be non-
metallic.
    6.3.2 Wash Bottles. Polyethylene wash bottle, for sample recovery 
absorbing solution.
    6.3.3 Sample Recovery Solution. Use 0.1 N NaOH or 0.1 N 
NaHCO3, whichever is used as the impinger absorbing solution, 
to replace the acetone.
    6.3.4 Sample Storage Containers.
    6.3.4.1 Glass Canning Jar. The first canning jar container of the 
sampling train may serve as the sample shipping container. A new lid and 
sealing plastic wrap shall be substituted for the container lid 
assembly.
    6.3.4.2 Polyethylene or Glass Containers. Transfer the Greenburg-
Smith impinger contents to precleaned polyethylene or glass containers. 
The samples shall be stored and shipped in 250-mL, 500-mL or 1000-mL 
polyethylene or glass containers with leak-free, non metal screw caps.
    6.3.5 pH Indicator Strip, for Cr +6 Samples. pH indicator 
strips, or equivalent, capable of determining the pH of solutions 
between the range of 7 and 12, at 0.5 pH increments.
    6.3.6 Plastic Storage Containers. Air tight containers to store 
silica gel.
    6.4 Analysis. Same as Method 306, Section 6.3.

                       7.0 Reagents and Standards.

    Note: Unless otherwise indicated, all reagents shall conform to the 
specifications established by the Committee on Analytical Reagents of 
the American Chemical Society (ACS reagent grade). Where such 
specifications are not available, use the best available grade. It is 
recommended, but not required, that reagents be checked by the 
appropriate analysis prior to field use to assure that contamination is 
below the analytical detection limit for the ICP or GFAAS total chromium 
analysis; and that contamination is below the analytical detection limit 
for

[[Page 210]]

Cr+6 using IC/PCR for direct injection or, if selected, 
preconcentration.
    7.1 Sampling.
    7.1.1 Water. Reagent water that conforms to ASTM Specification D1193 
Type II (incorporated by reference see Sec. 63.14). All references to 
water in the method refer to reagent water unless otherwise specified. 
It is recommended that water blanks be checked prior to preparing the 
sampling reagents to ensure that the Cr content is less than three (3) 
times the anticipated detection limit of the analytical method.
    7.1.2 Sodium Hydroxide (NaOH) Absorbing Solution, 0.1 N. Dissolve 
4.0 g of sodium hydroxide in 1 liter of water to obtain a pH of 
approximately 8.5.
    7.1.3 Sodium Bicarbonate (NaHCO3) Absorbing Solution, 0.1 
N. Dissolve approximately 8.5 g of sodium bicarbonate in 1 liter of 
water to obtain a pH of approximately 8.3.
    7.1.4 Chromium Contamination.
    7.1.4.1 The absorbing solution shall not exceed the QC criteria 
noted in Method 306, Section 7.1.1 (<=3 times the instrument detection 
limit).
    7.1.4.2 When the Cr+6 content in the field samples 
exceeds the blank concentration by at least a factor of ten (10), 
Cr+\6\ blank levels <=10 times the detection limit will be 
allowed.

    Note: At sources with high concentrations of acids and/or 
SO2, the concentration of NaOH or NaHCO3 should be 
=0.5 N to insure that the pH of the solution remains at or 
above 8.5 for NaOH and 8.0 for NaHCO3 during and after 
sampling.

    7.1.3 Desiccant. Silica Gel, 6-16 mesh, indicating type. 
Alternatively, other types of desiccants may be used, subject to the 
approval of the Administrator.
    7.2 Sample Recovery. Same as Method 306, Section 7.2.
    7.3 Sample Preparation and Analysis. Same as Method 306, Section 
7.3.
    7.4 Glassware Cleaning Reagents. Same as Method 306, Section 7.4.
    7.5 Quality Assurance Audit Samples.
    7.5.1 It is recommended, but not required, that a performance audit 
sample be analyzed in conjunction with the field samples. The audit 
sample should be in a suitable sample matrix at a concentration similar 
to the actual field samples.
    7.5.2 When making compliance determinations, and upon availability, 
audit samples may be obtained from the appropriate EPA regional Office 
or from the responsible enforcement authority and analyzed in 
conjunction with the field samples.

    Note: The responsible enforcement authority should be notified at 
least 30 days prior to the test date to allow sufficient time for the 
audit sample to be delivered.

 8.0 Sample Collection, Recovery, Preservation, Holding Times, Storage, 
                              and Transport

    Note: Prior to sample collection, consideration should be given as 
to the type of analysis (Cr+6 or total Cr) that will be 
performed. Deciding which analysis will be performed will enable the 
tester to determine which appropriate sample recovery and storage 
procedures will be required to process the sample.

    8.1 Sample Collection.
    8.1.1 Pretest Preparation.
    8.1.1.1 Selection of Measurement Site. Locate the sampling ports as 
specified in Section 11.0 of Method 1 (40 CFR Part 60, Appendix A).
    8.1.1.2 Location of Traverse Points.
    8.1.1.2.1 Locate the traverse points as specified in Section 11.0 of 
Method 1 (40 CFR Part 60, Appendix A). Use a total of 24 sampling points 
for round ducts and 24 or 25 points for rectangular ducts. Mark the 
pitot and sampling probe to identify the sample traversing points.
    8.1.1.2.2 For round ducts less than 12 inches in diameter, use a 
total of 16 points.
    8.1.1.3 Velocity Pressure Traverse. Perform an initial velocity 
traverse before obtaining samples. The Figure 306A-2 data sheet may be 
used to record velocity traverse data.
    8.1.1.3.1 To demonstrate that the flow rate is constant over several 
days of testing, perform complete traverses at the beginning and end of 
each day's test effort, and calculate the deviation of the flow rate for 
each daily period. The beginning and end flow rates are considered 
constant if the deviation does not exceed 10 percent. If the flow rate 
exceeds the 10 percent criteria, either correct the inconsistent flow 
rate problem, or obtain the Administrator's approval for the test 
results.
    8.1.1.3.2 Perform traverses as specified in Section 8.0 of Method 2, 
but record only the [Delta]p (velocity pressure) values for each 
sampling point. If a mass emission rate is desired, stack velocity 
pressures shall be recorded before and after each test, and an average 
stack velocity pressure determined for the testing period.
    8.1.1.4 Verification of Absence of Cyclonic Flow. Check for cyclonic 
flow during the initial traverse to verify that it does not exist. 
Perform the cyclonic flow check as specified in Section 11.4 of Method 1 
(40 CFR Part 60, Appendix A).
    8.1.1.4.1 If cyclonic flow is present, verify that the absolute 
average angle of the tangential flow does not exceed 20 degrees. If the 
average value exceeds 20 degrees at the sampling location, the flow 
condition in the stack is unacceptable for testing.

[[Page 211]]

    8.1.1.4.2 Alternative procedures, subject to approval of the 
Administrator, e.g., installing straightening vanes to eliminate the 
cyclonic flow, must be implemented prior to conducting the testing.
    8.1.1.5 Stack Gas Moisture Measurements. Not required. Measuring the 
moisture content is optional when a mass emission rate is to be 
calculated.
    8.1.1.5.1 The tester may elect to either measure the actual stack 
gas moisture during the sampling run or utilize a nominal moisture value 
of 2 percent.
    8.1.1.5.2 For additional information on determining sampling train 
moisture, please refer to Method 4 (40 CFR Part 60, Appendix A).
    8.1.1.6 Stack Temperature Measurements. If a mass emission rate is 
to be calculated, a temperature sensor must be placed either near the 
center of the stack, or attached to the pitot tube as described in 
Section 8.3 of Method 2. Stack temperature measurements, shall be 
recorded before and after each test, and an average stack temperature 
determined for the testing period.
    8.1.1.7 Point Sampling Times. Since the sampling rate of the train 
(0.75 cfm) is maintained constant by the critical orifice, it is 
necessary to calculate specific sampling times for each traverse point 
in order to obtain a proportional sample.
    8.1.1.7.1 If the sampling period (3 runs) is to be completed in a 
single day, the point sampling times shall be calculated only once.
    8.1.1.7.2 If the sampling period is to occur over several days, the 
sampling times must be calculated daily using the initial velocity 
pressure data recorded for that day. Determine the average of the 
[Delta]p values obtained during the velocity traverse (Figure 306A-2).
    8.1.1.7.3 If the stack diameter is less than 12 inches, use 7.5 
minutes in place of 5 minutes in the equation and 16 sampling points 
instead of 24 or 25 points. Calculate the sampling times for each 
traverse point using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.579

Where:
n = Sampling point number.
[Delta]p = Average pressure differential across pitot tube, mm 
H2O (in. H2O).
[Delta]Pavg = Average of [Delta]p values, mm H2O 
(in. H2O).

    Note: Convert the decimal fractions for minutes to seconds.
    8.1.1.8 Pretest Preparation. It is recommended, but not required, 
that all items which will be in contact with the sample be cleaned prior 
to performing the testing to avoid possible sample contamination 
(positive chromium bias). These items include, but are not limited to: 
Sampling probe, connecting tubing, impingers, and jar containers.
    8.1.1.8.1 Sample train components should be: (1) Rinsed with hot tap 
water; (2) washed with hot soapy water; (3) rinsed with tap water; (4) 
rinsed with reagent water; (5) soaked in a 10 percent (v/v) nitric acid 
solution for at least four hours; and (6) rinsed throughly with reagent 
water before use.
    8.1.1.8.2 At a minimum, the tester should, rinse the probe, 
connecting tubing, and first and second impingers twice with either 0.1 
N sodium hydroxide (NaOH) or 0.1 N sodium bicarbonate 
(NaHCO3) and discard the rinse solution.
    8.1.1.8.3 If separate sample shipping containers are to be used, 
these also should be precleaned using the specified cleaning procedures.
    8.1.1.9 Preparation of Sampling Train. Assemble the sampling train 
as shown in Figure 306A-1. Secure the nozzle-liner assembly to the outer 
sheath to prevent movement when sampling.
    8.1.1.9.1 Place 250 mL of 0.1 N NaOH or 0.1 N NaHCO3 
absorbing solution into the first jar container or impinger. The second 
jar/impinger is to remain empty. Place 6 to 16 mesh indicating silica 
gel, or equivalent desiccant into the third jar/impinger until the 
container is half full ( 300 to 400 g).
    8.1.1.9.2 Place a small cotton ball in the outlet exit tube of the 
third jar to collect small silica gel particles that may dislodge and 
impair the pump and/or gas meter.
    8.1.1.10 Pretest Leak-Check. A pretest leak-check is recommended, 
but not required. If the tester opts to conduct the pretest leak-check, 
the following procedures shall be performed: (1) Place the jar/impinger 
containers into an ice bath and wait 10 minutes for the ice to cool the 
containers before performing the leak check and/or start sampling; (2) 
to perform the leak check, seal the nozzle using a piece of clear 
plastic wrap placed over the end of a finger and switch on the pump; and 
(3) the train system leak rate should not exceed 0.02 cfm at a vacuum of 
380 mm Hg (15 in. Hg) or greater. If the leak rate

[[Page 212]]

does exceed the 0.02 cfm requirement, identify and repair the leak area 
and perform the leak check again.

    Note: Use caution when releasing the vacuum following the leak 
check. Always allow air to slowly flow through the nozzle end of the 
train system while the pump is still operating. Switching off the pump 
with vacuum on the system may result in the silica gel being pulled into 
the second jar container.
    8.1.1.11 Leak-Checks During Sample Run. If, during the sampling run, 
a component (e.g., jar container) exchange becomes necessary, a leak-
check shall be conducted immediately before the component exchange is 
made. The leak-check shall be performed according to the procedure 
outlined in Section 8.1.1.10 of this method. If the leakage rate is 
found to be <= 0.02 cfm at the maximum operating vacuum, the results are 
acceptable. If, however, a higher leak rate is obtained, either record 
the leakage rate and correct the sample volume as shown in Section 12.3 
of Method 5 or void the sample and initiate a replacement run. Following 
the component change, leak-checks are optional, but are recommended as 
are the pretest leak-checks.
    8.1.1.12 Post Test Leak Check. Remove the probe assembly and 
flexible tubing from the first jar/impinger container. Seal the inlet 
tube of the first container using clear plastic wrap and switch on the 
pump. The vacuum in the line between the pump and the critical orifice 
must be =15 in. Hg. Record the vacuum gauge measurement along 
with the leak rate observed on the train system.
    8.1.1.12.1 If the leak rate does not exceed 0.02 cfm, the results 
are acceptable and no sample volume correction is necessary.
    8.1.1.12.2 If, however, a higher leak rate is obtained 
(0.02 cfm), the tester shall either record the leakage rate 
and correct the sample volume as shown in Section 12.3 of Method 5, or 
void the sampling run and initiate a replacement run. After completing 
the leak-check, slowly release the vacuum at the first container while 
the pump is still operating. Afterwards, switch-off the pump.
    8.1.2 Sample Train Operation.
    8.1.2.1 Data Recording. Record all pertinent process and sampling 
data on the data sheet (see Figure 306A-3). Ensure that the process 
operation is suitable for sample collection.
    8.1.2.2 Starting the Test. Place the probe/nozzle into the duct at 
the first sampling point and switch on the pump. Start the sampling 
using the time interval calculated for the first point. When the first 
point sampling time has been completed, move to the second point and 
continue to sample for the time interval calculated for that point; 
sample each point on the traverse in this manner. Maintain ice around 
the sample containers during the run.
    8.1.2.3 Critical Flow. The sample line between the critical orifice 
and the pump must operate at a vacuum of = 380 mm Hg 
(=15 in. Hg) in order for critical flow to be maintained. 
This vacuum must be monitored and documented using the vacuum gauge 
located between the critical orifice and the pump.

    Note: Theoretically, critical flow for air occurs when the ratio of 
the orifice outlet absolute pressure to the orifice inlet absolute 
pressure is less than a factor of 0.53. This means that the system 
vacuum should be at least = 356 mm Hg (= 14 in. 
Hg) at sea level and  305 mm Hg ( 12 in. Hg) at higher elevations.

    8.1.2.4 Completion of Test.
    8.1.2.4.1 Circular Stacks. Complete the first port traverse and 
switch off the pump. Testers may opt to perform a leak-check between the 
port changes to verify the leak rate however, this is not mandatory. 
Move the sampling train to the next sampling port and repeat the 
sequence. Be sure to record the final dry gas meter reading after 
completing the test run. After performing the post test leak check, 
disconnect the jar/impinger containers from the pump and meter assembly 
and transport the probe, connecting tubing, and containers to the sample 
recovery area.
    8.1.2.4.2 Rectangle Stacks. Complete each port traverse as per the 
instructions provided in 8.1.2.4.1.

    Note: If an approximate mass emission rate is to be calculated, 
measure and record the stack velocity pressure and temperature before 
and after the test run.

    8.2 Sample Recovery. After the train has been transferred to the 
sample recovery area, disconnect the tubing that connects the jar/
impingers. The tester shall select either the total Cr or 
Cr+\6\ sample recovery option. Samples to be analyzed for 
both total Cr and Cr+\6\ shall be recovered using the 
Cr+\6\ sample option (Section 8.2.2).

    Note: Collect a reagent blank sample for each of the total Cr or the 
Cr+\6\ analytical options. If both analyses (Cr and 
Cr+\6\) are to be conducted on the samples, collect separate 
reagent blanks for each analysis.

    8.2.1 Total Cr Sample Option.
    8.2.1.1 Shipping Container No. 1. The first jar container may either 
be used to store and transport the sample, or if GS impingers are used, 
samples may be stored and shipped in precleaned 250-mL, 500-mL or 1000-
mL polyethylene or glass bottles with leak-free, non-metal screw caps.
    8.2.1.1.1 Unscrew the lid from the first jar/impinger container.
    8.2.1.1.2 Lift the inner tube assembly almost out of the container, 
and using the wash bottle containing fresh absorbing solution, rinse the 
outside of the tube that was immersed in the container solution; rinse

[[Page 213]]

the inside of the tube as well, by rinsing twice from the top of the 
tube down through the inner tube into the container.
    8.2.1.2 Recover the contents of the second jar/impinger container by 
removing the lid and pouring any contents into the first shipping 
container.
    8.2.1.2.1 Rinse twice, using fresh absorbing solution, the inner 
walls of the second container including the inside and outside of the 
inner tube.
    8.2.1.2.2 Rinse the connecting tubing between the first and second 
sample containers with absorbing solution and place the rinses into the 
first container.
    8.2.1.3 Position the nozzle, probe and connecting plastic tubing in 
a vertical position so that the tubing forms a ``U''.
    8.2.1.3.1 Using the wash bottle, partially fill the tubing with 
fresh absorbing solution. Raise and lower the end of the plastic tubing 
several times to allow the solution to contact the internal surfaces. Do 
not allow the solution to overflow or part of the sample will be lost. 
Place the nozzle end of the probe over the mouth of the first container 
and elevate the plastic tubing so that the solution flows into the 
sample container.
    8.2.1.3.2 Repeat the probe/tubing sample recovery procedure but 
allow the solution to flow out the opposite end of the plastic tubing 
into the sample container. Repeat the entire sample recovery procedure 
once again.
    8.2.1.4 Use approximately 200 to 300 mL of the 0.1 N NaOH or 0.1 N 
NaHCO3 absorbing solution during the rinsing of the probe 
nozzle, probe liner, sample containers, and connecting tubing.
    8.2.1.5 Place a piece of clear plastic wrap over the mouth of the 
sample jar to seal the shipping container. Use a standard lid and band 
assembly to seal and secure the sample in the jar.
    8.2.1.5.1 Label the jar clearly to identify its contents, sample 
number and date.
    8.2.1.5.2 Mark the height of the liquid level on the container to 
identify any losses during shipping and handling.
    8.2.1.5.3 Prepare a chain-of-custody sheet to accompany the sample 
to the laboratory.
    8.2.2 Cr+\6\ Sample Option.
    8.2.2.1 Shipping Container No. 1. The first jar container may either 
be used to store and transport the sample, or if GS impingers are used, 
samples may be stored and shipped in precleaned 250-mL, 500-mL or 1000-
mL polyethylene or glass bottles with leak-free non-metal screw caps.
    8.2.2.1.1 Unscrew and remove the lid from the first jar container.
    8.2.2.1.2 Measure and record the pH of the solution in the first 
container by using a pH indicator strip. The pH of the solution must be 
=8.5 for NaOH and =8.0 for NaHCO3. If 
not, discard the collected sample, increase the concentration of the 
NaOH or NaHCO3 absorbing solution to 0.5 M and collect another air 
emission sample.
    8.2.2.2 After measuring the pH of the first container, follow sample 
recovery procedures described in Sections 8.2.1.1 through 8.2.1.5.

    Note: Since particulate matter is not usually present at chromium 
electroplating and/or chromium anodizing facilities, it is not necessary 
to filter the Cr+\6\ samples unless there is observed 
sediment in the collected solutions. If it is necessary to filter the 
Cr+\6\ solutions, please refer to the EPA Method 0061, 
Determination of Hexavalent Chromium Emissions from Stationary Sources, 
Section 7.4, Sample Preparation in SW-846 (see Reference 5) for 
procedure.

    8.2.3 Silica Gel Container. Observe the color of the indicating 
silica gel to determine if it has been completely spent and make a 
notation of its condition/color on the field data sheet. Do not use 
water or other liquids to remove and transfer the silica gel.
    8.2.4 Total Cr and/or Cr+\6\ Reagent Blank.
    8.2.4.1 Shipping Container No. 2. Place approximately 500 mL of the 
0.1 N NaOH or 0.1 N NaHCO3 absorbing solution in a 
precleaned, labeled sample container and include with the field samples 
for analysis.
    8.3 Sample Preservation, Storage, and Transport.
    8.3.1 Total Cr Option. Samples that are to be analyzed for total Cr 
need not be refrigerated.
    8.3.2 Cr+\6\ Option. Samples that are to be analyzed for 
Cr+\6\ must be shipped and stored at 4 [deg]C (40 [deg]F).

    Note: Allow Cr+\6\ samples to return to ambient 
temperature prior to analysis.

    8.4 Sample Holding Times.
    8.4.1 Total Cr Option. Samples that are to be analyzed for total 
chromium must be analyzed within 60 days of collection.
    8.4.2 Cr+\6\ Option. Samples that are to be analyzed for 
Cr+\6\ must be analyzed within 14 days of collection.

                           9.0 Quality Control

    9.1 Same as Method 306, Section 9.0.

                  10.0 Calibration and Standardization

    Note: Tester shall maintain a performance log of all calibration 
results.

    10.1 Pitot Tube. The Type S pitot tube assembly shall be calibrated 
according to the procedures outlined in Section 10.1 of Method 2.
    10.2 Temperature Sensor. Use the procedure in Section 10.3 of Method 
2 to calibrate the in-stack temperature sensor.
    10.3 Metering System.
    10.3.1 Sample Train Dry Gas Meter Calibration. Calibrations may be 
performed as described in Section 16.2 of Method 5 by either the 
manufacturer, a firm who provides calibration services, or the tester.

[[Page 214]]

    10.3.2 Dry Gas Meter Calibration Coefficient (Ym). The 
meter calibration coefficient (Ym) must be determined prior 
to the initial use of the meter, and following each field test program. 
If the dry gas meter is new, the manufacturer will have specified the 
Ym value for the meter. This Ym value can be used 
as the pretest value for the first test. For subsequent tests, the 
tester must use the Ym value established during the pretest 
calibration.
    10.3.3 Calibration Orifice. The manufacturer may have included a 
calibration orifice and a summary spreadsheet with the meter that may be 
used for calibration purposes. The spreadsheet will provide data 
necessary to determine the calibration for the orifice and meter 
(standard cubic feet volume, sample time, etc.). These data were 
produced when the initial Ym value was determined for the 
meter.
    10.3.4 Ym Meter Value Verification or Meter Calibration.
    10.3.4.1 The Ym meter value may be determined by 
replacing the sampling train critical orifice with the calibration 
orifice. Replace the critical orifice assembly by installing the 
calibration orifice in the same location. The inlet side of the 
calibration orifice is to be left open to the atmosphere and is not to 
be reconnected to the sample train during the calibration procedure.
    10.3.4.2 If the vacuum pump is cold, switch on the pump and allow it 
to operate (become warm) for several minutes prior to starting the 
calibration. After stopping the pump, record the initial dry gas meter 
volume and meter temperature.
    10.3.4.3 Perform the calibration for the number of minutes specified 
by the manufacturer's data sheet (usually 5 minutes). Stop the pump and 
record the final dry gas meter volume and temperature. Subtract the 
start volume from the stop volume to obtain the Vm and 
average the meter temperatures (tm).
    10.3.5 Ym Value Calculation. Ym is the 
calculated value for the dry gas meter. Calculate Ym using 
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.580

Where:

Pbar = Barometric pressure at meter, mm Hg, (in. Hg).
Pstd = Standard absolute pressure,
Metric = 760 mm Hg.
English = 29.92 in. Hg.
tm = Average dry gas meter temperature, [deg]C, ( [deg]F).
Tm = Absolute average dry gas meter temperature,
Metric [deg]K = 273 + tm ( [deg]C).
English [deg]R = 460 + tm( [deg]F).
Tstd = Standard absolute temperature,
Metric = 293 [deg]K.
English = 528 [deg]R.
Vm = Volume of gas sample as measured (actual) by dry gas 
meter, dcm,(dcf).
Vm(std),mfg = Volume of gas sample measured by manufacture's 
calibrated orifice and dry gas meter, corrected to standard conditions 
(pressure/temperature) dscm (dscf).
Ym = Dry gas meter calibration factor, (dimensionless).

    10.3.6 Ym Comparison. Compare the Ym value 
provided by the manufacturer (Section 10.3.3) or the pretest 
Ym value to the post test Ym value using the 
following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.581

    10.3.6.1 If this ratio is between 0.95 and 1.05, the designated 
Ym value for the meter is acceptable for use in later 
calculations.
    10.3.6.1.1 If the value is outside the specified range, the test 
series shall either be: 1)

[[Page 215]]

voided and the samples discarded; or 2) calculations for the test series 
shall be conducted using whichever meter coefficient value (i.e., 
manufacturers's/pretest Ym value or post test Ym 
value) produces the lowest sample volume.
    10.3.6.1.2 If the post test dry gas meter Ym value 
differs by more than 5% as compared to the pretest value, either perform 
the calibration again to determine acceptability or return the meter to 
the manufacturer for recalibration.
    10.3.6.1.3 The calibration may also be conducted as specified in 
Section 10.3 or Section 16.0 of Method 5 (40 CFR Part 60, Appendix A), 
except that it is only necessary to check the calibration at one flow 
rate of  0.75 cfm.
    10.3.6.1.4 The calibration of the dry gas meter must be verified 
after each field test program using the same procedures.
    Note: The tester may elect to use the Ym post test value 
for the next pretest Ym value; e.g., Test 1 post test 
Ym value and Test 2 pretest Ym value would be the 
same.

    10.4 Barometer. Calibrate against a mercury barometer that has been 
corrected for temperature and elevation.
    10.5 ICP Spectrometer Calibration. Same as Method 306, Section 10.2.
    10.6 GFAA Spectrometer Calibration. Same as Method 306, Section 
10.3.
    10.7 IC/PCR Calibration. Same as Method 306, Section 10.4.

                       11.0 Analytical Procedures

    Note: The method determines the chromium concentration in [mu]g Cr/
mL. It is important that the analyst measure the volume of the field 
sample prior to analyzing the sample. This will allow for conversion of 
[mu]g Cr/mL to [mu]g Cr/sample.

    11.1 Analysis. Refer to Method 306 for sample preparation and 
analysis procedures.

                   12.0 Data Analysis and Calculations

    12.1 Calculations. Perform the calculations, retaining one extra 
decimal point beyond that of the acquired data. When reporting final 
results, round number of figures consistent with the original data.
    12.2 Nomenclature.

A = Cross-sectional area of stack, m2 (ft2).
Bws = Water vapor in gas stream, proportion by volume, 
dimensionless (assume 2 percent moisture = 0.02).
Cp = Pitot tube coefficient; ``S'' type pitot coefficient 
usually 0.840, dimensionless.
CS = Concentration of Cr in sample solution, [mu]g Cr/mL.
CCr = Concentration of Cr in stack gas, dry basis, corrected 
to standard conditions [mu]g/dscm (gr/dscf).
d = Diameter of stack, m (ft).
D = Digestion factor, dimensionless.
ER = Approximate mass emission rate, mg/hr (lb/hr).
F = Dilution factor, dimensionless.
L = Length of a square or rectangular duct, m (ft).
MCr = Total Cr in each sample, [mu]g (gr).
Ms = Molecular weight of wet stack gas, wet basis, g/g-mole, 
(lb/lb-mole); in a nominal gas stream at 2% moisture the value is 28.62.
Pbar = Barometric pressure at sampling site, mm Hg (in. Hg).
Ps = Absolute stack gas pressure; in this case, usually the 
same value as the barometric pressure, mm Hg (in. Hg).
Pstd = Standard absolute pressure:
Metric = 760 mm Hg.
English = 29.92 in. Hg.
Qstd = Average stack gas volumetric flow, dry, corrected to 
standard conditions, dscm/hr (dscf/hr).
tm = Average dry gas meter temperature, [deg]C ( [deg]F).
Tm = Absolute average dry gas meter temperature:
Metric [deg]K = 273 + tm ( [deg]C).
English [deg]R = 460 + tm( [deg]F).
ts = Average stack temperature, [deg]C ( [deg]F).
Ts = Absolute average stack gas temperature: Metric [deg]K = 
273 + ts ( [deg]C). English [deg]R = 460 + ts( 
[deg]F).
Tstd = Standard absolute temperature: Metric = 293 [deg]K. 
English = 528 [deg]R.
Vad = Volume of sample aliquot after digestion (mL).
Vaf = Volume of sample aliquot after dilution (mL).
Vbd = Volume of sample aliquot submitted to digestion (mL).
Vbf = Volume of sample aliquot before dilution (mL).
Vm = Volume of gas sample as measured (actual, dry) by dry 
gas meter, dcm (dcf).
VmL = Volume of impinger contents plus rinses (mL).
Vm(std) = Volume of gas sample measured by the dry gas meter, 
corrected to standard conditions (temperature/pressure), dscm (dscf).
vs = Stack gas average velocity, calculated by Method 2, 
Equation 2-9, m/sec (ft/sec).
W = Width of a square or rectangular duct, m (ft).
Ym = Dry gas meter calibration factor, (dimensionless).
[Delta]p = Velocity head measured by the Type S pitot tube, cm 
H2O (in. H2O).
[Delta]pavg = Average of [Delta]p values, mm H2O 
(in. H2O).

    12.3 Dilution Factor. The dilution factor is the ratio of the volume 
of sample aliquot after dilution to the volume before dilution. The 
dilution factor is usually calculated by the laboratory. This ratio is 
derived by the following equation:

[[Page 216]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.582

    12.4 Digestion Factor. The digestion factor is the ratio of the 
volume of sample aliquot after digestion to the volume before digestion. 
The digestion factor is usually calculated by the laboratory. This ratio 
is derived by the following equation.
[GRAPHIC] [TIFF OMITTED] TR17OC00.583

    12.5 Total Cr in Sample. Calculate MCr, the total [mu]g 
Cr in each sample, using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.584

    12.6 Dry Gas Volume. Correct the sample volume measured by the dry 
gas meter to standard conditions (20 [deg]C, 760 mm Hg or 68'F, 29.92 
in. Hg) using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.585

Where:

K1 = Metric units--0.3855 [deg]K/mm Hg.
English units--17.64 [deg]R/in. Hg.

    12.7 Cr Emission Concentration (CCr). Calculate 
CCr, the Cr concentration in the stack gas, in [mu]g/dscm 
([mu]g/dscf) on a dry basis, corrected to standard conditions, using the 
following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.586

    Note: To convert [mu]g/dscm ([mu]g/dscf) to mg/dscm (mg/dscf), 
divide by 1000.

    12.8 Stack Gas Velocity.
12.8.1 Kp = Velocity equation constant:
[GRAPHIC] [TIFF OMITTED] TR17OC00.587


[[Page 217]]


[GRAPHIC] [TIFF OMITTED] TR17OC00.588

    12.8.2 Average Stack Gas Velocity.
    [GRAPHIC] [TIFF OMITTED] TR17OC00.589
    
    12.9 Cross sectional area of stack.
    [GRAPHIC] [TIFF OMITTED] TR17OC00.591
    
    12.10 Average Stack Gas Dry Volumetric Flow Rate.
    Note: The emission rate may be based on a nominal stack moisture 
content of 2 percent (0.02). To calculate an emission rate, the tester 
may elect to use either the nominal stack gas moisture value or the 
actual stack gas moisture collected during the sampling run.
    Volumetric Flow Rate Equation:
    [GRAPHIC] [TIFF OMITTED] TR17OC00.592
    
Where:
3600 = Conversion factor, sec/hr.
[GRAPHIC] [TIFF OMITTED] TR17OC00.593

    Note: To convert Qstd from dscm/hr (dscf/hr) to dscm/min 
(dscf/min), divide Qstd by 60.
    12.11 Mass emission rate, mg/hr (lb/hr):
    [GRAPHIC] [TIFF OMITTED] TR17OC00.594
    

[[Page 218]]


[GRAPHIC] [TIFF OMITTED] TR17OC00.595

                         13.0 Method Performance

    13.1 Range. The recommended working range for all of the three 
analytical techniques starts at five times the analytical detection 
limit (see also Method 306, Section 13.2.2). The upper limit of all 
three techniques can be extended indefinitely by appropriate dilution.
    13.2 Sensitivity.
    13.2.1 Analytical Sensitivity. The estimated instrumental detection 
limits listed are provided as a guide for an instrumental limit. The 
actual method detection limits are sample and instrument dependent and 
may vary as the sample matrix varies.
    13.2.1.1 ICP Analytical Sensitivity. The minimum estimated detection 
limits for ICP, as reported in Method 6010A and the recently revised 
Method 6010B of SW-846 (Reference 1), are 7.0 [mu]g Cr/L and 4.7 [mu]g 
Cr/L, respectively.
    13.2.1.2 GFAAS Analytical Sensitivity. The minimum estimated 
detection limit for GFAAS, as reported in Methods 7000A and 7191 of SW-
846 (Reference 1), is 1.0 [mu]g Cr/L.
    13.2.1.3 IC/PCR Analytical Sensitivity. The minimum detection limit 
for IC/PCR with a preconcentrator, as reported in Methods 0061 and 7199 
of SW-846 (Reference 1), is 0.05 [mu]g Cr+6/L.
    13.2.2 In-stack Sensitivity. The in-stack sensitivity depends upon 
the analytical detection limit, the volume of stack gas sampled, and the 
total volume of the impinger absorbing solution plus the rinses. Using 
the analytical detection limits given in Sections 13.2.1.1, 13.2.1.2, 
and 13.2.1.3; a stack gas sample volume of 1.7 dscm; and a total liquid 
sample volume of 500 mL; the corresponding in-stack detection limits are 
0.0014 mg Cr/dscm to 0.0021 mg Cr/dscm for ICP, 0.00029 mg Cr/dscm for 
GFAAS, and 0.000015 mg Cr+36/dscm for IC/PCR with 
preconcentration.
    Note: It is recommended that the concentration of Cr in the 
analytical solutions be at least five times the analytical detection 
limit to optimize sensitivity in the analyses. Using this guideline and 
the same assumptions for impinger sample volume and stack gas sample 
volume (500 mL and 1.7 dscm, respectively), the recommended minimum 
stack concentrations for optimum sensitivity are 0.0068 mg Cr/dscm to 
0.0103 mg Cr/dscm for ICP, 0.0015 mg Cr/dscm for GFAAS, and 0.000074 mg 
Cr+6 dscm for IC/PCR with preconcentration. If required, the 
in-stack detection limits can be improved by either increasing the 
sampling time, the stack gas sample volume, reducing the volume of the 
digested sample for GFAAS, improving the analytical detection limits, or 
any combination of the three.

    13.3 Precision.
    13.3.1 The following precision data have been reported for the three 
analytical methods. In each case, when the sampling precision is 
combined with the reported analytical precision, the resulting overall 
precision may decrease.
    13.3.2 Bias data is also reported for GFAAS.
    13.4 ICP Precision.
    13.4.1 As reported in Method 6010B of SW-846 (Reference 1), in an 
EPA round-robin Phase 1 study, seven laboratories applied the ICP 
technique to acid/distilled water matrices that had been spiked with 
various metal concentrates. For true values of 10, 50, and 150 [mu]g Cr/
L; the mean reported values were 10, 50, and 149 [mu]g Cr/L; and the 
mean percent relative standard deviations were 18, 3.3, and 3.8 percent, 
respectively.
    13.4.2 In another multilaboratory study cited in Method 6010B, a 
mean relative standard of 8.2 percent was reported for an aqueous sample 
concentration of approximately 3750 [mu]g Cr/L.
    13.5 GFAAS Precision. As reported in Method 7191 of SW-846 
(Reference 1), in a single laboratory (EMSL), using Cincinnati, Ohio tap 
water spiked at concentrations of 19, 48, and 77 [mu]g Cr/L, the 
standard deviations were 0.1, 0.2, and 0.8, respectively. 
Recoveries at these levels were 97 percent, 101 percent, and 102 
percent, respectively.
    13.6 IC/PCR Precision. As reported in Methods 0061 and 7199 of SW-
846 (Reference 1), the precision of IC/PCR with sample preconcentration 
is 5 to 10 percent; the overall precision for sewage sludge incinerators 
emitting 120 ng/dscm of Cr+6 and 3.5 [mu]g/dscm of total Cr 
is 25 percent and 9 percent, respectively; and for hazardous waste 
incinerators emitting 300 ng/dscm of Cr+6 the precision is 20 
percent.

                        14.0 Pollution Prevention

    14.1 The only materials used in this method that could be considered 
pollutants are the chromium standards used for instrument calibration 
and acids used in the cleaning of the collection and measurement 
containers/labware, in the preparation of standards, and in the acid 
digestion of samples. Both reagents can be stored in the same waste 
container.
    14.2 Cleaning solutions containing acids should be prepared in 
volumes consistent with use to minimize the disposal of excessive 
volumes of acid.

[[Page 219]]

    14.3 To the extent possible, the containers/vessels used to collect 
and prepare samples should be cleaned and reused to minimize the 
generation of solid waste.

                          15.0 Waste Management

    15.1 It is the responsibility of the laboratory and the sampling 
team to comply with all federal, state, and local regulations governing 
waste management, particularly the discharge regulations, hazardous 
waste identification rules, and land disposal restrictions; and to 
protect the air, water, and land by minimizing and controlling all 
releases from field operations.
    15.2 For further information on waste management, consult The Waste 
Management Manual for Laboratory Personnel and Less is Better-Laboratory 
Chemical Management for Waste Reduction, available from the American 
Chemical Society's Department of Government Relations and Science 
Policy, 1155 16th Street NW, Washington, DC 20036.

                             16.0 References

    1. F.R. Clay, Memo, Impinger Collection Efficiency--Mason Jars vs. 
Greenburg-Smith Impingers, Dec. 1989.
    2. Segall, R.R., W.G. DeWees, F.R. Clay, and J.W. Brown. Development 
of Screening Methods for Use in Chromium Emissions Measurement and 
Regulations Enforcement. In: Proceedings of the 1989 EPA/A&WMA 
International Symposium-Measurement of Toxic and Related Air Pollutants, 
A&WMA Publication VIP-13, EPA Report No. 600/9-89-060, p. 785.
    3. Clay, F.R., Chromium Sampling Method. In: Proceedings of the 1990 
EPA/A&WMA International Symposium-Measurement of Toxic and Related Air 
Pollutants, A&WMA Publication VIP-17, EPA Report No. 600/9-90-026, p. 
576.
    4. Clay, F.R., Proposed Sampling Method 306A for the Determination 
of Hexavalent Chromium Emissions from Electroplating and Anodizing 
Facilities. In: Proceedings of the 1992 EPA/A&WMA International 
Symposium-Measurement of Toxic and Related Air Pollutants, A&WMA 
Publication VIP-25, EPA Report No. 600/R-92/131, p. 209.
    5. Test Methods for Evaluating Solid Waste, Physical/Chemical 
Methods, SW-846, Third Edition as amended by Updates I, II, IIA, IIB, 
and III. Document No. 955-001-000001. Available from Superintendent of 
Documents, U.S. Government Printing Office, Washington, DC, November 
1986.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 220]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.596


[[Page 221]]


[GRAPHIC] [TIFF OMITTED] TR17OC00.597


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[GRAPHIC] [TIFF OMITTED] TR17OC00.598

 Method 306B--Surface Tension Measurement for Tanks Used at Decorative 
        Chromium Electroplating and Chromium Anodizing Facilities

    Note: This method does not include all of the specifications (e.g., 
equipment and supplies) and procedures (e.g., sampling and analytical) 
essential to its performance. Some material is incorporated by reference 
from other methods in 40 CFR Part 60, Appendix A and in this part. 
Therefore, to obtain reliable results, persons using this method should 
have a thorough knowledge of at least Methods 5 and 306.

                        1.0 Scope and Application

    1.1 Analyte. Not applicable.
    1.2 Applicability. This method is applicable to all decorative 
chromium plating and chromium anodizing operations, and continuous 
chromium plating at iron and steel facilities where a wetting agent is 
used in the tank as the primary mechanism for reducing

[[Page 223]]

emissions from the surface of the plating solution.

                          2.0 Summary of Method

    2.1 During an electroplating or anodizing operation, gas bubbles 
generated during the process rise to the surface of the liquid and 
burst. Upon bursting, tiny droplets of chromic acid become entrained in 
ambient air. The addition of a wetting agent to the tank bath reduces 
the surface tension of the liquid and diminishes the formation of these 
droplets.
    2.2 This method determines the surface tension of the bath using a 
stalagmometer or a tensiometer to confirm that there is sufficient 
wetting agent present.

                       3.0 Definitions. [Reserved]

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method may not address all of the 
safety problems associated with its use. It is the responsibility of the 
user to establish appropriate safety and health practices and to 
determine the applicability of regulatory limitations prior to 
performing this test method.

                       6.0 Equipment and Supplies

    6.1 Stalagmometer. Any commercially available stalagmometer or 
equivalent surface tension measuring device may be used to measure the 
surface tension of the plating or anodizing tank liquid.
    6.2 Tensiometer. A tensiometer may be used to measure the surface 
tension of the tank liquid provided the procedures specified in ASTM 
Method D 1331-89, Standard Test Methods for Surface and Interfacial 
Tension of Solutions of Surface Active Agents (incorporated by 
reference--see Sec. 63.14) are followed.

                 7.0 Reagents and Standards. [Reserved]

  8.0 Sample Collection, Sample Recovery, Sample Preservation, Sample 
            Holding Times, Storage, and Transport. [Reserved]

                     9.0 Quality Control. [Reserved]

            10.0 Calibration and Standardization. [Reserved]

                        11.0 Analytical Procedure

    11.1 Procedure. The surface tension of the tank bath may be measured 
by using a tensiometer, a stalagmometer or any other equivalent surface 
tension measuring device approved by the Administrator for measuring 
surface tension in dynes per centimeter. If the tensiometer is used, the 
procedures specified in ASTM Method D 1331-89 must be followed. If a 
stalagmometer or other device is used to measure surface tension, the 
instructions provided with the measuring device must be followed.
    11.2 Frequency of Measurements.
    11.2.1 Measurements of the bath surface tension are performed using 
a progressive system which decreases the frequency of surface tension 
measurements required when the proper surface tension is maintained.
    11.2.1.1 Initially, following the compliance date, surface tension 
measurements must be conducted once every 4 hours of tank operation for 
the first 40 hours of tank operation.
    11.2.1.2 Once there are no exceedances during a period of 40 hours 
of tank operation, measurements may be conducted once every 8 hours of 
tank operation.
    11.2.1.3 Once there are no exceedances during a second period of 40 
consecutive hours of tank operation, measurements may be conducted once 
every 40 hours of tank operation on an on-going basis, until an 
exceedance occurs. The maximum time interval for measurements is once 
every 40 hours of tank operation.
    11.2.2 If a measurement of the surface tension of the solution is 
above the 45 dynes per centimeter limit, or above an alternate surface 
tension limit established during the performance test, the time interval 
shall revert back to the original monitoring schedule of once every 4 
hours. A subsequent decrease in frequency would then be allowed 
according to Section 11.2.1.

                   12.0 Data Analysis and Calculations

    12.1 Log Book of Surface Tension Measurements and Fume Suppressant 
Additions.
    12.1.1 The surface tension of the plating or anodizing tank bath 
must be measured as specified in Section 11.2.
    12.1.2 The measurements must be recorded in the log book. In 
addition to the record of surface tension measurements, the frequency of 
fume suppressant maintenance additions and the amount of fume 
suppressant added during each maintenance addition must be recorded in 
the log book.
    12.1.3 The log book will be readily available for inspection by 
regulatory personnel.
    12.2 Instructions for Apparatus Used in Measuring Surface Tension.
    12.2.1 Included with the log book must be a copy of the instructions 
for the apparatus used for measuring the surface tension of the plating 
or anodizing bath.
    12.2.2 If a tensiometer is used, a copy of ASTM Method D 1331-89 
must be included with the log book.

[[Page 224]]

                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                       16.0 References. [Reserved]

   17.0 Tables, Diagrams, Flowcharts, and Validation Data. [Reserved]

 Method 307--Determination of Emissions From Halogenated Solvent Vapor 
            Cleaning Machines Using a Liquid Level Procedure

                     1. Applicability and Principle

    1.1 Applicability. This method is applicable to the determination of 
the halogenated solvent emissions from solvent vapor cleaners in the 
idling mode.
    1.2 Principle. The solvent level in the solvent cleaning machine is 
measured using inclined liquid level indicators. The change in liquid 
level corresponds directly to the amount of solvent lost from the 
solvent cleaning machine.

                              2. Apparatus

    Note: Mention of trade names or specific products does not 
constitute endorsement by the Environmental Protection Agency.
    2.1 Inclined Liquid Level Indicator. A schematic of the inclined 
liquid level indicators used in this method is shown in figure 307-1; 
two inclined liquid level indicators having 0.05 centimeters divisions 
or smaller shall be used. The liquid level indicators shall be made of 
glass, Teflon, or any similar material that will not react with the 
solvent being used. A 6-inch by 1-inch slope is recommended; however the 
slope may vary depending on the size and design of the solvent cleaning 
machine.
    Note: It is important that the inclined liquid level indicators be 
constructed with ease of reading in mind. The inclined liquid level 
indicators should also be mounted so that they can be raised or lowered 
if necessary to suit the solvent cleaning machine size.
[GRAPHIC] [TIFF OMITTED] TC01MY92.075

    2.2 Horizontal Indicator. Device to check the inclined liquid level 
indicators orientation relative to horizontal.
    2.3 Velocity Meter. Hotwire and vane anemometers, or other devices 
capable of measuring the flow rates ranging from 0 to 15.2 meters per 
minute across the solvent cleaning machine.

                              3. Procedure

    3.1 Connection of the Inclined Liquid Level Indicator. Connect one 
of the inclined liquid level indicators to the boiling sump drain and 
the other inclined liquid level indicator to the immersion sump drain 
using Teflon tubing and the appropriate fittings. A schematic diagram is 
shown in figure 307-2.

[[Page 225]]

[GRAPHIC] [TIFF OMITTED] TC01MY92.076

    3.2 Positioning of Velocity Meter. Position the velocity meter so 
that it measures the flow rate of the air passing directly across the 
solvent cleaning machine.
    3.3 Level the Inclined Liquid Level Indicators.
    3.4 Initial Inclined Liquid Level Indicator Readings. Open the sump 
drainage valves. Allow the solvent cleaning machine to operate long 
enough for the vapor zone to form and the system to stabilize (check 
with manufacturer). Record the inclined liquid level indicators readings 
and the starting time on the data sheet. A sample data sheet is provided 
in figure 307-3.

Date____________________________________________________________________

Run_____________________________________________________________________

Solvent type____________________________________________________________

Solvent density, g/m \3\ (lb/ft \3\)____________________________________

Length of boiling sump (SB), m (ft)__________________________

Width of boiling sump (WB), m (ft)___________________________

Length of immersion sump (SI), m (ft)________________________

Width of immersion sump (WI), m (ft)_________________________

Length of solvent vapor/air interface (SV), m (ft) ----------
--

Width of solvent vapor/air interface (WV), m (ft) ----------
--

------------------------------------------------------------------------
                                          Boiling   Immersion
               Clock time                   sump       sump    Flow rate
                                          reading    reading    reading
------------------------------------------------------------------------
 
 
 
 
 
 
------------------------------------------------------------------------

                        Figure 307-3. Data sheet.

    3.5 Final Inclined Liquid Level Indicator Readings. At the end of 
the 16-hour test run, check to make sure the inclined liquid level 
indicators are level; if not, make the necessary adjustments. Record the 
final inclined liquid level indicators readings and time.
    3.6 Determination of Solvent Vapor/Air Interface Area for Each Sump. 
Determine the area of the solvent/air interface of the individual sumps. 
Whenever possible, physically measure these dimensions, rather than 
using factory specifications. A schematic of the dimensions of a solvent 
cleaning machine is provided in figure 307-4.
[GRAPHIC] [TIFF OMITTED] TC01MY92.077

                             4. Calculations

    4.1 Nomenclature.
AB = area of boiling sump interface, m\2\ (ft\2\).
AI = area of immersion sump interface, m\2\ (ft\2\).

[[Page 226]]

AV = area of solvent/air interface, m\2\ (ft\2\).
E = emission rate, kg/m\2\-hr (lb/ft\2\-hr).
K = 100,000 cm . g/m . kg for metric units.
= 12 in./ft for English units.
LBF = final boiling sump inclined liquid level indicators 
reading, cm (in.).
LBi = initial boiling sump inclined liquid level indicators 
reading, cm (in.).
LIf = final immersion sump inclined liquid level indicators 
reading, cm (in.).
LIi = initial immersion sump inclined liquid level indicators 
reading, cm (in.).
SB = length of the boiling sump, m (ft).
SI = length of the immersion sump, m (ft).
SV = length of the solvent vapor/air interface, m (ft).
WB = width of the boiling sump, m (ft).
WI = width of the immersion sump, m (ft).
WV = width of the solvent vapor/air interface, m (ft).
[rho] = density of solvent, g/m3 (lb/ft3).
[thetas] = test time, hr.
    4.2 Area of Sump Interfaces. Calculate the areas of the boiling and 
immersion sump interfaces as follows:

AB = SB WB Eq. 307-1
AI = SI WI Eq. 307-2

    4.3 Area of Solvent/Air Interface. Calculate the area of the solvent 
vapor/air interface as follows:

AV = SV WV Eq. 307-3
    4.4 Emission Rate. Calculate the emission rate as follows:
    [GRAPHIC] [TIFF OMITTED] TR02DE94.007
    
   Method 308--Procedure for Determination of Methanol Emission From 
                           Stationary Sources

                        1.0 Scope and Application

    1.1 Analyte. Methanol. Chemical Abstract Service (CAS) No. 67-56-1.
    1.2 Applicability. This method applies to the measurement of 
methanol emissions from specified stationary sources.

                          2.0 Summary of Method

    A gas sample is extracted from the sampling point in the stack. The 
methanol is collected in deionized distilled water and adsorbed on 
silica gel. The sample is returned to the laboratory where the methanol 
in the water fraction is separated from other organic compounds with a 
gas chromatograph (GC) and is then measured by a flame ionization 
detector (FID). The fraction adsorbed on silica gel is extracted with an 
aqueous solution of n-propanol and is then separated and measured by GC/
FID.

                       3.0 Definitions. [Reserved]

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 Disclaimer. This method may involve hazardous materials, 
operations, and equipment. This test method does not purport to address 
all of the safety problems associated with its use. It is the 
responsibility of the user of this test method to establish appropriate 
safety and health practices and to determine the applicability of 
regulatory limitations before performing this test method.
    5.2 Methanol Characteristics. Methanol is flammable and a dangerous 
fire and explosion risk. It is moderately toxic by ingestion and 
inhalation.

                       6.0 Equipment and Supplies

    6.1 Sample Collection. The following items are required for sample 
collection:
    6.1.1 Sampling Train. The sampling train is shown in Figure 308-1 
and component parts are discussed below.
    6.1.1.1 Probe. Teflon[reg], approximately 6-millimeter (mm) (0.24 
inch) outside diameter.
    6.1.1.2 Impinger. A 30-milliliter (ml) midget impinger. The impinger 
must be connected with leak-free glass connectors. Silicone grease may 
not be used to lubricate the connectors.
    6.1.1.3 Adsorbent Tube. Glass tubes packed with the required amount 
of the specified adsorbent.
    6.1.1.4 Valve. Needle valve, to regulate sample gas flow rate.
    6.1.1.5 Pump. Leak-free diaphragm pump, or equivalent, to pull gas 
through the sampling train. Install a small surge tank between the pump 
and rate meter to eliminate the pulsation effect of the diaphragm pump 
on the rotameter.
    6.1.1.6 Rate Meter. Rotameter, or equivalent, capable of measuring 
flow rate to within 2 percent of the selected flow rate of up to 1000 
milliliter per minute (ml/min). Alternatively, the tester may use a 
critical orifice to set the flow rate.
    6.1.1.7 Volume Meter. Dry gas meter (DGM), sufficiently accurate to 
measure the sample volume to within 2 percent, calibrated at the 
selected flow rate and conditions actually encountered during sampling, 
and equipped with a temperature sensor (dial thermometer, or equivalent) 
capable of measuring temperature accurately to within 3 [deg]C (5.4 
[deg]F).
    6.1.1.8 Barometer. Mercury (Hg), aneroid, or other barometer capable 
of measuring atmospheric pressure to within 2.5 mm (0.1 inch) Hg. See 
the NOTE in Method 5 (40 CFR part 60, appendix A), section 6.1.2.
    6.1.1.9 Vacuum Gauge and Rotameter. At least 760-mm (30-inch) Hg 
gauge and 0- to 40-

[[Page 227]]

ml/min rotameter, to be used for leak-check of the sampling train.
    6.2 Sample Recovery. The following items are required for sample 
recovery:
    6.2.1 Wash Bottles. Polyethylene or glass, 500-ml, two.
    6.2.2 Sample Vials. Glass, 40-ml, with Teflon[reg]-lined septa, to 
store impinger samples (one per sample).
    6.2.3 Graduated Cylinder. 100-ml size.
    6.3 Analysis. The following are required for analysis:
    6.3.1 Gas Chromatograph. GC with an FID, programmable temperature 
control, and heated liquid injection port.
    6.3.2 Pump. Capable of pumping 100 ml/min. For flushing sample loop.
    6.3.3 Flow Meter. To monitor accurately sample loop flow rate of 100 
ml/min.
    6.3.4 Regulators. Two-stage regulators used on gas cylinders for GC 
and for cylinder standards.
    6.3.5 Recorder. To record, integrate, and store chromatograms.
    6.3.6 Syringes. 1.0- and 10-microliter (l) size, calibrated, for 
injecting samples.
    6.3.7 Tubing Fittings. Stainless steel, to plumb GC and gas 
cylinders.
    6.3.8 Vials. Two 5.0-ml glass vials with screw caps fitted with 
Teflon[reg]-lined septa for each sample.
    6.3.9 Pipettes. Volumetric type, assorted sizes for preparing 
calibration standards.
    6.3.10 Volumetric Flasks. Assorted sizes for preparing calibration 
standards.
    6.3.11 Vials. Glass 40-ml with Teflon[reg]-lined septa, to store 
calibration standards (one per standard).

                       7.0 Reagents and Standards

    Note: Unless otherwise indicated, all reagents must conform to the 
specifications established by the Committee on Analytical Reagents of 
the American Chemical Society. Where such specifications are not 
available, use the best available grade.

    7.1 Sampling. The following are required for sampling:
    7.1.1 Water. Deionized distilled to conform to the American Society 
for Testing and Materials (ASTM) Specification D 1193-77, Type 3. At the 
option of the analyst, the potassium permanganate (KMnO4) 
test for oxidizable organic matter may be omitted when high 
concentrations of organic matter are not expected to be present.
    7.1.2 Silica Gel. Deactivated chromatographic grade 20/40 mesh 
silica gel packed in glass adsorbent tubes. The silica gel is packed in 
two sections. The front section contains 520 milligrams (mg) of silica 
gel, and the back section contains 260 mg.
    7.2 Analysis. The following are required for analysis:
    7.2.1 Water. Same as specified in section 7.1.1.
    7.2.2 n-Propanol, 3 Percent. Mix 3 ml of n-propanol with 97 ml of 
water.
    7.2.3 Methanol Stock Standard. Prepare a methanol stock standard by 
weighing 1 gram of methanol into a 100-ml volumetric flask. Dilute to 
100 ml with water.
    7.2.3.1 Methanol Working Standard. Prepare a methanol working 
standard by pipetting 1 ml of the methanol stock standard into a 100-ml 
volumetric flask. Dilute the solution to 100 ml with water.
    7.2.3.2 Methanol Standards For Impinger Samples. Prepare a series of 
methanol standards by pipetting 1, 2, 5, 10, and 25 ml of methanol 
working standard solution respectively into five 50-ml volumetric 
flasks. Dilute the solutions to 50 ml with water. These standards will 
have 2, 4, 10, 20, and 50 [mu]g/ml of methanol, respectively. After 
preparation, transfer the solutions to 40-ml glass vials capped with 
Teflon[reg] septa and store the vials under refrigeration. Discard any 
excess solution.
    7.2.3.3 Methanol Standards for Adsorbent Tube Samples. Prepare a 
series of methanol standards by first pipetting 10 ml of the methanol 
working standard into a 100-ml volumetric flask and diluting the 
contents to exactly 100 ml with 3 percent n-propanol solution. This 
standard will contain 10 [mu]g/ml of methanol. Pipette 5, 15, and 25 ml 
of this standard, respectively, into four 50-ml volumetric flasks. 
Dilute each solution to 50 ml with 3 percent n-propanol solution. These 
standards will have 1, 3, and 5 [mu]g/ml of methanol, respectively. 
Transfer all four standards into 40-ml glass vials capped with 
Teflon[reg]-lined septa and store under refrigeration. Discard any 
excess solution.
    7.2.4 GC Column. Capillary column, 30 meters (100 feet) long with an 
inside diameter (ID) of 0.53 mm (0.02 inch), coated with DB 624 to a 
film thickness of 3.0 micrometers, ([mu]m) or an equivalent column. 
Alternatively, a 30-meter capillary column coated with polyethylene 
glycol to a film thickness of 1 [mu]m such as AT-WAX or its equivalent.
    7.2.5 Helium. Ultra high purity.
    7.2.6 Hydrogen. Zero grade.
    7.2.7 Oxygen. Zero grade.

                              8.0 Procedure

    8.1 Sampling. The following items are required for sampling:
    8.1.1 Preparation of Collection Train. Measure 20 ml of water into 
the midget impinger. The adsorbent tube must contain 520 mg of silica 
gel in the front section and 260 mg of silica gel in the backup section. 
Assemble the train as shown in Figure 308-1. An optional, second 
impinger that is left empty may be placed in front of the water-
containing impinger to act as a condensate trap. Place crushed ice and 
water around the impinger.

[[Page 228]]

[GRAPHIC] [TIFF OMITTED] TR15AP98.014

    8.1.2 Leak Check. A leak check prior to the sampling run is 
optional; however, a leak check after the sampling run is mandatory. The 
leak-check procedure is as follows:
    Temporarily attach a suitable (e.g., 0-to 40-ml/min) rotameter to 
the outlet of the DGM, and place a vacuum gauge at or near the probe 
inlet. Plug the probe inlet, pull a vacuum of at least 250 mm (10 inch) 
Hg, and note the flow rate as indicated by the rotameter. A leakage rate 
not in excess of 2 percent of the average sampling rate is acceptable.

    Note: Carefully release the probe inlet plug before turning off the 
pump.

    8.1.3 Sample Collection. Record the initial DGM reading and 
barometric pressure. To begin sampling, position the tip of the 
Teflon[reg] tubing at the sampling point, connect the tubing to the 
impinger, and start the pump. Adjust the sample flow to a constant rate 
between 200 and 1000 ml/min as indicated by the rotameter. Maintain this 
constant rate (10 percent) during the entire 
sampling run. Take readings (DGM, temperatures at DGM and at impinger 
outlet, and rate meter) at least every 5 minutes. Add more ice during 
the run to keep the temperature of the gases leaving the last impinger 
at 20 [deg]C (68 [deg]F) or less. At the conclusion of each run,

[[Page 229]]

turn off the pump, remove the Teflon[reg] tubing from the stack, and 
record the final readings. Conduct a leak check as in section 8.1.2. 
(This leak check is mandatory.) If a leak is found, void the test run or 
use procedures acceptable to the Administrator to adjust the sample 
volume for the leakage.
    8.2 Sample Recovery. The following items are required for sample 
recovery:
    8.2.1 Impinger. Disconnect the impinger. Pour the contents of the 
midget impinger into a graduated cylinder. Rinse the midget impinger and 
the connecting tubes with water, and add the rinses to the graduated 
cylinder. Record the sample volume. Transfer the sample to a glass vial 
and cap with a Teflon[reg] septum. Discard any excess sample. Place the 
samples in an ice chest for shipment to the laboratory.
    8.2.2. Adsorbent Tubes. Seal the silica gel adsorbent tubes and 
place them in an ice chest for shipment to the laboratory.

                           9.0 Quality Control

    9.1 Miscellaneous Quality Control Measures. The following quality 
control measures are required:

------------------------------------------------------------------------
       Section         Quality control measure           Effect
------------------------------------------------------------------------
8.1.2, 8.1.3, 10.1..  Sampling equipment leak   Ensures accurate
                       check and calibration.    measurement of sample
                                                 volume.
10.2................  GC calibration..........  Ensures precision of GC
                                                 analysis.
------------------------------------------------------------------------

    9.2 Applicability. When the method is used to analyze samples to 
demonstrate compliance with a source emission regulation, an audit 
sample must be analyzed, subject to availability.
    9.3 Audit Procedure. Analyze an audit sample with each set of 
compliance samples. Concurrently analyze the audit sample and a set of 
compliance samples in the same manner to evaluate the technique of the 
analyst and the standards preparation. The same analyst, analytical 
reagents, and analytical system shall be used both for the compliance 
samples and the EPA audit sample.
    9.4 Audit Sample Availability. Audit samples will be supplied only 
to enforcement agencies for compliance tests. Audit samples may be 
obtained by writing: Source Test Audit Coordinator (MD-77B), Air 
Measurement Research Division, National Exposure Research Laboratory, 
U.S. Environmental Protection Agency, Research Triangle Park, NC 27711; 
or by calling the Source Test Audit Coordinator (STAC) at (919) 541-
7834. The audit sample request must be made at least 30 days prior to 
the scheduled compliance sample analysis.
    9.5 Audit Results. Calculate the audit sample concentration 
according to the calculation procedure provided in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form included 
with the audit instructions. Send one copy to the EPA Regional Office or 
the appropriate enforcement agency and a second copy to the STAC. The 
EPA Regional office or the appropriate enforcement agency will report 
the results of the audit to the laboratory being audited. Include this 
response with the results of the compliance samples in relevant reports 
to the EPA Regional Office or the appropriate enforcement agency.

                  10.0 Calibration and Standardization

    10.1 Metering System. The following items are required for the 
metering system:
    10.1.1 Initial Calibration.
    10.1.1.1 Before its initial use in the field, first leak-check the 
metering system (drying tube, needle valve, pump, rotameter, and DGM) as 
follows: Place a vacuum gauge at the inlet to the drying tube, and pull 
a vacuum of 250 mm (10 inch) Hg; plug or pinch off the outlet of the 
flow meter, and then turn off the pump. The vacuum shall remain stable 
for at least 30 seconds. Carefully release the vacuum gauge before 
releasing the flow meter end.
    10.1.1.2 Next, remove the drying tube, and calibrate the metering 
system (at the sampling flow rate specified by the method) as follows: 
Connect an appropriately sized wet test meter (e.g., 1 liter per 
revolution (0.035 cubic feet per revolution)) to the inlet of the drying 
tube. Make three independent calibrations runs, using at least five 
revolutions of the DGM per run. Calculate the calibration factor, Y (wet 
test meter calibration volume divided by the DGM volume, both volumes 
adjusted to the same reference temperature and pressure), for each run, 
and average the results. If any Y-value deviates by more than 2 percent 
from the average, the metering system is unacceptable for use. 
Otherwise, use the average as the calibration factor for subsequent test 
runs.
    10.1.2 Posttest Calibration Check. After each field test series, 
conduct a calibration check as in section 10.1.1 above, except for the 
following variations: (a) The leak check is not to be conducted, (b) 
three, or more revolutions of the DGM may be used, and (c) only two 
independent runs need be made. If the calibration factor does not 
deviate by more than 5 percent from the initial calibration factor 
(determined in section 10.1.1), then the DGM volumes obtained during the 
test series are acceptable. If the calibration factor deviates by more 
than 5 percent, recalibrate the metering system as in section 10.1.1, 
and for the calculations, use the calibration factor (initial or 
recalibration) that yields the lower gas volume for each test run.
    10.1.3 Temperature Sensors. Calibrate against mercury-in-glass 
thermometers.

[[Page 230]]

    10.1.4 Rotameter. The rotameter need not be calibrated, but should 
be cleaned and maintained according to the manufacturer's instruction.
    10.1.5 Barometer. Calibrate against a mercury barometer.
    10.2 Gas Chromatograph. The following procedures are required for 
the gas chromatograph:
    10.2.1 Initial Calibration. Inject 1 [mu]l of each of the standards 
prepared in sections 7.2.3.3 and 7.2.3.4 into the GC and record the 
response. Repeat the injections for each standard until two successive 
injections agree within 5 percent. Using the mean response for each 
calibration standard, prepare a linear least squares equation relating 
the response to the mass of methanol in the sample. Perform the 
calibration before analyzing each set of samples.
    10.2.2 Continuing Calibration. At the beginning of each day, analyze 
the mid level calibration standard as described in section 10.5.1. The 
response from the daily analysis must agree with the response from the 
initial calibration within 10 percent. If it does not, the initial 
calibration must be repeated.

                        11.0 Analytical Procedure

    11.1 Gas Chromatograph Operating Conditions. The following operating 
conditions are required for the GC:
    11.1.1 Injector. Configured for capillary column, splitless, 200 
[deg]C (392 [deg]F).
    11.1.2 Carrier. Helium at 10 ml/min.
    11.1.3 Oven. Initially at 45 [deg]C for 3 minutes; then raise by 10 
[deg]C to 70 [deg]C; then raise by 70 [deg]C/min to 200 [deg]C.
    11.2 Impinger Sample. Inject 1 [mu]l of the stored sample into the 
GC. Repeat the injection and average the results. If the sample response 
is above that of the highest calibration standard, either dilute the 
sample until it is in the measurement range of the calibration line or 
prepare additional calibration standards. If the sample response is 
below that of the lowest calibration standard, prepare additional 
calibration standards. If additional calibration standards are prepared, 
there shall be at least two that bracket the response of the sample. 
These standards should produce approximately 50 percent and 150 percent 
of the response of the sample.
    11.3 Silica Gel Adsorbent Sample. The following items are required 
for the silica gel adsorbent samples:
    11.3.1 Preparation of Samples. Extract the front and backup sections 
of the adsorbent tube separately. With a file, score the glass adsorbent 
tube in front of the first section of silica gel. Break the tube open. 
Remove and discard the glass wool. Transfer the first section of the 
silica gel to a 5-ml glass vial and stopper the vial. Remove the spacer 
between the first and second section of the adsorbent tube and discard 
it. Transfer the second section of silica gel to a separate 5-ml glass 
vial and stopper the vial.
    11.3.2 Desorption of Samples. Add 3 ml of the 10 percent n-propanol 
solution to each of the stoppered vials and shake or vibrate the vials 
for 30 minutes.
    11.3.3 Inject a 1-[mu]l aliquot of the diluted sample from each vial 
into the GC. Repeat the injection and average the results. If the sample 
response is above that of the highest calibration standard, either 
dilute the sample until it is in the measurement range of the 
calibration line or prepare additional calibration standards. If the 
sample response is below that of the lowest calibration standard, 
prepare additional calibration standards. If additional calibration 
standards are prepared, there shall be at least two that bracket the 
response of the sample. These standards should produce approximately 50 
percent and 150 percent of the response of the sample.

                   12.0 Data Analysis and Calculations

    12.1 Nomenclature.

Caf=Concentration of methanol in the front of the adsorbent 
tube, [mu]g/ml.
Cab=Concentration of methanol in the back of the adsorbent 
tube, [mu]g/ml.
Ci=Concentration of methanol in the impinger portion of the 
sample train, [mu]g/ml.
E=Mass emission rate of methanol, [mu]g/hr (lb/hr).
Mtot=Total mass of methanol collected in the sample train, 
[mu]g.
Pbar=Barometric pressure at the exit orifice of the DGM, mm 
Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qstd=Dry volumetric stack gas flow rate corrected to standard 
conditions, dscm/hr (dscf/hr).
Tm=Average DGM absolute temperature, degrees K ( [deg]R).
Tstd=Standard absolute temperature, 293 degrees K (528 
[deg]R).
Vaf=Volume of front half adsorbent sample, ml.
Vab=Volume of back half adsorbent sample, ml.
Vi=Volume of impinger sample, ml.
Vm=Dry gas volume as measured by the DGM, dry cubic meters 
(dcm), dry cubic feet (dcf).
Vm(std)=Dry gas volume measured by the DGM, corrected to 
standard conditions, dry standard cubic meters (dscm), dry standard 
cubic feet (dscf).

    12.2 Mass of Methanol. Calculate the total mass of methanol 
collected in the sampling train using Equation 308-1.

[[Page 231]]

[GRAPHIC] [TIFF OMITTED] TR15AP98.015

    12.3 Dry Sample Gas Volume, Corrected to Standard Conditions. 
Calculate the volume of gas sampled at standard conditions using 
Equation 308-2.
[GRAPHIC] [TIFF OMITTED] TR15AP98.016

    12.4 Mass Emission Rate of Methanol. Calculate the mass emission 
rate of methanol using Equation 308-3.
[GRAPHIC] [TIFF OMITTED] TR15AP98.017

                   13.0 Method Performance. [Reserved]

                  14.0 Pollution Prevention. [Reserved]

                    15.0 Waste Management. [Reserved]

                            16.0 Bibliography

    1. Rom, J.J. ``Maintenance, Calibration, and Operation of Isokinetic 
Source Sampling Equipment.'' Office of Air Programs, Environmental 
Protection Agency. Research Triangle Park, NC. APTD-0576 March 1972.
    2. Annual Book of ASTM Standards. Part 31; Water, Atmospheric 
Analysis. American Society for Testing and Materials. Philadelphia, PA. 
1974. pp. 40-42.
    3. Westlin, P.R. and R.T. Shigehara. ``Procedure for Calibrating and 
Using Dry Gas Volume Meters as Calibration Standards.'' Source 
Evaluation Society Newsletter. 3(1) :17-30. February 1978.
    4. Yu, K.K. ``Evaluation of Moisture Effect on Dry Gas Meter 
Calibration.'' Source Evaluation Society Newsletter. 5(1) :24-28. 
February 1980.
    5. NIOSH Manual of Analytical Methods, Volume 2. U.S. Department of 
Health and Human Services National Institute for Occupational Safety and 
Health. Center for Disease Control. 4676 Columbia Parkway, Cincinnati, 
OH 45226. (available from the Superintendent of Documents, Government 
Printing Office, Washington, DC 20402.)
    6. Pinkerton, J.E. ``Method for Measuring Methanol in Pulp Mill Vent 
Gases.'' National Council of the Pulp and Paper Industry for Air and 
Stream Improvement, Inc., New York, NY.

   17.0 Tables, Diagrams, Flowcharts, and Validation Data. [Reserved]

Method 310A--Determination of Residual Hexane Through Gas Chromatography

                        1.0 Scope and Application

    1.1 This method is used to analyze any crumb rubber or water samples 
for residual hexane content.
    1.2 The sample is heated in a sealed bottle with an internal 
standard and the vapor is analyzed by gas chromatography.

                          2.0 Summary of Method

    2.1 This method, utilizing a capillary column gas chromatograph with 
a flame ionization detector, determines the concentration of residual 
hexane in rubber crumb samples.

                             3.0 Definitions

    3.1 The definitions are included in the text as needed.

                            4.0 Interferences

    4.1 There are no known interferences.

                               5.0 Safety

    5.1 It is the responsibility of the user of this procedure to 
establish safety and health practices applicable to their specific 
operation.

                       6.0 Equipment and Supplies

    6.1 Gas Chromatograph with a flame ionization detector and data 
handling station equipped with a capillary column 30 meters long.

[[Page 232]]

    6.2 Chromatograph conditions for Sigma 1:
    6.2.1 Helium pressure: 50 inlet A, 14 aux
    6.2.2 Carrier flow: 25 cc/min
    6.2.3 Range switch: 100x
    6.2.4 DB: 1 capillary column
    6.3 Chromatograph conditions for Hewlett-Packard GC:
    6.3.1 Initial temperature: 40 [deg]C
    6.3.2 Initial time: 8 min
    6.3.3 Rate: 0
    6.3.4 Range: 2
    6.3.5 DB: 1705 capillary column
    6.4 Septum bottles and stoppers
    6.5 Gas Syringe--0.5 cc

                       7.0 Reagents and Standards

    7.1 Chloroform, 99.9+%, A.S.C. HPLC grade

            8.0 Sample Collection, Preservation, and Storage

    8.1 A representative sample should be caught in a clean 8 oz. 
container with a secure lid.
    8.2 The container should be labeled with sample identification, date 
and time.

                           9.0 Quality Control

    9.1 The instrument is calibrated by injecting calibration solution 
(Section 10.2 of this method) five times.
    9.2 The retention time for components of interest and relative 
response of monomer to the internal standard is determined.
    9.3 Recovery efficiency must be determined once for each sample type 
and whenever modifications are made to the method.
    9.3.1 Determine the percent hexane in three separate dried rubber 
crumb samples.
    9.3.2 Weigh a portion of each crumb sample into separate sample 
bottles and add a known amount of hexane (10 microliters) by microliter 
syringe and 20 microliters of internal standard. Analyze each by the 
described procedure and calculate the percent recovery of the known 
added hexane.
    9.3.3 Repeat the previous step using twice the hexane level (20 
microliters), analyze and calculate the percent recovery of the known 
added hexane.
    9.3.4 Set up two additional sets of samples using 10 microliters and 
20 microliters of hexane as before, but add an amount of water equal to 
the dry crumb used. Analyze and calculate percent recovery to show the 
effect of free water on the results obtained.
    9.3.5 A value of R between 0.70 and 1.30 is acceptable.
    9.3.6 R shall be used to correct all reported results for each 
compound by dividing the measured results of each compound by the R for 
that compound for the same sample type.

                10.0 Calibration and Instrument Settings

    10.1 Calibrate the chromatograph using a standard made by injecting 
10 [mu]l of fresh hexane and 20 [mu]l of chloroform into a sealed septum 
bottle. This standard will be 0.6 wt.% total hexane based on 1 gram of 
dry rubber.
    10.2 Analyze the hexane used and calculate the percentage of each 
hexane isomer (2-methylpentane, 3-methylpentane, n-hexane, and 
methylcyclo-pentane). Enter these percentages into the method 
calibration table.
    10.3 Heat the standard bottle for 30 minutes in a 105 [deg]C oven.
    10.4 Inject about 0.25 cc of vapor into the gas chromatograph and 
after the analysis is finished, calibrate according to the procedures 
described by the instrument manufacturer.

                             11.0 Procedure

    11.1 Using a cold mill set at a wide roller gap (125-150 mm), mill 
about 250 grams of crumb two times to homogenize the sample.
    11.2 Weigh about 2 grams of wet crumb into a septum bottle and cap 
with a septum ring. Add 20 [mu]l of chloroform with a syringe and place 
in a 105 [deg]C oven for 45 minutes.
    11.3 Run the moisture content on a separate portion of the sample 
and calculate the grams of dry rubber put into the septum bottle.
    11.4 Set up the data station on the required method and enter the 
dry rubber weight in the sample weight field.
    11.5 Inject a 0.25 cc vapor sample into the chromatograph and push 
the start button.
    11.6 At the end of the analysis, the data station will print a 
report listing the concentration of each identified component.
    11.7 To analyze water samples, pipet 5 ml of sample into the septum 
bottle, cap and add 20 [mu]l of chloroform. Place in a 105 [deg]C oven 
for 30 minutes.
    11.8 Enter 5 grams into the sample weight field.
    11.9 Inject a 0.25 cc vapor sample into the chromatograph and push 
the start button.
    11.10 At the end of the analysis, the data station will print a 
report listing the concentration of each identified component.

                   12.0 Data Analysis and Calculation

    12.1 For samples that are prepared as in section 11 of this method, 
ppm n-hexane is read directly from the computer.
    12.2 The formulas for calculation of the results are as follows:

ppmhexane=(AhexanexRhexane)/
(AisxRis)

Where:
Ahexane=area of hexane
Rhexane=response of hexane
Ais=area of the internal standard
Ris=response of the internal standard

[[Page 233]]

% hexane in crumb=(ppmhexane/sample amount)100
    12.3 Correct the results by the value of R (as determined in 
sections 9.3.4, 9.3.5, and 9.3.6 of this method).

                         13.0 Method Performance

    13.1 The test has a standard deviation of 0.14 wt% at 0.66 wt% 
hexane. Spike recovery of 12 samples at two levels of hexane averaged 
102.3%. Note: Recovery must be determined for each type of sample. The 
values given here are meant to be examples of method performance.

                        14.0 Pollution Prevention

    14.1 Waste generation should be minimized where possible. Sample 
size should be an amount necessary to adequately run the analysis.

                          15.0 Waste Management

    15.1 All waste shall be handled in accordance with federal and state 
environmental regulations.

                    16.0 References and Publications

    16.1 DSM Copolymer Test Method T-3380.

Method 310B--Determination of Residual Hexane Through Gas Chromatography

                        1.0 Scope and Application

----------------------------------------------------------------------------------------------------------------
                                                                                       Method sensitivity (5.5g
                 Analyte                       CAS No.               Matrix                  sample size)
----------------------------------------------------------------------------------------------------------------
Hexane...................................        110-54-3  Rubber crumb.............  .01 wt%.
Applicable Termonomer....................  ..............  Rubber crumb.............  .001 wt%.
----------------------------------------------------------------------------------------------------------------

    1.1 Data Quality Objectives:
    In the production of ethylene-propylene terpolymer crumb rubber, the 
polymer is recovered from solution by flashing off the solvent with 
steam and hot water. The resulting water-crumb slurry is then pumped to 
the finishing units. Certain amounts of solvent (hexane being the most 
commonly used solvent) and diene monomer remain in the crumb. The 
analyst uses the following procedure to determine those amounts.

                          2.0 Summary of Method

    2.1 The crumb rubber sample is dissolved in toluene to which heptane 
has been added as an internal standard. Acetone is then added to this 
solution to precipitate the crumb, and the supernatant is analyzed for 
hexane and diene by a gas chromatograph equipped with a flame ionization 
detector (FID).

                             3.0 Definitions

    3.1 Included in text as needed.

                            4.0 Interferences

    4.1 None known.
    4.2 Benzene, introduced as a contaminant in the toluene solvent, 
elutes between methyl cyclopentane and cyclohexane. However, the benzene 
peak is completely resolved.
    4.3 2,2-dimethyl pentane, a minor component of the hexane used in 
our process, elutes just prior to methyl cyclopentane. It is included as 
``hexane'' in the analysis whether it is integrated separately or 
included in the methyl cyclopentane peak.

                               5.0 Safety

    5.1 This procedure does not purport to address all of the safety 
concerns associated with its use. It is the responsibility of the user 
of this procedure to establish appropriate safety and health practices 
and determine the applicability of regulatory limitations prior to use.
    5.2 Chemicals used in this analysis are flammable and hazardous (see 
specific toxicity information below). Avoid contact with sources of 
ignition during sample prep. All handling should be done beneath a hood. 
Playtex or nitrile gloves recommended.
    5.3 Hexane is toxic by ingestion and inhalation. Vapor inhalation 
causes irritation of nasal and respiratory passages, headache, 
dizziness, nausea, central nervous system depression. Chronic 
overexposure can cause severe nerve damage. May cause irritation on 
contact with skin or eyes. May cause damage to kidneys.
    5.4 Termonomer may be harmful by inhalation, ingestion, or skin 
absorption. Vapor or mist is irritating to the eyes, mucous membranes, 
and upper respiratory tract. Causes skin irritation.
    5.5 Toluene is harmful or fatal if swallowed. Vapor harmful if 
inhaled. Symptoms: headache, dizziness, hallucinations, distorted 
perceptions, changes in motor activity, nausea, diarrhea, respiratory 
irritation, central nervous system depression, unconsciousness, liver, 
kidney and lung damage. Contact can cause severe eye irritation. May 
cause skin irritation. Causes irritation of eyes, nose, and throat.

[[Page 234]]

    5.6 Acetone, at high concentrations or prolonged overexposure, may 
cause headache, dizziness, irritation of eyes and respiratory tract, 
loss of strength, and narcosis. Eye contact causes severe irritation; 
skin contact may cause mild irritation. Concentrations of 20,000 ppm are 
immediately dangerous to life and health.
    5.7 Heptane is harmful if inhaled or swallowed. May be harmful if 
absorbed through the skin. Vapor or mist is irritating to the eyes, 
mucous membranes, and upper respiratory tract. Prolonged or repeated 
exposure to skin causes defatting and dermatitis.
    5.8 The steam oven used to dry the polymer in this procedure is set 
at 110 [deg]C. Wear leather gloves when removing bottles from the oven.

                       6.0 Equipment and Supplies

    6.1 4000-ml volumetric flask
    6.2 100-ml volumetric pipette
    6.3 1000-ml volumetric flask
    6.4 8-oz. French Square sample bottles with plastic-lined caps
    6.5 Top-loading balance
    6.6 Laboratory shaker
    6.7 Laboratory oven set at 110 [deg]C (steam oven)
    6.8 Gas chromatograph, Hewlett-Packard 5890A, or equivalent, 
interfaced with HP 7673A (or equivalent) autosampler (equipped with 
nanoliter adapter and robotic arm), and HP 3396 series II or 3392A (or 
equivalent) integrator/controller.
    6.9 GC column, capillary type, 50m x 0.53mm, methyl silicone, 5 
micron film thickness, Quadrex, or equivalent.
    6.10 Computerized data acquisition system, such as CIS/CALS
    6.11 Crimp-top sample vials and HP p/n 5181-1211 crimp caps, or 
screw-top autosampler vials and screw tops.
    6.12 Glass syringes, 5-ml, with ``Luer-lock'' fitting
    6.13 Filters, PTFE, .45[mu]m pore size, Gelman Acrodisc or 
equivalent, to fit on Luer-lock syringes (in 6.12, above).

                       7.0 Reagents and Standards

    7.1 Reagent toluene, EM Science Omnisolv (or equivalent)
    Purity Check: Prior to using any bottle of reagent toluene, analyze 
it according to section 11.2 of this method. Use the bottle only if 
hexane, heptane, and termonomer peak areas are less than 15 each (note 
that an area of 15 is equivalent to less than 0.01 wt% in a 10g sample).
    7.2 Reagent acetone, EM Science Omnisolv HR-GC (or equivalent)
    Purity Check: Prior to using any bottle of reagent acetone, analyze 
it according to section 11.2 of this method. Use the bottle only if 
hexane, heptane, and termonomer peak areas are less than 15 each.
    7.3 Reagent heptane, Aldrich Chemical Gold Label, Cat 
15,487-3 (or equivalent)
    Purity Check: Prior to using any bottle of reagent heptane, analyze 
it according to section 11.2 of this method. Use the bottle only if 
hexane and termonomer peak areas are less than 5 each.
    7.4 Internal standard solution--used as a concentrate for 
preparation of the more dilute Polymer Dissolving Solution. It contains 
12.00g heptane/100ml of solution which is 120.0g per liter.
    Preparation of internal standard solution (polymer dissolving stock 
solution):

------------------------------------------------------------------------
                 Action                               Notes
------------------------------------------------------------------------
7.4.1 Tare a clean, dry 1-liter          If the 1-liter volumetric flask
 volumetric flask on the balance.         is too tall to fit in the
 Record the weight to three places.       balance case, you can shield
                                          the flask from drafts by
                                          inverting a paint bucket with
                                          a hole cut in the bottom over
                                          the balance cover. Allow the
                                          neck of the flask to project
                                          through the hole in the
                                          bucket.
7.4.2 Weigh 120.00 g of n-heptane into   Use 99+% n-heptane from Aldrich
 the flask. Record the total weight of    or Janssen Chimica.
 the flask and heptane as well as the
 weight of heptane added.
7.4.3 Fill the flask close to the mark   Use EM Science Omnisolve
 with toluene, about 1 to 2    toluene, Grade TX0737-1, or
 below the mark.                          equivalent.
7.4.4 Shake the flask vigorously to mix  Allow any bubbles to clear
 the contents.                            before proceeding to the next
                                          step.
7.4.5 Top off the flask to the mark
 with toluene. Shake vigorously, as in
 section 7.4.4 of this method, to mix
 well.
7.4.6 Weigh the flask containing the
 solution on the three place balance
 record the weight
7.4.7 Transfer the contents of the       Discard any excess solution
 flask to a 1 qt Boston round bottle.
7.4.8 Label the bottle with the          Be sure to include the words
 identity of the contents, the weights    ``Hexane in Crumb Polymer
 of heptane and toluene used, the date    Dissolving Stock Solution'' on
 of preparation and the preparer's name.  the label.
7.4.9 Refrigerate the completed blend
 for the use of the routine Technicians.
------------------------------------------------------------------------


[[Page 235]]

    7.5 Polymer Dissolving Solution (``PDS'')--Heptane (as internal 
standard) in toluene. This solution contains 0.3g of heptane internal 
standard per 100 ml of solution.
    7.5.1 Preparation of Polymer Dissolving Solution. Fill a 4,000-ml 
volumetric flask about \3/4\ full with toluene.
    7.5.2 Add 100 ml of the internal standard solution (section 7.4 of 
this method) to the flask using the 100ml pipette.
    7.5.3 Fill the flask to the mark with toluene. Discard any excess.
    7.5.4 Add a large magnetic stirring bar to the flask and mix by 
stirring.
    7.5.5 Transfer the polymer solvent solution to the one-gallon 
labeled container with 50ml volumetric dispenser attached.
    7.5.6 Purity Check: Analyze according to section 11.2. NOTE: You 
must ``precipitate'' the sample with an equal part of acetone (thus 
duplicating actual test conditions-- see section 11.1 of this method, 
sample prep) before analyzing. Analyze the reagent 3 times to quantify 
the C6 and termonomer interferences. Inspect the results to 
ensure good agreement among the three runs (within 10%).
    7.5.7 Tag the bottle with the following information:

     POLYMER DISSOLVING SOLUTION FOR C6 IN CRUMB ANALYSIS
     PREPARER'S NAME
     DATE
     CALS FILE ID'S OF THE THREE ANALYSES FOR PURITY (from section 7.5.6 
of this method)

    7.6 Quality Control Solution: the quality control solution is 
prepared by adding specific amounts of mixed hexanes (barge hexane), n-
nonane and termonomer to some polymer dissolving solution. Nonane elutes 
in the same approximate time region as termonomer and is used to 
quantify in that region because it has a longer shelf life. Termonomer, 
having a high tendency to polymerize, is used in the QC solution only to 
ensure that both termonomer isomers elute at the proper time.
    First, a concentrated stock solution is prepared; the final QC 
solution can then be prepared by diluting the stock solution.
    7.6.1 In preparation of stock solution, fill a 1-liter volumetric 
flask partially with polymer dissolving solution (PDS)--see section 7.5 
of this method. Add 20.0 ml barge hexane, 5.0 ml n-nonane, and 3 ml 
termonomer. Finish filling the volumetric to the mark with PDS.
    7.6.2 In preparation of quality control solution, dilute the quality 
control stock solution (above) precisely 1:10 with PDS, i.e. 10 ml of 
stock solution made up to 100 ml (volumetric flask) with PDS. Pour the 
solution into a 4 oz. Boston round bottle and store in the refrigerator.

             8.0 Sample Collection, Preservation and Storage

    8.1 Line up facility to catch crumb samples. The facility is a 
special facility where the sample is drawn.
    8.1.1 Ensure that the cock valve beneath facility is closed.
    8.1.2 Line up the system from the slurry line cock valve to the cock 
valve at the nozzle on the stripper.
    8.1.3 Allow the system to flush through facility for a period of 30 
seconds.
    8.2 Catch a slurry crumb sample.
    8.2.1 Simultaneously close the cock valves upstream and downstream 
of facility.
    8.2.2 Close the cock valve beneath the slurry line in service.
    8.2.3 Line up the cooling tower water through the sample bomb water 
jacket to the sewer for a minimum of 30 minutes.
    8.2.4 Place the sample catching basket beneath facility and open the 
cock valve underneath the bomb to retrieve the rubber crumb.
    8.2.5 If no rubber falls by gravity into the basket, line up 
nitrogen to the bleeder upstream of the sample bomb and force the rubber 
into the basket.
    8.2.6 Close the cock valve underneath the sample bomb.
    8.3 Fill a plastic ``Whirl-pak'' sample bag with slurry crumb and 
send it to the lab immediately.
    8.4 Once the sample reaches the lab, it should be prepped as soon as 
possible to avoid hexane loss through evaporation. Samples which have 
lain untouched for more than 30 minutes should be discarded.

                           9.0 Quality Control

    Quality control is monitored via a computer program that tracks 
analyses of a prepared QC sample (from section 7.6.2 of this method). 
The QC sample result is entered daily into the program, which plots the 
result as a data point on a statistical chart. If the data point does 
not satisfy the ``in-control'' criteria (as defined by the lab quality 
facilitator), an ``out-of-control'' flag appears, mandating corrective 
action.
    In addition, the area of the n-heptane peak is monitored so that any 
errors in making up the polymer dissolving solution will be caught and 
corrected. Refer to section 12.4 of this method.

    9.1 Fill an autosampler vial with the quality control solution (from 
section 7.6.2 of this method) and analyze on the GC as normal (per 
section 11 of this method).
    9.2 Add the concentrations of the 5 hexane isomers as they appear on 
the CALS printout. Also include the 2,2-dimethyl-pentane peak just ahead 
of the methyl cyclopentane (the fourth major isomer) peak in the event 
that the peak integration split this peak out. Do not include the 
benzene peak in the sum.

[[Page 236]]

Note the nonane concentration. Record both results (total hexane and 
nonane) in the QC computer program. If out of control, and GC appears to 
be functioning within normal parameters, reanalyze a fresh control 
sample. If the fresh QC is not in control, check stock solution for 
contaminants or make up a new QC sample with the toluene currently in 
use. If instrument remains out-of-control, more thorough GC 
troubleshooting may be needed.
    Also, verify that the instrument has detected both isomers of 
termonomer (quantification not necessary--see section 7.0 of this 
method).
    9.3 Recovery efficiency must be determined for high ethylene 
concentration, low ethylene concentration, E-P terpolymer, or oil 
extended samples and whenever modifications are made to the method. 
Recovery shall be between 70 and 130 percent. All test results must be 
corrected by the recovery efficiency value (R).
    9.3.1 Approximately 10 grams of wet EPDM crumb (equivalent to about 
5 grams of dry rubber) shall be added to six sample bottles containing 
100 ml of hexane in crumb polymer dissolving solution (toluene 
containing 0.3 gram n-heptane/100 ml solution). The polymer shall be 
dissolved by agitating the bottles on a shaker for 4 hours. The polymer 
shall be precipitated using 100 ml acetone.
    9.3.2 The supernatant liquid shall be decanted from the polymer. 
Care shall be taken to remove as much of the liquid phase from the 
sample as possible to minimize the effect of retained liquid phase upon 
the next cycle of the analysis. The supernatant liquid shall be analyzed 
by gas chromatography using an internal standard quantitation method 
with heptane as the internal standard.
    9.3.3 The precipitated polymer from the steps described above shall 
be redissolved using toluene as the solvent. No heptane shall be added 
to the sample in the second dissolving step. The toluene solvent and 
acetone precipitant shall be determined to be free of interfering 
compounds.
    9.3.4 The rubber which was dissolved in the toluene shall be 
precipitated with acetone as before, and the supernatant liquid decanted 
from the precipitated polymer. The liquid shall be analyzed by gas 
chromatography and the rubber phase dried in a steam-oven to determine 
the final polymer weight.
    9.3.5 The ratios of the areas of the hexane peaks and of the heptane 
internal standard peak shall be calculated for each of the six samples 
in the two analysis cycles outlined above. The area ratios of the total 
hexane to heptane (R1) shall be determined for the two analysis cycles 
of the sample set. The ratio of the values of R1 from the second 
analysis cycle to the first cycle shall be determined to give a second 
ratio (R2).

                  10.0 Calibration and Standardization

    The procedure for preparing a Quality Control sample with the 
internal standard in it is outlined in section 7.6 of this method.

    10.1 The relative FID response factors for n-heptane, the internal 
standard, versus the various hexane isomers and termonomer are 
relatively constant and should seldom need to be altered. However 
Baseline construction is a most critical factor in the production of 
good data. For this reason, close attention should be paid to peak 
integration. Procedures for handling peak integration will depend upon 
the data system used.
    10.2 If recalibration of the analysis is needed, make up a 
calibration blend of the internal standard and the analytes as detailed 
below and analyze it using the analytical method used for the samples.
    10.2.1 Weigh 5 g heptane into a tared scintillation vial to five 
places.
    10.2.2 Add 0.2 ml termonomer to the vial and reweigh.
    10.2.3 Add 0.5 ml hexane to the vial and reweigh.
    10.2.4 Cap, and shake vigorously to mix.
    10.2.5 Calculate the weights of termonomer and of hexane added and 
divide their weights by the weight of the n-heptane added. The result is 
the known of given value for the calibration.
    10.2.6 Add 0.4 ml of this mixture to a mixture of 100 ml toluene and 
100 ml of acetone. Cap and shake vigorously to mix.
    10.2.7 Analyze the sample.
    10.2.8 Divide the termonomer area and the total areas of the hexane 
peaks by the n-heptane area. This result is the ``found'' value for the 
calibration.
    10.2.9 Divide the appropriate ``known'' value from 10.2.5 by the 
found value from 10.2.8. The result is the response factor for the 
analyte in question. Previous work has shown that the standard deviation 
of the calibration method is about 1% relative.

                             11.0 Procedure

    11.1 SAMPLE PREPARATION
    11.1.1 Tare an 8oz sample bottle--Tag attached, cap off; record 
weight and sample ID on tag in pencil.
    11.1.2 Place crumb sample in bottle: RLA-3: 10 g (gives a dry wt. of 
5.5 g).
    11.1.3 Dispense 100ml of PDS into each bottle. SAMPLE SHOULD BE 
PLACED INTO SOLUTION ASAP TO AVOID HEXANE LOSS--Using ``Dispensette'' 
pipettor. Before dispensing, ``purge'' the dispensette (25% of its 
volume) into a waste bottle to eliminate any voids.
    11.1.4 Tightly cap bottles and load samples into shaker.
    11.1.5 Insure that ``ON-OFF'' switch on the shaker itself is ``ON.''
    11.1.6 Locate shaker timer. Insure that toggle switch atop timer 
control box is in

[[Page 237]]

the middle (``off'') position. If display reads ``04:00'' (4 hours), 
move toggle switch to the left position. Shaker should begin operating.
    11.1.7 After shaker stops, add 100 ml acetone to each sample to 
precipitate polymer. Shake minimum of 5 minutes on shaker--Vistalon 
sample may not have fully dissolved; nevertheless, for purposes of 
consistency, 4 hours is the agreed-upon dissolving time.
    11.1.8 Using a 5-ml glass Luer-lock syringe and Acrodisc filter, 
filter some of the supernatant liquid into an autosampler vial; crimp 
the vial and load it into the GC autosampler for analysis (section 11.2 
of this method)--The samples are filtered to prevent polymer buildup in 
the GC. Clean the syringes in toluene.
    11.1.9 Decant remaining supernatant into a hydrocarbon waste sink, 
being careful not to discard any of the polymer. Place bottle of 
precipitate into the steam oven and dry for six hours--Some grades of 
Vistalon produce very small particles in the precipitate, thus making 
complete decanting impossible without discarding some polymer. In this 
case, decant as much as possible and put into the oven as is, allowing 
the oven to drive off remaining supernatant (this practice is avoided 
for environmental reasons). WARNING: OVEN IS HOT--110 [deg]C (230 
[deg]F).
    11.1.10 Cool, weigh and record final weight of bottle.
    11.2 GC ANALYSIS
    11.2.1 Initiate the CALS computer channel.
    11.2.2 Enter the correct instrument method into the GC's integrator.
    11.2.3 Load sample vial(s) into autosampler.
    11.2.4 Start the integrator.
    11.2.5 When analysis is complete, plot CALS run to check baseline 
skim.

                   12.0 Data Analysis and Calculations

    12.1 Add the concentrations of the hexane peaks as they appear on 
the CALS printout. Do not include the benzene peak in the sum.
    12.2 Subtract any hexane interferences found in the PDS (see section 
7.5.6 of this method); record the result.
    12.3 Note the termonomer concentration on the CALS printout. 
Subtract any termonomer interference found in the PDS and record this 
result in a ``% termonomer by GC'' column in a logbook.
    12.4 Record the area (from CALS printout) of the heptane internal 
standard peak in a ``C7 area'' column in the logbook. This helps track 
instrument performance over the long term.
    12.5 After obtaining the final dry weight of polymer used (Section 
11.1.10 of this method), record that result in a ``dry wt.'' column of 
the logbook (for oil extended polymer, the amount of oil extracted is 
added to the dry rubber weight).
    12.6 Divide the %C6 by the dry weight to obtain the total PHR hexane 
in crumb. Similarly, divide the % termonomer by the dry weight to obtain 
the total PHR termonomer in crumb. Note that PHR is an abbreviation for 
``parts per hundred''. Record both the hexane and termonomer results in 
the logbook.
    12.7 Correct all results by the recovery efficiency value (R).

                         13.0 Method Performance

    13.1 The method has been shown to provide 100% recovery of the 
hexane analyte. The method was found to give a 6% relative standard 
deviation when the same six portions of the same sample were carried 
through the procedure. Note: These values are examples; each sample 
type, as specified in Section 9.3, must be tested for sample recovery.

                        14.0 Pollution Prevention

    14.1 Dispose of all hydrocarbon liquids in the appropriate disposal 
sink system; never pour hydrocarbons down a water sink.
    14.2 As discussed in section 11.1.9 of this method, the analyst can 
minimize venting hydrocarbon vapor to the atmosphere by decanting as 
much hydrocarbon liquid as possible before oven drying.

                          15.0 Waste Mamagement

    15.1 The Technician conducting the analysis should follow the proper 
waste management practices for their laboratory location.

                             16.0 References

    16.1 Baton Rouge Chemical Plant Analytical Procedure no. BRCP 1302
    16.2 Material Safety Data Sheets (from chemical vendors) for hexane, 
ENB, toluene, acetone, and heptane

 Method 310C--Determination of Residual N-Hexane in EPDM Rubber Through 
                           Gas Chromatography

                        1.0 Scope and Application

    1.1 This method describes a procedure for the determination of 
residual hexane in EPDM wet crumb rubber in the 0.01--2% range by 
solvent extraction of the hexane followed by gas chromatographic 
analysis where the hexane is detected by flame ionization and quantified 
via an internal standard.
    1.2 This method may involve hazardous materials operations and 
equipment. This method does not purport to address all the safety 
problems associated with it use, if any. It is the responsibility of the 
user to consult and establish appropriate safety and health practices 
and determine the applicability of regulatory limitations prior to use.

[[Page 238]]

                               2.0 Summary

    2.1 Residual hexane contained in wet pieces of EPDM polymer is 
extracted with MIBK. A known amount of an internal standard (IS) is 
added to the extract which is subsequently analyzed via gas 
chromatography where the hexane and IS are separated and detected 
utilizing a megabore column and flame ionization detection (FID). From 
the response to the hexane and the IS, the amount of hexane in the EPDM 
polymer is calculated.

                             3.0 Definitions

    3.1 Hexane--refers to n-hexane
    3.2 Heptane--refers to n-heptane
    3.3 MIBK--methyl isobutyl ketone (4 methyl 2--Pentanone)

                            4.0 Interferences

    4.1 Material eluting at or near the hexane and/or the IS will cause 
erroneous results. Prior to extraction, solvent blanks must be analyzed 
to confirm the absence of interfering peaks.

                               5.0 Safety

    5.1 Review Material Safety Data Sheets of the chemicals used in this 
method.

                       6.0 Equipment and Supplies

    6.1 4 oz round glass jar with a wide mouth screw cap lid.
    6.2 Vacuum oven.
    6.3 50 ml pipettes.
    6.4 A gas chromatograph with an auto sampler and a 50 meter, 0.53 
ID, methyl silicone column with 5 micron phase thickness.
    6.5 Shaker, large enough to hold 10, 4 oz. jars.
    6.6 1000 and 4000 ml volumetric flasks.
    6.7 Electronic integrator or equivalent data system.
    6.8 GC autosampler vials.
    6.9 50 uL syringe.

                       7.0 Reagents and Standards

    7.1 Reagent grade Methyl-Iso-Butyl-Ketone (MIBK)
    7.2 n-heptane, 99% + purity
    7.3 n-hexane, 99% + purity

                          8.0 Sample Collection

    8.1 Trap a sample of the EPDM crumb slurry in the sampling 
apparatus. Allow the crumb slurry to circulate through the sampling 
apparatus for 5 minutes; then close off the values at the bottom and top 
of the sampling apparatus, trapping the crumb slurry. Run cooling water 
through the water jacket for a minimum of 30 minutes. Expel the cooled 
crumb slurry into a sample catching basket. If the crumb does not fall 
by gravity, force it out with demineralized water or nitrogen. Send the 
crumb slurry to the lab for analysis.

                           9.0 Quality Control

    9.1 The Royalene crumb sample is extracted three times with MIBK 
containing an internal standard. The hexane from each extraction is 
added together to obtain a total hexane content. The percent hexane in 
the first extraction is then calculated and used as the recovery factor 
for the analysis.
    9.2 Follow this test method through section 11.4 of the method. 
After removing the sample of the first extraction to be run on the gas 
chromatograph, drain off the remainder of the extraction solvent, 
retaining the crumb sample in the sample jar. Rinse the crumb with 
demineralized water to remove any MIBK left on the surface of the crumb. 
Repeat the extraction procedure with fresh MIBK with internal standard 
two more times.
    9.3 After the third extraction, proceed to section 11.5 of this 
method and obtain the percent hexane in each extraction. Use the sample 
weight obtained in section 12.1 of this method to calculate the percent 
hexane in each of the extracts.
    9.4 Add the percent hexane obtained from the three extractions for a 
total percent hexane in the sample.
    9.5 Use the following equations to determine the recovery factor 
(R):
    % Recovery of the first extraction=(% hexane in the first extract/
total % hexane)x100
    Recovery Factor (R)=(% Hexane Recovered in the first extract)/100

                            10.0 Calibration

    10.1 Preparation of Internal Standard (IS) solution:
    Accuracy weigh 30 grams of n-heptane into a 1000 ml volumetric 
flask. Dilute to the mark with reagent grade MIBK. Label this Solution 
``A''. Pipette 100 mls. of Solution A into a 4 liter volumetric flask. 
Fill the flask to the mark with reagent MIBK. Label this Solution ``B''. 
Solution ``B'' will have a concentration of 0.75 mg/ml of heptane.
    10.2 Preparation of Hexane Standard Solution (HS):
    Using a 50 uL syringe, weigh by difference, 20 mg of n-hexane into a 
50 ml volumetric flask containing approximately 40 ml of Solution B. 
Fill the flask to the mark with Solution B and mix well.
    10.3 Conditions for GC analysis of standards and samples:
    Temperature:
    Initial=40 [deg]C
    Final=150 [deg]C
    Injector=160 [deg]C
    Detector=280 [deg]C
    Program Rate=5.0 [deg]C/min


[[Page 239]]


    Initial Time=5 minutes Final Time=6 minutes
    Flow Rate=5.0 ml/min
    Sensitivity=detector response must be adjusted to keep the hexane 
and IS on scale.
    10.4 Fill an autosampler vial with the HS, analyze it three times 
and calculate a Hexane Relative Response Factor (RF) as follows:

RF=(AIS x CHS x PHS)/(AHS x 
CIS x PIS) (1)

Where:
AIS=Area of IS peak (Heptane)
AHS=Area of peak (Hexane Standard)
CHS=Mg of Hexane/50 ml HS
CIS=Mg of Heptane/50 ml IS Solution B
PIS=Purity of the IS n-heptane
PHS=Purity of the HS n-hexane

                             11.0 Procedure

    11.1 Weight 10 grams of wet crumb into a tared (W1), wide mouth 4 
oz. jar.
    11.2 Pipette 50 ml of Solution B into the jar with the wet crumb 
rubber.
    11.3 Screw the cap on tightly and place it on a shaker for 4 hours.
    11.4 Remove the sample from the shaker and fill an autosampler vial 
with the MIBK extract.
    11.5 Analyze the sample two times.
    11.6 Analyze the HS twice, followed by the samples. Inject the HS 
twice at the end of each 10 samples or at the end of the run.

                            12.0 Calculations

    12.1 Drain off the remainder of the MIBK extract from the polymer in 
the 4 oz. jar. Retain all the polymer in the jar. Place the uncovered 
jar and polymer in a heated vacuum oven until the polymer is dry. 
Reweigh the jar and polymer (W2) and calculate the dried sample weight 
of the polymer as follows:

    Dried SW=W2--W1 (2)

    12.2 Should the polymer be oil extended, pipette 10 ml of the MIBK 
extract into a tared evaporating dish (W1) and evaporate to dryness on a 
steam plate.
    Reweigh the evaporating dish containing the extracted oil (W2). 
Calculate the oil content of the polymer as follows:

    Gram of oil extracted =5 (W2--W1) (3)

% Hexane in polymer=(AsxRFxCISxPIS)/
(AISxSW) (4)
Where:
As=Area of sample hexane sample peak.
AIS=Area of IS peak in sample.
CIS=Concentration of IS in 50 ml.
PIS=Purity of IS.
SW=Weight of dried rubber after extraction. (For oil extended polymer, 
the amount of oil extracted is added to the dry rubber weight).
% Corrected Hexane=(% Hexane in Polymer)/R (5)
R=Recovery factor determined in section 9 of this method.

                         13.0 Method Performance

    13.1 Performance must be determined for each sample type by 
following the procedures in section 9 of this method.

                          14.0 Waste Generation

    14.1 Waste generation should be minimized where possible.

                          15.0 Waste Management

    15.1 All waste shall be handled in accordance with Federal and State 
environmental regulations.

                       16.0 References. [Reserved]

Method 311--Analysis of Hazardous Air Pollutant Compounds in Paints and 
          Coatings by Direct Injection Into a Gas Chromatograph

                        1. Scope and Application

    1.1 Applicability. This method is applicable for determination of 
most compounds designated by the U.S. Environmental Protection Agency as 
volatile hazardous air pollutants (HAP's) (See Reference 1) that are 
contained in paints and coatings. Styrene, ethyl acrylate, and methyl 
methacrylate can be measured by ASTM D 4827-93 or ASTM D 4747-87. 
Formaldehyde can be measured by ASTM PS 9-94 or ASTM D 1979-91. Toluene 
diisocyanate can be measured in urethane prepolymers by ASTM D 3432-89. 
Method 311 applies only to those volatile HAP's which are added to the 
coating when it is manufactured, not to those which may form as the 
coating cures (reaction products or cure volatiles). A separate or 
modified test procedure must be used to measure these reaction products 
or cure volatiles in order to determine the total volatile HAP emissions 
from a coating. Cure volatiles are a significant component of the total 
HAP content of some coatings. The term ``coating'' used in this method 
shall be understood to mean paints and coatings.
    1.2 Principle. The method uses the principle of gas chromatographic 
separation and quantification using a detector that responds to 
concentration differences. Because there are many potential analytical 
systems or sets of operating conditions that may represent useable 
methods for determining the concentrations of the compounds cited in 
Section 1.1 in the applicable matrices, all systems that employ this 
principle, but differ only in details of equipment and operation, may be 
used as alternative methods, provided that the prescribed quality 
control, calibration, and method performance requirements are met. 
Certified product data sheets (CPDS) may also include information 
relevant to the analysis of the coating sample including, but not 
limited to, separation

[[Page 240]]

column, oven temperature, carrier gas, injection port temperature, 
extraction solvent, and internal standard.

                          2. Summary of Method

    Whole coating is added to dimethylformamide and a suitable internal 
standard compound is added. An aliquot of the sample mixture is injected 
onto a chromatographic column containing a stationary phase that 
separates the analytes from each other and from other volatile compounds 
contained in the sample. The concentrations of the analytes are 
determined by comparing the detector responses for the sample to the 
responses obtained using known concentrations of the analytes.

                       3. Definitions. [Reserved]

                            4. Interferences

    4.1 Coating samples of unknown composition may contain the compound 
used as the internal standard. Whether or not this is the case may be 
determined by following the procedures of Section 11 and deleting the 
addition of the internal standard specified in Section 11.5.3. If 
necessary, a different internal standard may be used.
    4.2 The GC column and operating conditions developed for one coating 
formulation may not ensure adequate resolution of target analytes for 
other coating formulations. Some formulations may contain nontarget 
analytes that coelute with target analytes. If there is any doubt about 
the identification or resolution of any gas chromatograph (GC) peak, it 
may be necessary to analyze the sample using a different GC column or 
different GC operating conditions.
    4.3 Cross-contamination may occur whenever high-level and low-level 
samples are analyzed sequentially. The order of sample analyses 
specified in Section 11.7 is designed to minimize this problem.
    4.4 Cross-contamination may also occur if the devices used to 
transfer coating during the sample preparation process or for injecting 
the sample into the GC are not adequately cleaned between uses. All such 
devices should be cleaned with acetone or other suitable solvent and 
checked for plugs or cracks before and after each use.

                                5. Safety

    5.1 Many solvents used in coatings are hazardous. Precautions should 
be taken to avoid unnecessary inhalation and skin or eye contact. This 
method may involve hazardous materials, operations, and equipment. This 
test method does not purport to address all of the safety problems 
associated with its use. It is the responsibility of the user of this 
test method to establish appropriate safety and health practices and to 
determine the applicability of regulatory limitations in regards to the 
performance of this test method.
    5.2 Dimethylformamide is harmful if inhaled or absorbed through the 
skin. The user should obtain relevant health and safety information from 
the manufacturer. Dimethylformamide should be used only with adequate 
ventilation. Avoid contact with skin, eyes, and clothing. In case of 
contact, immediately flush skin or eyes with plenty of water for at 
least 15 minutes. If eyes are affected, consult a physician. Remove and 
wash contaminated clothing before reuse.
    5.3 User's manuals for the gas chromatograph and other related 
equipment should be consulted for specific precautions to be taken 
related to their use.

                        6. Equipment and Supplies

    Note: Certified product data sheets (CPDS) may also include 
information relevant to the analysis of the coating sample including, 
but not limited to, separation column, oven temperature, carrier gas, 
injection port temperature, extraction solvent, and internal standard.

    6.1 Sample Collection.
    6.1.1 Sampling Containers. Dual-seal sampling containers, four to 
eight fluid ounce capacity, should be used to collect the samples. Glass 
sample bottles or plastic containers with volatile organic compound 
(VOC) impermeable walls must be used for corrosive substances (e.g., 
etch primers and certain coating catalysts such as methyl ethyl ketone 
(MEK) peroxide). Sample containers, caps, and inner seal liners must be 
inert to the compounds in the sample and must be selected on a case-by-
case basis.
    6.1.1.1 Other routine sampling supplies needed include waterproof 
marking pens, tubing, scrappers/spatulas, clean rags, paper towels, 
cooler/ice, long handle tongs, and mixing/stirring paddles.
    6.1.2 Personal safety equipment needed includes eye protection, 
respiratory protection, a hard hat, gloves, steel toe shoes, etc.
    6.1.3 Shipping supplies needed include shipping boxes, packing 
material, shipping labels, strapping tape, etc.
    6.1.4 Data recording forms and labels needed include coating data 
sheets and sample can labels.

    Note: The actual requirements will depend upon the conditions 
existing at the source sampled.

    6.2 Laboratory Equipment and Supplies.
    6.2.1 Gas Chromatograph (GC). Any instrument equipped with a flame 
ionization detector and capable of being temperature programmed may be 
used. Optionally, other types of detectors (e.g., a mass spectrometer), 
and any necessary interfaces, may be used provided that the detector 
system

[[Page 241]]

yields an appropriate and reproducible response to the analytes in the 
injected sample. Autosampler injection may be used, if available.
    6.2.2 Recorder. If available, an electronic data station or 
integrator may be used to record the gas chromatogram and associated 
data. If a strip chart recorder is used, it must meet the following 
criteria: A 1 to 10 millivolt (mV) linear response with a full scale 
response time of 2 seconds or less and a maximum noise level of 0.03 percent of full scale. Other types of recorders may 
be used as appropriate to the specific detector installed provided that 
the recorder has a full scale response time of 2 seconds or less and a 
maximum noise level of 0.03 percent of full scale.
    6.2.3 Column. The column must be constructed of materials that do 
not react with components of the sample (e.g., fused silica, stainless 
steel, glass). The column should be of appropriate physical dimensions 
(e.g., length, internal diameter) and contain sufficient suitable 
stationary phase to allow separation of the analytes. DB-5, DB-Wax, and 
FFAP columns are commonly used for paint analysis; however, it is the 
responsibility of each analyst to select appropriate columns and 
stationary phases.
    6.2.4 Tube and Tube Fittings. Supplies to connect the GC and gas 
cylinders.
    6.2.5 Pressure Regulators. Devices used to regulate the pressure 
between gas cylinders and the GC.
    6.2.6 Flow Meter. A device used to determine the carrier gas flow 
rate through the GC. Either a digital flow meter or a soap film bubble 
meter may be used to measure gas flow rates.
    6.2.7 Septa. Seals on the GC injection port through which liquid or 
gas samples can be injected using a syringe.
    6.2.8 Liquid Charging Devices. Devices used to inject samples into 
the GC such as clean and graduated 1, 5, and 10 microliter ([mu]l) 
capacity syringes.
    6.2.9 Vials. Containers that can be sealed with a septum in which 
samples may be prepared or stored. The recommended size is 25 ml 
capacity. Mininert[reg] valves have been found satisfactory and are 
available from Pierce Chemical Company, Rockford, Illinois.
    6.2.10 Balance. Device used to determine the weights of standards 
and samples. An analytical balance capable of accurately weighing to 
0.0001 g is required.

                        7. Reagents and Standards

    7.1 Purity of Reagents. Reagent grade chemicals shall be used in all 
tests. Unless otherwise specified, all reagents shall conform to the 
specifications of the Committee on Analytical Reagents of the American 
Chemical Society, where such specifications are available. Other grades 
may be used provided it is first ascertained that the reagent is of 
sufficient purity to permit its use without lessening the accuracy of 
determination.
    7.2 Carrier Gas. Helium carrier gas shall have a purity of 99.995 
percent or higher. High purity nitrogen may also be used. Other carrier 
gases that are appropriate for the column system and analyte may also be 
used. Ultra-high purity grade hydrogen gas and zero-grade air shall be 
used for the flame ionization detector.
    7.3 Dimethylformamide (DMF). Solvent for all standards and samples. 
Some other suitable solvent may be used if DMF is not compatible with 
the sample or coelutes with a target analyte.

    Note: DMF may coelute with ethylbenzene or p-xylene under the 
conditions described in the note under Section 6.2.3.

    7.4 Internal Standard Materials. The internal standard material is 
used in the quantitation of the analytes for this method. It shall be 
gas chromatography spectrophotometric quality or, if this grade is not 
available, the highest quality available. Obtain the assay for the 
internal standard material and maintain at that purity during use. The 
recommended internal standard material is 1-propanol; however, selection 
of an appropriate internal standard material for the particular coating 
and GC conditions used is the responsibility of each analyst.
    7.5 Reference Standard Materials. The reference standard materials 
are the chemicals cited in Section 1.1 which are of known identity and 
purity and which are used to assist in the identification and 
quantification of the analytes of this method. They shall be the highest 
quality available. Obtain the assays for the reference standard 
materials and maintain at those purities during use.
    7.6 Stock Reference Standards. Stock reference standards are 
dilutions of the reference standard materials that may be used on a 
daily basis to prepare calibration standards, calibration check 
standards, and quality control check standards. Stock reference 
standards may be prepared from the reference standard materials or 
purchased as certified solutions.
    7.6.1 Stock reference standards should be prepared in 
dimethylformamide for each analyte expected in the coating samples to be 
analyzed. The concentrations of analytes in the stock reference 
standards are not specified but must be adequate to prepare the 
calibration standards required in the method. A stock reference standard 
may contain more than one analyte provided all analytes are chemically 
compatible and no analytes coelute. The actual concentrations prepared 
must be known to within 0.1 percent (e.g., 0.1000  
0.0001 g/g solution). The following procedure is suggested. Place about 
35 ml of dimethylformamide into a

[[Page 242]]

tared ground-glass stoppered 50 ml volumetric flask. Weigh the flask to 
the nearest 0.1 mg. Add 12.5 g of the reference standard material and 
reweigh the flask. Dilute to volume with dimethylformamide and reweigh. 
Stopper the flask and mix the contents by inverting the flask several 
times. Calculate the concentration in grams per gram of solution from 
the net gain in weights, correcting for the assayed purity of the 
reference standard material.

    Note: Although a glass-stoppered volumetric flask is convenient, any 
suitable glass container may be used because stock reference standards 
are prepared by weight.

    7.6.2 Transfer the stock reference standard solution into one or 
more Teflon-sealed screw-cap bottles. Store, with minimal headspace, at 
-10 [deg]C to 0 [deg]C and protect from light.
    7.6.3 Prepare fresh stock reference standards every six months, or 
sooner if analysis results from daily calibration check standards 
indicate a problem. Fresh stock reference standards for very volatile 
HAP's may have to be prepared more frequently.
    7.7 Calibration Standards. Calibration standards are used to 
determine the response of the detector to known amounts of reference 
material. Calibration standards must be prepared at a minimum of three 
concentration levels from the stock reference standards (see Section 
7.6). Prepare the calibration standards in dimethylformamide (see 
Section 7.3). The lowest concentration standard should contain a 
concentration of analyte equivalent either to a concentration of no more 
than 0.01% of the analyte in a coating or to a concentration that is 
lower than the actual concentration of the analyte in the coating, 
whichever concentration is higher. The highest concentration standard 
should contain a concentration of analyte equivalent to slightly more 
than the highest concentration expected for the analyte in a coating. 
The remaining calibration standard should contain a concentration of 
analyte roughly at the midpoint of the range defined by the lowest and 
highest concentration calibration standards. The concentration range of 
the standards should thus correspond to the expected range of analyte 
concentrations in the prepared coating samples (see Section 11.5). Each 
calibration standard should contain each analyte for detection by this 
method expected in the actual coating samples (e.g., some or all of the 
compounds listed in Section 1.1 may be included). Each calibration 
standard should also contain an appropriate amount of internal standard 
material (response for the internal standard material is within 25 to 75 
percent of full scale on the attenuation setting for the particular 
reference standard concentration level). Calibration Standards should be 
stored for 1 week only in sealed vials with minimal headspace. If the 
stock reference standards were prepared as specified in Section 7.6, the 
calibration standards may be prepared by either weighing each addition 
of the stock reference standard or by adding known volumes of the stock 
reference standard and calculating the mass of the standard reference 
material added. Alternative 1 (Section 7.7.1) specifies the procedure to 
be followed when the stock reference standard is added by volume. 
Alternative 2 (Section 7.7.2) specifies the procedure to be followed 
when the stock reference standard is added by weight.

    Note: To assist with determining the appropriate amount of internal 
standard to add, as required here and in other sections of this method, 
the analyst may find it advantageous to prepare a curve showing the area 
response versus the amount of internal standard injected into the GC.

    7.7.1 Preparation Alternative 1. Determine the amount of each stock 
reference standard and dimethylformamide solvent needed to prepare 
approximately 25 ml of the specific calibration concentration level 
desired. To a tared 25 ml vial that can be sealed with a crimp-on or 
Mininert[reg] valve, add the total amount of dimethylformamide 
calculated to be needed. As quickly as practical, add the calculated 
amount of each stock reference standard using new pipets (or pipet tips) 
for each stock reference standard. Reweigh the vial and seal it. Using 
the known weights of the standard reference materials per ml in the 
stock reference standards, the volumes added, and the total weight of 
all reagents added to the vial, calculate the weight percent of each 
standard reference material in the calibration standard prepared. Repeat 
this process for each calibration standard to be prepared.
    7.7.2 Preparation Alternative 2. Determine the amount of each stock 
reference standard and dimethylformamide solvent needed to prepare 
approximately 25 ml of the specific calibration concentration level 
desired. To a tared 25 ml vial that can be sealed with a crimp-on or 
Mininert[reg] valve, add the total amount of dimethylformamide 
calculated to be needed. As quickly as practical, add the calculated 
amount of a stock reference standard using a new pipet (or pipet tip) 
and reweigh the vial. Repeat this process for each stock reference 
standard to be added. Seal the vial after obtaining the final weight. 
Using the known weight percents of the standard reference materials in 
the stock reference standards, the weights of the stock reference 
standards added, and the total weight of all reagents added to the vial, 
calculate the weight percent of each standard reference material in the 
calibration standard prepared. Repeat this process for each calibration 
standard to be prepared.

[[Page 243]]

       8. Sample Collection, Preservation, Transport, and Storage

    8.1 Copies of material safety data sheets (MSDS's) for each sample 
should be obtained prior to sampling. The MSDS's contain information on 
the ingredients, and physical and chemical properties data. The MSDS's 
also contain recommendations for proper handling or required safety 
precautions. Certified product data sheets (CPDS) may also include 
information relevant to the analysis of the coating sample including, 
but not limited to, separation column, oven temperature, carrier gas, 
injection port temperature, extraction solvent, and internal standard.
    8.2 A copy of the blender's worksheet can be requested to obtain 
data on the exact coating being sampled. A blank coating data sheet form 
(see Section 18) may also be used. The manufacturer's formulation 
information from the product data sheet should also be obtained.
    8.3 Prior to sample collection, thoroughly mix the coating to ensure 
that a representative, homogeneous sample is obtained. It is preferred 
that this be accomplished using a coating can shaker or similar device; 
however, when necessary, this may be accomplished using mechanical 
agitation or circulation systems.
    8.3.1 Water-thinned coatings tend to incorporate or entrain air 
bubbles if stirred too vigorously; mix these types of coatings slowly 
and only as long as necessary to homogenize.
    8.3.2 Each component of multicomponent coatings that harden when 
mixed must be sampled separately. The component mix ratios must be 
obtained at the facility at the time of sampling and submitted to the 
analytical laboratory.
    8.4 Sample Collection. Samples must be collected in a manner that 
prevents or minimizes loss of volatile components and that does not 
contaminate the coating reservoir. A suggested procedure is as follows. 
Select a sample collection container which has a capacity at least 25 
percent greater than the container in which the sample is to be 
transported. Make sure both sample containers are clean and dry. Using 
clean, long-handled tongs, turn the sample collection container upside 
down and lower it into the coating reservoir. The mouth of the sample 
collection container should be at approximately the midpoint of the 
reservoir (do not take the sample from the top surface). Turn the sample 
collection container over and slowly bring it to the top of the coating 
reservoir. Rapidly pour the collected coating into the sample container, 
filling it completely. It is important to fill the sample container 
completely to avoid any loss of volatiles due to volatilization into the 
headspace. Return any unused coating to the reservoir or dispose as 
appropriate.

    Note: If a company requests a set of samples for its own analysis, a 
separate set of samples, using new sample containers, should be taken at 
the same time.

    8.5 Once the sample is collected, place the sample container on a 
firm surface and insert the inner seal in the container by placing the 
seal inside the rim of the container, inverting a screw cap, and 
pressing down on the screw cap which will evenly force the inner seal 
into the container for a tight fit. Using clean towels or rags, remove 
all residual coating material from the outside of the sample container 
after inserting the inner seal. Screw the cap onto the container.
    8.5.1 Affix a sample label (see Section 18) clearly identifying the 
sample, date collected, and person collecting the sample.
    8.5.2 Prepare the sample for transportation to the laboratory. The 
sample should be maintained at the coating's recommended storage 
temperature specified on the Material Safety Data Sheet, or, if no 
temperature is specified, the sample should be maintained within the 
range of 5 [deg]C to 38 [deg]C.
    8.9 The shipping container should adhere to U.S. Department of 
Transportation specification DOT 12-B. Coating samples are considered 
hazardous materials; appropriate shipping procedures should be followed.

                           9. Quality Control

    9.1 Laboratories using this method should operate a formal quality 
control program. The minimum requirements of the program should consist 
of an initial demonstration of laboratory capability and an ongoing 
analysis of blanks and quality control samples to evaluate and document 
quality data. The laboratory must maintain records to document the 
quality of the data generated. When results indicate atypical method 
performance, a quality control check standard (see Section 9.4) must be 
analyzed to confirm that the measurements were performed in an in-
control mode of operation.
    9.2 Before processing any samples, the analyst must demonstrate, 
through analysis of a reagent blank, that there are no interferences 
from the analytical system, glassware, and reagents that would bias the 
sample analysis results. Each time a set of analytical samples is 
processed or there is a change in reagents, a reagent blank should be 
processed as a safeguard against chronic laboratory contamination. The 
blank samples should be carried through all stages of the sample 
preparation and measurement steps.
    9.3 Required instrument quality control parameters are found in the 
following sections:
    9.3.1 Baseline stability must be demonstrated to be <=5 percent of 
full scale using the procedures given in Section 10.1.

[[Page 244]]

    9.3.2 The GC calibration is not valid unless the retention time (RT) 
for each analyte at each concentration is within 0.05 min of the retention time measured for that analyte 
in the stock standard.
    9.3.3 The retention time (RT) of any sample analyte must be within 
0.05 min of the average RT of the analyte in the 
calibration standards for the analyte to be considered tentatively 
identified.
    9.3.4 The GC system must be calibrated as specified in Section 10.2.
    9.3.5 A one-point daily calibration check must be performed as 
specified in Section 10.3.
    9.4 To establish the ability to generate results having acceptable 
accuracy and precision, the analyst must perform the following 
operations.
    9.4.1 Prepare a quality control check standard (QCCS) containing 
each analyte expected in the coating samples at a concentration expected 
to result in a response between 25 percent and 75 percent of the limits 
of the calibration curve when the sample is prepared as described in 
Section 11.5. The QCCS may be prepared from reference standard materials 
or purchased as certified solutions. If prepared in the laboratory, the 
QCCS must be prepared independently from the calibration standards.
    9.4.2 Analyze three aliquots of the QCCS according to the method 
beginning in Section 11.5.3 and calculate the weight percent of each 
analyte using Equation 1, Section 12.
    9.4.3 Calculate the mean weight percent (X) for each analyte from 
the three results obtained in Section 9.4.2.
    9.4.4 Calculate the percent accuracy for each analyte using the 
known concentrations (Ti) in the QCCS using Equation 3, Section 12.
    9.4.5 Calculate the percent relative standard deviation (percent 
RSD) for each analyte using Equation 7, Section 12, substituting the 
appropriate values for the relative response factors (RRF's) in said 
equation.
    9.4.6 If the percent accuracy (Section 9.4.4) for all analytes is 
within the range 90 percent to 110 percent and the percent RSD (Section 
9.4.5) for all analytes is <=20 percent, system performance is 
acceptable and sample analysis may begin. If these criteria are not met 
for any analyte, then system performance is not acceptable for that 
analyte and the test must be repeated for those analytes only. Repeated 
failures indicate a general problem with the measurement system that 
must be located and corrected. In this case, the entire test, beginning 
at Section 9.4.1, must be repeated after the problem is corrected.
    9.5 Great care must be exercised to maintain the integrity of all 
standards. It is recommended that all standards be stored at -10 [deg]C 
to 0 [deg]C in screw-cap amber glass bottles with Teflon liners.
    9.6 Unless otherwise specified, all weights are to be recorded 
within 0.1 mg.

                  10. Calibration and Standardization.

    10.1 Column Baseline Drift. Before each calibration and series of 
determinations and before the daily calibration check, condition the 
column using procedures developed by the laboratory or as specified by 
the column supplier. Operate the GC at initial (i.e., before sample 
injection) conditions on the lowest attenuation to be used during sample 
analysis. Adjust the recorder pen to zero on the chart and obtain a 
baseline for at least one minute. Initiate the GC operating cycle that 
would be used for sample analysis. On the recorder chart, mark the pen 
position at the end of the simulated sample analysis cycle. Baseline 
drift is defined as the absolute difference in the pen positions at the 
beginning and end of the cycle in the direction perpendicular to the 
chart movement. Calculate the percent baseline drift by dividing the 
baseline drift by the chart width representing full-scale deflection and 
multiply the result by 100.
    10.2 Calibration of GC. Bring all stock standards and calibration 
standards to room temperature while establishing the GC at the 
determined operating conditions.
    10.2.1 Retention Times (RT's) for Individual Compounds.

    Note: The procedures of this subsection are required only for the 
initial calibration. However, it is good laboratory practice to follow 
these procedures for some or all analytes before each calibration. The 
procedures were written for chromatograms output to a strip chart 
recorder. More modern instruments (e.g., integrators and electronic data 
stations) determine and print out or display retention times 
automatically.

    The RT for each analyte should be determined before calibration. 
This provides a positive identification for each peak observed from the 
calibration standards. Inject an appropriate volume (see Note in Section 
11.5.2) of one of the stock reference standards into the gas 
chromatograph and record on the chart the pen position at the time of 
the injection (see Section 7.6.1). Dilute an aliquot of the stock 
reference standard as required in dimethylformamide to achieve a 
concentration that will result in an on-scale response. Operate the gas 
chromatograph according to the determined procedures. Select the peak(s) 
that correspond to the analyte(s) [and internal standard, if used] and 
measure the retention time(s). If a chart recorder is used, measure the 
distance(s) on the chart from the injection point to the peak maxima. 
These distances, divided by the chart speed, are defined as the RT's of 
the analytes in question. Repeat this process for each of the stock 
reference standard solutions.


[[Page 245]]


    Note: If gas chromatography with mass spectrometer detection (GC-MS) 
is used, a stock reference standard may contain a group of analytes, 
provided all analytes are adequately separated during the analysis. Mass 
spectral library matching can be used to identify the analyte associated 
with each peak in the gas chromatogram. The retention time for the 
analyte then becomes the retention time of its peak in the chromatogram.

    10.2.2 Calibration. The GC must be calibrated using a minimum of 
three concentration levels of each potential analyte. (See Section 7.7 
for instructions on preparation of the calibration standards.) Beginning 
with the lowest concentration level calibration standard, carry out the 
analysis procedure as described beginning in Section 11.7. Repeat the 
procedure for each progressively higher concentration level until all 
calibration standards have been analyzed.
    10.2.2.1 Calculate the RT's for the internal standard and for each 
analyte in the calibration standards at each concentration level as 
described in Section 10.2.1. The RT's for the internal standard must not 
vary by more than 0.10 minutes. Identify each analyte by comparison of 
the RT's for peak maxima to the RT's determined in Section 10.2.1.
    10.2.2.2 Compare the retention times (RT's) for each potential 
analyte in the calibration standards for each concentration level to the 
retention times determined in Section 10.2.1. The calibration is not 
valid unless all RT's for all analytes meet the criteria given in 
Section 9.3.2.
    10.2.2.3 Tabulate the area responses and the concentrations for the 
internal standard and each analyte in the calibration standards. 
Calculate the response factor for the internal standard 
(RFis) and the response factor for each compound relative to 
the internal standard (RRF) for each concentration level using Equations 
5 and 6, Section 12.
    10.2.2.4 Using the RRF's from the calibration, calculate the percent 
relative standard deviation (percent RSD) for each analyte in the 
calibration standard using Equation 7, Section 12. The percent RSD for 
each individual calibration analyte must be less than 15 percent. This 
criterion must be met in order for the calibration to be valid. If the 
criterion is met, the mean RRF's determined above are to be used until 
the next calibration.
    10.3 Daily Calibration Checks. The calibration curve (Section 
10.2.2) must be checked and verified at least once each day that samples 
are analyzed. This is accomplished by analyzing a calibration standard 
that is at a concentration near the midpoint of the working range and 
performing the checks in Sections 10.3.1, 10.3.2, and 10.3.3.
    10.3.1 For each analyte in the calibration standard, calculate the 
percent difference in the RRF from the last calibration using Equation 
8, Section 12. If the percent difference for each calibration analyte is 
less than 10 percent, the last calibration curve is assumed to be valid. 
If the percent difference for any analyte is greater than 5 percent, the 
analyst should consider this a warning limit. If the percent difference 
for any one calibration analyte exceeds 10 percent, corrective action 
must be taken. If no source of the problem can be determined after 
corrective action has been taken, a new three-point (minimum) 
calibration must be generated. This criterion must be met before 
quantitative analysis begins.
    10.3.2 If the RFis for the internal standard changes by 
more than 20 percent from the last daily 
calibration check, the system must be inspected for malfunctions and 
corrections made as appropriate.
    10.3.3 The retention times for the internal standard and all 
calibration check analytes must be evaluated. If the retention time for 
the internal standard or for any calibration check analyte changes by 
more than 0.10 min from the last calibration, the system must be 
inspected for malfunctions and corrections made as required.

                              11. Procedure

    11.1 All samples and standards must be allowed to warm to room 
temperature before analysis. Observe the given order of ingredient 
addition to minimize loss of volatiles.
    11.2 Bring the GC system to the determined operating conditions and 
condition the column as described in Section 10.1.

    Note: The temperature of the injection port may be an especially 
critical parameter.Information about the proper temperature may be found 
on the CPDS.

    11.3 Perform the daily calibration checks as described in Section 
10.3. Samples are not to be analyzed until the criteria in Section 10.3 
are met.
    11.4 Place the as-received coating sample on a paint shaker, or 
similar device, and shake the sample for a minimum of 5 minutes to 
achieve homogenization.
    11.5 Note: The steps in this section must be performed rapidly and 
without interruption to avoid loss of volatile organics. These steps 
must be performed in a laboratory hood free from solvent vapors. All 
weights must be recorded to the nearest 0.1 mg.
    11.5.1 Add 16 g of dimethylformamide to each of two tared vials (A 
and B) capable of being septum sealed.
    11.5.2 To each vial add a weight of coating that will result in the 
response for the major constituent being in the upper half of the linear 
range of the calibration curve.

    Note: The magnitude of the response obviously depends on the amount 
of sample injected into the GC as specified in Section 11.8. This volume 
must be the same as used

[[Page 246]]

for preparation of the calibration curve, otherwise shifts in compound 
retention times may occur. If a sample is prepared that results in a 
response outside the limits of the calibration curve, new samples must 
be prepared; changing the volume injected to bring the response within 
the calibration curve limits is not permitted.

    11.5.3 Add a weight of internal standard to each vial (A and B) that 
will result in the response for the internal standard being between 25 
percent and 75 percent of the linear range of the calibration curve.
    11.5.4 Seal the vials with crimp-on or Mininert[reg] septum seals.
    11.6 Shake the vials containing the prepared coating samples for 60 
seconds. Allow the vials to stand undisturbed for ten minutes. If solids 
have not settled out on the bottom after 10 minutes, then centrifuge at 
1,000 rpm for 5 minutes. The analyst also has the option of injecting 
the sample without allowing the solids to settle.
    11.7 Analyses should be conducted in the following order: daily 
calibration check sample, method blank, up to 10 injections from sample 
vials (i.e., one injection each from up to five pairs of vials, which 
corresponds to analysis of 5 coating samples).
    11.8 Inject the prescribed volume of supernatant from the 
calibration check sample, the method blank, and the sample vials onto 
the chromatographic column and record the chromatograms while operating 
the system under the specified operating conditions.
    Note: The analyst has the option of injecting the unseparated 
sample.

                   12. Data Analysis and Calculations

    12.1 Qualitative Analysis. An analyte (e.g., those cited in Section 
1.1) is considered tentatively identified if two criteria are satisfied: 
(1) elution of the sample analyte within 0.05 min 
of the average GC retention time of the same analyte in the calibration 
standard; and (2) either (a) confirmation of the identity of the 
compound by spectral matching on a gas chromatograph equipped with a 
mass selective detector or (b) elution of the sample analyte within 
0.05 min of the average GC retention time of the 
same analyte in the calibration standard analyzed on a dissimilar GC 
column.
    12.1.1 The RT of the sample analyte must meet the criteria specified 
in Section 9.3.3.
    12.1.2 When doubt exists as to the identification of a peak or the 
resolution of two or more components possibly comprising one peak, 
additional confirmatory techniques (listed in Section 12.1) must be 
used.
    12.2 Quantitative Analysis. When an analyte has been identified, the 
quantification of that compound will be based on the internal standard 
technique.
    12.2.1 A single analysis consists of one injection from each of two 
sample vials (A and B) prepared using the same coating. Calculate the 
concentration of each identified analyte in the sample as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.003

    12.2.2 Report results for duplicate analysis (sample vials A and B) 
without correction.
    12.3 Precision Data. Calculate the percent difference between the 
measured concentrations of each analyte in vials A and B as follows.
    12.3.1 Calculate the weight percent of the analyte in each of the 
two sample vials as described in Section 12.2.1.
    12.3.2 Calculate the percent difference for each analyte as:
    [GRAPHIC] [TIFF OMITTED] TR07DE95.004
    

[[Page 247]]


where Ai and Bi are the measured concentrations of 
the analyte in vials A and B.
    12.4 Calculate the percent accuracy for analytes in the QCCS (See 
Section 9.4) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.005

where Xx is the mean measured value and Tx is the 
known true value of the analyte in the QCCS.
    12.5 Obtain retention times (RT's) from data station or integrator 
or, for chromatograms from a chart recorder, calculate the RT's for 
analytes in the calibration standards (See Section 10.2.2.2) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.006

    12.6 Calculate the response factor for the internal standard (See 
Section 10.2.2.3) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.007

where:
    Ais = Area response of the internal standard.
    Cis = Weight percent of the internal standard.
    12.7 Calculate the relative response factors for analytes in the 
calibration standards (See Section 10.2.2.3) as follows:
where:
[GRAPHIC] [TIFF OMITTED] TR07DE95.008

    RRFx = Relative response factor for an individual 
analyte.
    Ax = Area response of the analyte being measured.
    Cx = Weight percent of the analyte being measured.
    12.8 Calculate the percent relative standard deviation of the 
relative response factors for analytes in the calibration standards (See 
Section 10.2.2.4) as follows:
[GRAPHIC] [TIFF OMITTED] TR07DE95.009

    12.9 Calculate the percent difference in the relative response 
factors between the calibration curve and the daily calibration checks 
(See Section 10.3) as follows:

[[Page 248]]

[GRAPHIC] [TIFF OMITTED] TR07DE95.010

    13. Measurement of Reaction Byproducts That are HAP. [Reserved]
    14. Method Performance. [Reserved]
    15. Pollution Prevention. [Reserved]
    16. Waste Management
    16.1 The coating samples and laboratory standards and reagents may 
contain compounds which require management as hazardous waste. It is the 
laboratory's responsibility to ensure all wastes are managed in 
accordance with all applicable laws and regulations.
    16.2 To avoid excessive laboratory waste, obtain only enough sample 
for laboratory analysis.
    16.3 It is recommended that discarded waste coating solids, used 
rags, used paper towels, and other nonglass or nonsharp waste materials 
be placed in a plastic bag before disposal. A separate container, 
designated ``For Sharp Objects Only,'' is recommended for collection of 
discarded glassware and other sharp-edge items used in the laboratory. 
It is recommended that unused or excess samples and reagents be placed 
in a solvent-resistant plastic or metal container with a lid or cover 
designed for flammable liquids. This container should not be stored in 
the area where analytical work is performed. It is recommended that a 
record be kept of all compounds placed in the container for 
identification of the contents upon disposal.

                             17. References

    1. Clean Air Act Amendments, Public Law 101-549, Titles I-XI, 
November, 1990.
    2. Standard Test Method for Water Content of Water-Reducible Paints 
by Direct Injection into a Gas Chromatograph. ASTM Designation D3792-79.
    3. Standard Practice for Sampling Liquid Paints and Related Pigment 
Coatings. ASTM Designation D3925-81.
    4. Standard Test Method for Determination of Dichloromethane and 
1,1,1-Trichloroethane in Paints and Coatings by Direct Injection into a 
Gas Chromatograph. ASTM Designation D4457-85.
    5. Standard Test Method for Determining the Unreacted Monomer 
Content of Latexes Using Capillary Column Gas Chromatography. ASTM 
Designation D4827-93.
    6. Standard Test Method for Determining Unreacted Monomer Content of 
Latexes Using Gas-Liquid Chromatography. ASTM Designation D 4747-87.
    7. Method 301--``Field Validation of Pollutant Measurement Methods 
from Various Waste Media,'' 40 CFR 63, Appendix A.
    8. ``Reagent Chemicals, American Chemical Society Specifications,'' 
American Chemical Society, Washington, DC. For suggestions on the 
testing of reagents not listed by the American Chemical Society, see 
``Reagent Chemicals and Standards'' by Joseph Rosin, D. Van Nostrand 
Co., Inc., New York, NY and the ``United States Pharmacopeia.''

          18. Tables, Diagrams, Flowcharts, and Validation Data

Agency:_________________________________________________________________
Inspector:______________________________________________________________
Date/Time:______________________________________________________________
Sample ID:_____________________________________________________
Source ID:______________________________________________________________
Coating Name/Type:______________________________________________________
Plant Witness:__________________________________________________________
Type Analysis Required:_________________________________________________
Special Handling:_______________________________________________________

                         Sample Container Label

                              Coating Data

Date:___________________________________________________________________

Source:_________________________________________________________________

------------------------------------------------------------------------
                  Data                     Sample ID No.   Sample ID No.
------------------------------------------------------------------------
Coating:
    Supplier Name.......................  ..............  ..............
    Name and Color of Coating...........  ..............  ..............
    Type of Coating (primer, clearcoat,   ..............  ..............
     etc.)..............................
    Identification Number for Coating...  ..............  ..............
    Coating Density (lbs/gal)...........  ..............  ..............

[[Page 249]]

 
    Total Volatiles Content (wt percent)  ..............  ..............
    Water Content (wt percent)..........  ..............  ..............
    Exempt Solvents Content (wt percent)  ..............  ..............
    VOC Content (wt percent)............  ..............  ..............
    Solids Content (vol percent)........  ..............  ..............
Diluent Properties:
    Name................................
    Identification Number...............  ..............  ..............
    Diluent Solvent Density (lbs/gal)...  ..............  ..............
    VOC Content (wt percent)............  ..............  ..............
    Water Content (wt percent)..........  ..............  ..............
    Exempt Solvent Content (wt percent).  ..............  ..............
    Diluent/Solvent Ratio (gal diluent    ..............  ..............
     solvent/gal coating)...............
------------------------------------------------------------------------

                        Stock Reference Standard

Name of Reference Material:_____________________________________________

Supplier Name:__________________________________________________________

Lot Number:_____________________________________________________________

Purity:_________________________________________________________________

Name of Solvent Material: Dimethylformamide_____________________________

Supplier Name:__________________________________________________________

Lot Number:_____________________________________________________________

Purity:_________________________________________________________________

Date Prepared:__________________________________________________________

Prepared By:____________________________________________________________

Notebook/page no.:______________________________________________________

                         Preparation Information
1. Weight Empty Flask..................  --------,g
2. Weight Plus DMF.....................  --------,g
3. Weight Plus Reference Material......  --------,g
4. Weight After Made to Volume.........  --------,g
5. Weight DMF (lines 2-1+3-4)..........  --------,g
6. Weight Ref. Material (lines 3-2)....  --------,g
7. Corrected Weight of Reference         --------,g
 Material (line 6 times purity).
8. Fraction Reference Material in        --------,g/g
 Standard (Line 7 / Line 5) soln.
9. Total Volume of Standard Solution...  --------, ml
10. Weight Reference Material per ml of  --------,g/ml
 Solution (Line 7 / Line 9).
Laboratory ID No. for this Standard....  --------
Expiration Date for this Standard......  --------
 

                          CALIBRATION STANDARD

Date Prepared:__________________________________________________________

Date Expires:___________________________________________________________

Prepared By:____________________________________________________________

Notebook/page:__________________________________________________________
Calibration Standard Identification No.:
________________________________________________________________________

                         Preparation Information
Final Weight Flask Plus Reagents.......  --------, g
Weight Empty Flask.....................  --------, g
Total Weight Of Reagents...............  --------, g
 


--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                               Amount of stock reference standard added (by
                                                                  Stock                    volume or by weight)                  Calculated     Weight
                                                                reference  ----------------------------------------------------    weight      percent
                        Analyte name a                         standard ID                Amount in                 Amount in     analyte     analyte in
                                                                   No.         Volume    standard, g/    Weight    standard, g/   added, g   calibration
                                                                             added, ml        ml        added, g      g soln                  standard b
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------
a Include internal standard(s).
b Weight percent = weight analyte added / total weight of reagents.


[[Page 250]]

                     Quality Control Check Standard

Date Prepared:__________________________________________________________

Date Expires:___________________________________________________________

Prepared By:____________________________________________________________

Notebook/page:__________________________________________________________

Quality Control Check Standard Identification No.:
________________________________________________________________________

                         Preparation Information
Final Weight Flask Plus Reagents.......  --------,g
Weight Empty Flask.....................  --------,g
Total Weight Of Reagents...............  --------,g
 


--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                               Amount of stock reference standard added (by
                                                                  Stock                    volume or by weight)                  Calculated     Weight
                                                                reference  ----------------------------------------------------    weight      percent
                        Analyte name a                         standard ID                Amount in                 Amount in     analyte     analyte in
                                                                   No.         Volume    standard, g/    Weight    standard, g/   added, g       QCC
                                                                             added, ml        ml        added, g      g soln                  standard b
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
                                                               ...........  ...........  ...........  ...........  ...........  ...........  ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------
a Include internal Standard(s).
b Weight percent=weight analyte added / total weight of reagents.

                 Quality Control Check Standard Analysis

Date OCCS Analyzed:_____________________________________________________

OCCS Identification No._________________________________________________

Analyst:________________________________________________________________

QCC Expiration Date:____________________________________________________

                                                                    Analysis Results
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                     Weight percent determined                                        Meets criteria in
                                                                 ---------------------------------                                      Section 9.4.6
                             Analyte                                                                Mean Wt    Percent    Percent  ---------------------
                                                                    Run 1      Run 2      Run 3     percent    accuracx     RSD      Percent    Percent
                                                                                                                                     accuracy     RSD
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
                                                                  .........  .........  .........  .........  .........  .........  .........  .........
--------------------------------------------------------------------------------------------------------------------------------------------------------

                    Calibration of Gas Chromatograph

Calibration Date:_______________________________________________________

Calibrated By:__________________________________________________________

                                                     Part 1--Retention Times for Individual Analytes
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                               Recorder chart speed        Distance from injection point
                                                               Stock     --------------------------------         to peak maximum            Retention
                         Analyte                           standard. ID                                  --------------------------------  time, minutes
                                                                No.         Inches/min.       cm/min.         Inches        Centimeters          a
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
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a Retention time=distance to peak maxima/chart speed.

                    CALIBRATION OF GAS CHROMATOGRAPH

Calibration Date:_______________________________________________________

Calibrated By:__________________________________________________________

                                    Part 2--Analysis of Calibration Standards
----------------------------------------------------------------------------------------------------------------
                                                                   Calib. STD ID   Calib. STD ID   Calib. STD ID
                             Analyte                                    No.             No.             No.
----------------------------------------------------------------------------------------------------------------
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
Internal Standard Name:
    Conc. in STD................................................  ..............  ..............  ..............
    Area Response...............................................  ..............  ..............  ..............
    RT..........................................................  ..............  ..............  ..............
----------------------------------------------------------------------------------------------------------------

                    Calibration of Gas Chromatograph

Calibration Date:_______________________________________________________

Calibrated By:__________________________________________________________

                                                     Part 3--Data Analysis for Calibration Standards
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                        Is RT within 0.05   Is percent
                       Analyte                             ID           ID           ID          Mean        of RF     min of RT for stock?  RSD <30% (Y/
                                                                                                                               (Y/N)              N)
--------------------------------------------------------------------------------------------------------------------------------------------------------
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........

[[Page 252]]

 
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
Name:
    RT..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
    RF..............................................  ...........  ...........  ...........  ...........  ...........  ....................  ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------

                         Daily Calibration Check

Date:___________________________________________________________________

Analyst:________________________________________________________________
Calibration Check Standard ID No.:

Expiration Date:________________________________________________________

--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Retention Time (RT)                            Response Factor (RF)
                         Analyte                         -----------------------------------------------------------------------------------------------
                                                               Last            This        Difference a        Last            This        Difference b
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
--------------------------------------------------------------------------------------------------------------------------------------------------------
a Retention time (RT) change (difference) must be less than 0.10 minutes.
b Response factor (RF) change (difference) must be less than 20 percent for each analyte and for the internal standard.

                             Sample Analysis

Vial A ID No.:__________________________________________________________

Vial B ID No.:__________________________________________________________

Analyzed By:____________________________________________________________

Date:___________________________________________________________________


----------------------------------------------------------------------------------------------------------------
                      Sample preparation information                            Vial A (g)         Vial B (g)
----------------------------------------------------------------------------------------------------------------
Measured:
    wt empty vial.........................................................  .................  .................
    wt plus DMF...........................................................  .................  .................
    wt plus sample........................................................  .................  .................
    wt plus internal......................................................  .................  .................
    standard..............................................................  .................  .................
Calculated:
    wt DMF................................................................  .................  .................
    wt sample.............................................................  .................  .................
    wt internal standard..................................................  .................  .................
----------------------------------------------------------------------------------------------------------------


                                                           Analysis Results: Duplicate Samples
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                   Area response                                       Wt percent in sample
                         Analyte                         --------------------------------       RF       -----------------------------------------------
                                                              Vial A          Vial B                          Vial A          Vial B          Average
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                          ..............  ..............  ..............  ..............  ..............  ..............

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                                                          ..............  ..............  ..............  ..............  ..............  ..............
                                                          ..............  ..............  ..............  ..............  ..............  ..............
Internal Standard.......................................  ..............  ..............  ..............  ..............  ..............  ..............
--------------------------------------------------------------------------------------------------------------------------------------------------------

Method 312A--Determination of Styrene in Latex Styrene-Butadiene Rubber, 
                       Through Gas Chromatography

                        1. Scope and Application

    1.1 This method describes a procedure for determining parts per 
million (ppm) styrene monomer (CAS No. 100-42-5) in aqueous samples, 
including latex samples and styrene stripper water.
    1.2 The sample is separated in a gas chromatograph equipped with a 
packed column and a flame ionization detector.

                          2.0 Summary of Method

    2.1 This method utilizes a packed column gas chromatograph with a 
flame ionization detector to determine the concentration of residual 
styrene in styrene butadiene rubber (SBR) latex samples.

                             3.0 Definitions

    3.1 The definitions are included in the text as needed.

                            4.0 Interferences

    4.1 In order to reduce matrix effects and emulsify the styrene, 
similar styrene free latex is added to the internal standard. There are 
no known interferences.
    4.2 The operating parameters are selected to obtain resolution 
necessary to determine styrene monomer concentrations in latex.

                               5.0 Safety

    5.1 It is the responsibility of the user of this procedure to 
establish appropriate safety and health practices.

                       6.0 Equipment and Supplies

    6.1 Adjustable bottle-top dispenser, set to deliver 3 ml. (for 
internal standard), Brinkmann Dispensette, or equivalent.
    6.2 Pipettor, set to 10 ml., Oxford Macro-set, or equivalent.
    6.3 Volumetric flask, 100-ml, with stopper.
    6.4 Hewlett Packard Model 5710A dual channel gas chromatograph 
equipped with flame ionization detector.
    6.4.1 11 ft. x \1/8\ in. stainless steel column packed with 10% TCEP 
on 100/120 mesh Chromosorb P, or equivalent.
    6.4.2 Perkin Elmer Model 023 strip chart recorder, or equivalent.
    6.5 Helium carrier gas, zero grade.
    6.6 Liquid syringe, 25-[mu]l.
    6.7 Digital MicroVAX 3100 computer with VG Multichrom software, or 
equivalent data handling system.
    6.6 Wire Screens, circular, 70-mm, 80-mesh diamond weave.
    6.7 DEHA--(N,N-Diethyl hydroxylamine), 97+% purity, CAS No. 3710-84-
7
    6.8 p-Dioxane, CAS No. 123-91-1

                       7.0 Reagents and Standards

    7.1 Internal standard preparation.
    7.1.1 Pipette 5 ml p-dioxane into a 1000-ml volumetric flask and 
fill to the mark with distilled water and mix thoroughly.
    7.2 Calibration solution preparation.
    7.2.1 Pipette 10 ml styrene-free latex (eg: NBR latex) into a 100-ml 
volumetric flask.
    7.2.2 Add 3 ml internal standard (section 7.1.1 of this method).
    7.2.3 Weigh exactly 10[mu]l fresh styrene and record the weight.
    7.2.4 Inject the styrene into the flask and mix well.
    7.2.5 Add 2 drops of DEHA, fill to the mark with water and mix well 
again.
    7.2.6 Calculate concentration of the calibration solution as 
follows:

    mg/l styrene=(mg styrene added)/0.1 L

            8.0 Sample Collection, Preservation, and Storage

    8.1 A representative SBR emulsion sample should be caught in a 
clean, dry 6-oz. teflon lined glass container. Close it properly to 
assure no sample leakage.
    8.2 The container should be labeled with sample identification, date 
and time.

[[Page 254]]

                           9.0 Quality Control

    9.1 The instrument is calibrated by injecting calibration solution 
(Section 7.2 of this method) five times.
    9.2 The retention time for components of interest and relative 
response of monomer to the internal standard is determined.
    9.3 Recovery efficiency must be determined once for each sample type 
and whenever modifications are made to the method.
    9.3.1 A set of six latex samples shall be collected. Two samples 
shall be prepared for analysis from each sample. Each sample shall be 
analyzed in duplicate.
    9.3.2 The second set of six latex samples shall be analyzed in 
duplicate before spiking each sample with approximately 1000 ppm 
styrene. The spiked samples shall be analyzed in duplicate.
    9.3.3 For each hydrocarbon, calculate the average recovery 
efficiency (R) using the following equations:

where:
R=[Sigma](Rn)/6

where:
Rn=(cns-cv)/Sn

n=sample number
cns=concentration of compound measured in spiked sample 
number n.
cnu= concentration of compound measured in unspiked sample 
number n.
Sn=theoretical concentration of compound spiked into sample 
n.
    9.3.4 A value of R between 0.70 and 1.30 is acceptable.
    9.3.5 R is used to correct all reported results for each compound by 
dividing the measured results of each compound by the R for that 
compound for the same sample type.

                10.0 Calibration and Instrument Settings

    10.1 Injection port temperature, 250 [deg]C.
    10.2 Oven temperature, 110 [deg]C, isothermal.
    10.3 Carrier gas flow, 25 cc/min.
    10.4 Detector temperature, 250 [deg]C.
    10.5 Range, 1X.

                             11.0 Procedure

    11.1 Turn on recorder and adjust baseline to zero.
    11.2 Prepare sample.
    11.2.1 For latex samples, add 3 ml Internal Standard (section 7.1 of 
this method) to a 100-ml volumetric flask. Pipet 10 ml sample into the 
flask using the Oxford pipettor, dilute to the 100-ml mark with water, 
and shake well.
    11.2.2 For water samples, add 3 ml Internal Standard (section 7.1 of 
this method) to a 100-ml volumetric flask and fill to the mark with 
sample. Shake well.
    11.3 Flush syringe with sample.
    11.4 Carefully inject 2 [mu]l of sample into the gas chromatograph 
column injection port and press the start button.
    11.5 When the run is complete the computer will print a report of 
the analysis.

                   12.0 Data Analysis and Calculation

    12.1 For samples that are prepared as in section 11.2.1 of this 
method:

ppm styrene = AxD

Where:
A = ``ppm'' readout from computer
D = dilution factor (10 for latex samples)

    12.2 For samples that are prepared as in section 11.2.2 of this 
method, ppm styrene is read directly from the computer.

                         13.0 Method Performance

    13.1 This test has a standard deviation (1) of 3.3 ppm at 100 ppm 
styrene. The average Spike Recovery from six samples at 1000 ppm Styrene 
was 96.7 percent. The test method was validated using 926 ppm styrene 
standard. Six analysis of the same standard provided average 97.7 
percent recovery. Note: These are example recoveries and do not replace 
quality assurance procedures in this method.

                        14.0 Pollution Prevention

    14.1 Waste generation should be minimized where possible. Sample 
size should be an amount necessary to adequately run the analysis.

                          15.0 Waste Management

    15.1 All waste shall be handled in accordance with Federal and State 
environmental regulations.

                    16.0 References and Publications

    16.1 40 CFR 63 Appendix A--Method 301 Test Methods Field Validation 
of Pollutant Measurement
    16.2 DSM Copolymer Test Method T-3060, dated October 19, 1995, 
entitled: Determination of Residual Styrene in Latex, Leonard, C.D., 
Vora, N.M.et al

  Method 312B--Determination of Residual Styrene in Styrene-Butadiene 
           (SBR) Rubber Latex by Capillary Gas Chromatography

                                1.0 Scope

    1.1 This method is applicable to SBR latex solutions.
    1.2 This method quantitatively determines residual styrene 
concentrations in SBR latex solutions at levels from 80 to 1200 ppm.

                         2.0 Principle of Method

    2.1 A weighed sample of a latex solution is coagulated with an ethyl 
alcohol (EtOH) solution containing a specific amount of alpha-methyl 
styrene (AMS) as the internal standard. The extract of this coagulation 
is then

[[Page 255]]

injected into a gas chromatograph and separated into individual 
components. Quantification is achieved by the method of internal 
standardization.

                             3.0 Definitions

    3.1 The definitions are included in the text as needed.

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 This method may involve hazardous materials, operations, and 
equipment. This method does not purport to address all of the safety 
problems associated with its use. It is the responsibility of the user 
of this method to establish appropriate safety and health practices and 
determine the applicability of regulatory limitations prior to use.

                       6.0 Equipment and Supplies

    6.1 Analytical balance, 160 g capacity, and 0.1 mg resolution
    6.2 Bottles, 2-oz capacity, with poly-cap screw lids
    6.3 Mechanical shaker
    6.4 Syringe, 10-ul capacity
    6.5 Gas chromatograph, Hewlett Packard model 5890A, or equivalent, 
configured with FID with a megabore jet, splitless injector packed with 
silanized glass wool.
    6.5.1 Establish the following gas chromatographic conditions, and 
allow the system to thoroughly equilibrate before use.

    Injection technique = Splitless
    Injector temperature = 225 deg C
    Oven temperature = 70 deg C (isothermal)
    Detector: temperature = 300 deg C
    range = 5
    attenuation = 0
    Carrier gas: helium = 47 ml/min
    Detector gases: hydrogen = 30 ml/min
    air = 270 ml/min
    make-up = 0 ml/min
    Analysis time: = 3.2 min at the specified carrier gas flow rate and 
column temperature.
    6.6 Gas chromatographic column, DB-1, 30 M X 0.53 ID, or equivalent, 
with a 1.5 micron film thickness.
    6.7 Data collection system, Perkin-Elmer/Nelson Series Turbochrom 4 
Series 900 Interface, or equivalent.
    6.8 Pipet, automatic dispensing, 50-ml capacity, and 2-liter 
reservoir.
    6.9 Flasks, volumetric, class A, 100-ml and 1000-ml capacity.
    6.10 Pipet, volumetric delivery, 10-ml capacity, class A.

                       7.0 Chemicals and Reagents

    CHEMICALS:
7.1 Styrene, C8H8, 99+%, CAS 100-42-5
7.2 Alpha methyl styrene, C9H10, 99%, CAS 98-83-9
7.3 Ethyl alcohol, C2H5OH, denatured formula 2B, CAS 64-17-5

    REAGENTS:
    7.4 Internal Standard Stock Solution: 5.0 mg/ml AMS in ethyl 
alcohol.
    7.4.1 Into a 100-ml volumetric flask, weigh 0.50 g of AMS to the 
nearest 0.1 mg.
    7.4.2 Dilute to the mark with ethyl alcohol. This solution will 
contain 5.0 mg/ml AMS in ethyl alcohol and will be labeled the AMS STOCK 
SOLUTION.
    7.5 Internal Standard Working Solution: 2500 ug/50 ml of AMS in 
ethyl alcohol.
    7.5.1 Using a 10 ml volumetric pipet, quantitatively transfer 10.0 
ml of the AMS STOCK SOLUTION into a 1000-ml volumetric flask.
    7.5.2 Dilute to the mark with ethyl alcohol. This solution will 
contain 2500 ug/50ml of AMS in ethyl alcohol and will be labeled the AMS 
WORKING SOLUTION.
    7.5.3 Transfer the AMS WORKING SOLUTION to the automatic dispensing 
pipet reservoir.
    7.6 Styrene Stock Solution: 5.0 mg/ml styrene in ethyl alcohol.
    7.6.1 Into a 100-ml volumetric flask, weigh 0.50 g of styrene to the 
nearest 0.1 mg.
    7.6.2 Dilute to the mark with ethyl alcohol. This solution will 
contain 5.0 mg/ml styrene in ethyl alcohol and will be labeled the 
STYRENE STOCK SOLUTION.
    7.7 Styrene Working Solution: 5000 ug/10 ml of styrene in ethyl 
alcohol.
    7.7.1 Using a 10-ml volumetric pipet, quantitatively transfer 10.0 
ml of the STYRENE STOCK SOLUTION into a 100-ml volumetric flask.
    7.7.2 Dilute to the mark with ethyl alcohol. This solution will 
contain 5000 ug/10 ml of styrene in ethyl alcohol and will be labeled 
the STYRENE WORKING SOLUTION.

             8.0 Sample Collection, Preservation and Storage

    8.1 Label a 2-oz sample poly-cap lid with the identity, date and 
time of the sample to be obtained.
    8.2 At the sample location, open sample valve for at least 15 
seconds to ensure that the sampling pipe has been properly flushed with 
fresh sample.
    8.3 Fill the sample jar to the top (no headspace) with sample, then 
cap it tightly.
    8.4 Deliver sample to the Laboratory for testing within one hour of 
sampling.
    8.5 Laboratory testing will be done within two hours of the sampling 
time.
    8.6 No special storage conditions are required unless the storage 
time exceeds 2 hours in which case refrigeration of the sample is 
recommended.

                           9.0 Quality Control

    9.1 For each sample type, 12 samples of SBR latex shall be obtained 
from the process

[[Page 256]]

for the recovery study. Half the vials and caps shall be tared, labeled 
``spiked'', and numbered 1 through 6. The other vials are labeled 
``unspiked'' and need not be tared, but are also numbered 1 through 6.
    9.2 The six vials labeled ``spiked'' shall be spiked with an amount 
of styrene to approximate 50% of the solution's expected residual 
styrene level.
    9.3 The spiked samples shall be shaken for several hours and allowed 
to cool to room temperature before analysis.
    9.4 The six samples of unspiked solution shall be coagulated and a 
mean styrene value shall be determined, along with the standard 
deviation, and the percent relative standard deviation.
    9.5 The six samples of the spiked solution shall be coagulated and 
the results of the analyses shall be determined using the following 
equations:

Mr=Ms-Mu
R=Mr/S

where:
Mu=Mean value of styrene in the unspiked sample
Ms=Measured amount of styrene in the spiked sample
Mr=Measured amount of the spiked compound
S=Amount of styrene added to the spiked sample
R=Fraction of spiked styrene recovered

    9.6 A value of R between 0.70 and 1.30 is acceptable.
    9.7 R is used to correct all reported results for each compound by 
dividing the measured results of each compound by the R for that 
compound for the same sample type.

                            10.0 Calibration

    10.1 Using a 10-ml volumetric pipet, quantitatively transfer 10.0 ml 
of the STYRENE WORKING SOLUTION (section 7.7.2 of this method) into a 2-
oz bottle.
    10.2 Using the AMS WORKING SOLUTION equipped with the automatic 
dispensing pipet (section 7.5.3 of this method), transfer 50.0 ml of the 
internal standard solution into the 2-oz bottle.
    10.3 Cap the 2-oz bottle and swirl. This is the calibration 
standard, which contains 5000 [mu]g of styrene and 2500 [mu]g of AMS.
    10.4 Using the conditions prescribed (section 6.5 of this method), 
chromatograph 1 [mu]l of the calibration standard.
    10.5 Obtain the peak areas and calculate the relative response 
factor as described in the calculations section (section 12.1 of this 
method).

                             11.0 Procedure

    11.1 Into a tared 2-oz bottle, weigh 10.0 g of latex to the nearest 
0.1 g.
    11.2 Using the AMS WORKING SOLUTION equipped with the automatic 
dispensing pipet (section 7.5.3 of this method), transfer 50.0 ml of the 
internal standard solution into the 2-oz bottle.
    11.3 Cap the bottle. Using a mechanical shaker, shake the bottle for 
at least one minute or until coagulation of the latex is complete as 
indicated by a clear solvent.
    11.4 Using the conditions prescribed (section 6.5 of this method), 
chromatograph 1 ul of the liquor.
    11.5 Obtain the peak areas and calculate the concentration of 
styrene in the latex as described in the calculations section (Section 
12.2 of this method).

                            12.0 Calculations

    12.1 Calibration:

RF=(WxxAis) / (WisxAx)

where:
RF=the relative response factor for styrene
Wx=the weight (ug) of styrene
Ais=the area of AMS
Wis=the weight (ug) of AMS
Ax=the area of styrene
12.2 Procedure:

ppmstyrene=(Ax RFxWis) / 
(AisxWs)

where:
ppmstyrene=parts per million of styrene in the latex
Ax=the area of styrene
RF=the response factor for styrene
Wis=the weight (ug) of AMS
Ais=the area of AMS
Ws=the weight (g) of the latex sample
12.3 Correct for recovery (R) as determined by section 9.0 of this 
method.

                             13.0 Precision

    13.1 Precision for the method was determined at the 80, 144, 590, 
and 1160 ppm levels. The standard deviations were 0.8, 1.5, 5 and 9 ppm 
respectively. The percent relative standard deviations (%RSD) were 1% or 
less at all levels. Five degrees of freedom were used for all precision 
data except at the 80 ppm level, where nine degrees of freedom were 
used. Note: These are example results and do not replace quality 
assurance procedures in this method.

                        14.0 Pollution Prevention

    14.1 Waste generation should be minimized where possible. Sample 
size should be an amount necessary to adequately run the analysis.

                          15.0 Waste Management

    15.1 Discard liquid chemical waste into the chemical waste drum.
    15.2 Discard latex sample waste into the latex waste drum.
    15.3 Discard polymer waste into the polymer waste container.

[[Page 257]]

                             16.0 References

    16.1 This method is based on Goodyear Chemical Division Test Method 
E-889.

Method 312C--Determination of Residual Styrene in SBR Latex Produced by 
                         Emulsion Polymerization

                                1.0 Scope

    1.1 This method is applicable for determining the amount of residual 
styrene in SBR latex as produced in the emulsion polymerization process.

                         2.0 Principle of Method

    2.1 A weighed sample of latex is coagulated in 2-propanol which 
contains alpha-methyl styrene as an Internal Standard. The extract from 
the coagulation will contain the alpha-methyl styrene as the Internal 
Standard and the residual styrene from the latex. The extract is 
analyzed by a Gas Chromatograph. Percent styrene is calculated by 
relating the area of the styrene peak to the area of the Internal 
Standard peak of known concentration.

                             3.0 Definitions

    3.1 The definitions are included in the text as needed.

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 When using solvents, avoid contact with skin and eyes. Wear hand 
and eye protection. Wash thoroughly after use.
    5.2 Avoid overexposure to solvent vapors. Handle only in well 
ventilated areas.

                       6.0 Equipment and Supplies

    6.1 Gas Chromatograph--Hewlett Packard 5890, Series II with flame 
ionization detector, or equivalent.
    Column--HP 19095F-123, 30m x 0.53mm, or equivalent. Substrate HP 
FFAP (cross-linked) film thickness 1 micrometer. Glass injector port 
liners with silanized glass wool plug.
    Integrator--HP 3396, Series II, or equivalent.
    6.2 Wrist action shaker
    6.3 Automatic dispenser
    6.4 Automatic pipet, calibrated to deliver 5.0 0.01 grams of latex
    6.5 Four-ounce wide-mouth bottles with foil lined lids
    6.6 Crimp cap vials, 2ml, teflon lined septa
    6.7 Disposable pipets
    6.8 Qualitative filter paper
    6.9 Cap crimper
    6.10 Analytical balance
    6.11 10ml pipette
    6.12 Two-inch funnel

                       7.0 Reagents and Standards

    7.1 2-Propanol (HP2C grade)
    7.2 Alpha methyl styrene (99+% purity)
    7.3 Styrene (99+% purity)
    7.4 Zero air
    7.5 Hydrogen (chromatographic grade)
    7.6 Helium
    7.7 Internal Standard preparation
    7.7.1 Weigh 5.000-5.005 grams of alpha-methyl styrene into a 100ml 
volumetric flask and bring to mark with 2-propanol to make Stock ``A'' 
Solution.

    Note: Shelf life--6 months.

    7.7.2 Pipette 10ml of Stock ``A'' Solution into a 100ml volumetric 
flask and bring to mark with 2-propanol to prepare Stock ``B'' Solution.
    7.7.3 Pipette 10ml of the Stock ``B'' solution to a 1000ml 
volumetric flask and bring to the mark with 2-propanol. This will be the 
Internal Standard Solution (0.00005 grams/ml).
    7.8 Certification of Internal Standard--Each batch of Stock ``B'' 
Solution will be certified to confirm concentration.
    7.8.1 Prepare a Standard Styrene Control Solution in 2-propanol by 
the following method:
    7.8.1.1 Weigh 5.000 .005g of styrene to a 
100ml volumetric flask and fill to mark with 2-propanol to make Styrene 
Stock ``A'' Solution.
    7.8.1.2 Pipette 10ml of Styrene Stock ``A'' Solution to a 100ml 
volumetric flask and fill to mark with 2-propanol to make Styrene Stock 
``B'' Solution.
    7.8.1.3 Pipette 10ml of Styrene Stock ``B'' soluion to a 250ml 
volumtric flask and fill to mark wtih 2-propanol to make the 
Certification Solution.
    7.8.2 Certify Alpha-Methyl Styrene Stock ``B'' Solution.
    7.8.2.1 Pipette 5ml of the Certification Solution and 25ml of the 
Alpha Methyl Styrene Internal Standard Solution to a 4-oz. bottle, cap 
and shake well.
    7.8.2.2 Analyze the resulting mixture by GC using the residual 
styrene method. (11.4-11.6 of this method)
    7.8.2.3 Calculate the weight of alpha methyl styrene present in the 
25ml aliquat of the new Alpha Methyl Styrene Standard by the following 
equation:

Wx = Fx xWis(Ax/
Ais)

Where
Ax = Peak area of alpha methyl styrene
Ais = Peak area of styrene
Wx = Weight of alpha methyl styrene
Wis = Weight of styrene (.00100)
Fx = Analyzed response factor = 1

    The Alpha Methyl Styrene Stock Solution used to prepare the Internal 
Standard Solution may be considered certified if the weight of alpha 
methyl styrene analyzed by

[[Page 258]]

this method is within the range of .00121g to .00129g.

                              8.0 Sampling

    8.1 Collect a latex sample in a capped container. Cap the bottle and 
identify the sample as to location and time.
    8.2 Deliver sample to Laboratory for testing within one hour.
    8.3 Laboratory will test within two hours.
    8.4 No special storage conditions are required.

                           9.0 Quality Control

    9.1 The laboratory is required to operate a formal quality control 
program. This consists of an initial demonstration of the capability of 
the method as well as ongoing analysis of standards, blanks, and spiked 
samples to demonstrate continued performance.
    9.1.1 When the method is first set up, a calibration is run and the 
recovery efficiency for each type of sample must be determined.
    9.1.2 If new types of samples are being analyzed, then recovery 
efficiency for each new type of sample must be determined. New type 
includes any change, such as polymer type, physical form or a 
significant change in the composition of the matrix.
    9.2 Recovery efficiency must be determined once for each sample type 
and whenever modifications are made to the method.
    9.2.1 In determining the recovery efficiency, the quadruplet 
sampling system shall be used. Six sets of samples (for a total of 24) 
shall be taken. In each quadruplet set, half of the samples (two out of 
the four) shall be spiked with styrene.
    9.2.2 Prepare the samples as described in section 8 of this method. 
To the vials labeled ``spiked'', add a known amount of styrene that is 
expected to be present in the latex.
    9.2.3 Run the spiked and unspiked samples in the normal manner. 
Record the concentrations of styrene reported for each pair of spiked 
and unspiked samples with the same vial number.
    9.2.4 For each hydrocarbon, calculate the average recovery 
efficiency (R) using the following equation:

R=[Sigma](Rn)/12
Where: n = sample number
Rn=(Ms-Mu)/S
Ms=total mass of compound (styrene) measured in spiked sample 
([mu]g)
Mu=total mass of compound (styrene) measured in unspiked 
sample ([mu]g)
S=theoretical mass of compound (styrene) spiked into sample ([mu]g)
R=fraction of spiked compound (styrene) recovered

    9.2.5 A different R value should be obtained for each sample type. A 
value of R between 0.70 and 1.30 is acceptable.
    9.2.6 R is used to correct all reported results for each compound by 
dividing the measured results of each compound by the R for that 
compound for the same sample type.

                            10.0 Calibration

    A styrene control sample will be tested weekly to confirm the FID 
response and calibration.

    10.1 Using the Styrene Certification Solution prepared in 7.8.1, 
perform test analysis as described in 7.8.2 using the equation in 
7.8.2.3 to calculate results.
    10.2 Calculate the weight of styrene in the styrene control sample 
using the following equation:

Wsty=(Fx xAsty 
xWis)Ais

    The instrument can be considered calibrated if the weight of the 
styrene analyzed is within range of 0.00097--0.00103gms.

                             11.0 Procedure

    11.1 Using an auto pipet, add 25ml of Internal Standard Solution to 
a 4 oz. wide-mouth bottle.
    11.2 Using a calibrated auto pipet, add 5.0  
0.01g latex to the bottle containing the 25ml of Internal Standard 
Solution.
    11.3 Cap the bottle and place on the wrist action shaker. Shake the 
sample for a minimum of five minutes using the timer on the shaker. 
Remove from shaker.
    11.4 Using a disposable pipet, fill the 2ml sample vial with the 
clear alcohol extract. (If the extract is not clear, it should be 
filtered using a funnel and filter paper.) Cap and seal the vial.
    11.5 Place the sample in the autosampler tray and start the GC and 
Integrator. The sample will be injected into the GC by the auto-
injector, and the Integrator will print the results.
    11.6 Gas Chromatograph Conditions

Oven Temp--70 [deg]C
Injector Temp--225 [deg]C
Detector Temp--275 [deg]C
Helium Pressure--500 KPA
Column Head Pressure--70 KPA
Makeup Gas--30 ml/min.
Column--HP 19095F--123, 30mx0.53mm Substrate: HP--FFAP (cross-linked) 1 
micrometer film thickness

                            12.0 Calculations

    12.1 The integrator is programmed to do the following calculation at 
the end of the analysis:

%ResidualStyrene=(Ax XWis)/(Ais 
XWx)XFx X100

Where:
Ax=Peak area of styrene
Ais=Peak area of internal standard
Wx=Weight of sample = 5g
Wis=Weight of internal std. = 0.00125g
Fx=Analyzed response factor = 1.0

    12.2 The response factor is determined by analyzing a solution of 
0.02g of styrene and

[[Page 259]]

0.02g of alpha methyl styrene in 100ml of 2-propanol. Calculate the 
factor by the following equation:

Fx=(Wx xAis)/(Wis 
xAx)

Where:
Wx=Weight of styrene
Ax=Peak area of styrene
Wis=Weight of alpha methyl styrene
Ais=Peak area of alpha methyl styrene

                         13.0 Method Performance

    13.1 Performance must be determined for each sample type by 
following the procedures in section 9 of this method.

                          14.0 Waste Generation

    14.1 Waste generation should be minimized where possible.

                          15.0 Waste Management

    15.1 All waste shall be handled in accordance with Federal and State 
environmental regulations.
    16.0 References. [Reserved]

   Method 313A--Determination of Residual Hydrocarbons in Rubber Crumb

                        1.0 Scope and Application

    1.1 This method determines residual toluene and styrene in stripper 
crumb of the of the following types of rubber: polybutadiene (PBR) and 
styrene/butadiene rubber (SBR), both derived from solution 
polymerization processes that utilize toluene as the polymerization 
solvent.
    1.2 The method is applicable to a wide range of concentrations of 
toluene and styrene provided that calibration standards cover the 
desired range. It is applicable at least over the range of 0.01 to 10.0 
% residual toluene and from 0.1 to 3.0 % residual styrene. It is 
probably applicable over a wider range, but this must be verified prior 
to use.
    1.3 The method may also be applicable to other process samples as 
long as they are of a similar composition to stripper crumb. See section 
3.1 of this method for a description of stripper crumb.

                          2.0 Summary of Method

    2.1 The wet crumb is placed in a sealed vial and run on a headspace 
sampler which heats the vial to a specified temperature for a specific 
time and then injects a known volume of vapor into a capillary GC. The 
concentration of each component in the vapor is proportional to the 
level of that component in the crumb sample and does not depend on water 
content of the crumb.
    2.2 Identification of each component is performed by comparing the 
retention times to those of known standards.
    2.3 Results are calculated by the external standard method since 
injections are all performed in an identical manner. The response for 
each component is compared with that obtained from dosed samples of 
crumb.
    2.4 Measured results of each compound are corrected by dividing each 
by the average recovery efficiency determined for the same compound in 
the same sample type.

                             3.0 Definitions

    3.1 Stripper crumb refers to pieces of rubber resulting from the 
steam stripping of a toluene solution of the same polymer in a water 
slurry. The primary component of this will be polymer with lesser 
amounts of entrained water and residual toluene and other hydrocarbons. 
The amounts of hydrocarbons present must be such that the crumb is a 
solid material, generally less that 10 % of the dry rubber weight.

                            4.0 Interferences

    4.1 Contamination is not normally a problem since samples are sealed 
into vials immediately on sampling.
    4.2 Cross contamination in the headspace sampler should not be a 
problem if the correct sampler settings are used. This should be 
verified by running a blank sample immediately following a normal or 
high sample. Settings may be modified if necessary if this proves to be 
a problem, or a blank sample may be inserted between samples.
    4.3 Interferences may occur if volatile hydrocarbons are present 
which have retention times close to that of the components of interest. 
Since the solvent makeup of the processes involved are normally fairly 
well defined this should not be a problem. If it is found to be the 
case, switching to a different chromatographic column will probably 
resolve the situation.

                               5.0 Safety

    5.1 The chemicals specified in this method should all be handled 
according to standard laboratory practices as well as any special 
precautions that may be listed in the MSDS for that compound.
    5.2 Sampling of strippers or other process streams may involve high 
pressures and temperatures or may have the potential for exposure to 
chemical fumes. Only personnel who have been trained in the specific 
sampling procedures required for that process should perform this 
operation. An understanding of the process involved is necessary. Proper 
personal protective equipment should be worn. Any sampling devices 
should be inspected prior to use. A detailed sampling procedure which 
specifies exactly how to obtain the sample must be written and followed.

[[Page 260]]

                       6.0 Equipment and Supplies

    6.1 Hewlett Packard (HP) 7694 Headspace sampler, or equivalent, with 
the following conditions:

Times (min.): GC cycle time 6.0 , vial equilibration 30.0 , 
pressurization 0.25 , loop fill 0.25, loop equilibration 0.05 , inject 
0.25
Temperatures (deg C): oven 70, loop 80, transfer line 90
Pressurization gas: He @ 16 psi

    6.2 HP 5890 Series II capillary gas chromatograph, or equivalent, 
with the following conditions:

Column: Supelco SPB-1, or equivalent, 15m x .25mm x .25[mu] film
Carrier: He @ 6 psi
Run time: 4 minutes
Oven: 70 deg C isothermal
Injector: 200 deg C split ratio 50:1
Detector: FID @ 220 deg C

    6.3 HP Chemstation consisting of computer, printer and Chemstation 
software, or an equivalent chromatographic data system.
    6.4 20 ml headspace vials with caps and septa.
    6.5 Headspace vial crimper.
    6.6 Microliter pipetting syringes.
    6.7 Drying oven at 100 deg C vented into cold trap or other means of 
trapping hydrocarbons released.
    6.8 Laboratory shaker or tumbler suitable for the headspace vials.
    6.9 Personal protective equipment required for sampling the process 
such as rubber gloves and face and eye protection.

                       7.0 Reagents and Standards

    7.1 Toluene, 99.9+% purity, HPLC grade.
    7.2 Styrene, 99.9+% purity, HPLC grade.
    7.3 Dry rubber of same type as the stripper crumb samples.

             8.0 Sample Collection, Preservation and Storage

    8.1 Collect a sample of crumb in a manner appropriate for the 
process equipment being sampled.
    8.1.1 If conditions permit, this may be done by passing a stream of 
the crumb slurry through a strainer, thus separating the crumb from the 
water. Allow the water to drain freely, do not attempt to squeeze any 
water from the crumb. Results will not depend on the exact water content 
of the samples. Immediately place several pieces of crumb directly into 
a headspace vial. This should be done with rubber gloves to protect the 
hands from both the heat and from contact with residual hydrocarbons. 
The vial should be between \1/4\ and \1/3\ full. Results do not depend 
on sample size as long as there is sufficient sample to reach an 
equilibrium vapor pressure in the headspace of the vial. Cap and seal 
the vial. Prepare each sample at least in duplicate. This is to minimize 
the effect of the variation that naturally occurs in the composition of 
non homogeneous crumb. The free water is not analyzed by this method and 
should be disposed of appropriately along with any unused rubber crumb.
    8.1.2 Alternatively the process can be sampled in a specially 
constructed sealed bomb which can then be transported to the laboratory. 
The bomb is then cooled to ambient temperature by applying a stream of 
running water. The bomb can then be opened and the crumb separated from 
the water and the vials filled as described in section 8.1.1 of this 
method. The bomb may be stored up to 8 hours prior to transferring the 
crumb into vials.
    8.2 The sealed headspace vials may be run immediately or may be 
stored up to 72 hours prior to running. It is possible that even longer 
storage times may be acceptable, but this must be verified for the 
particular type of sample being analyzed (see section 9.2.3 of this 
method). The main concern here is that some types of rubber eventually 
may flow, thus compacting the crumb so that the surface area is reduced. 
This may have some effect on the headspace equilibration.

                           9.0 Quality Control

    9.1 The laboratory is required to operate a formal quality control 
program. This consists of an initial demonstration of the capability of 
the method as well as ongoing analysis of standards, blanks and spiked 
samples to demonstrate continued performance.
    9.1.1 When the method is first set up a calibration is run 
(described in section 10 of this method) and an initial demonstration of 
method capability is performed (described in section 9.2 of this 
method). Also recovery efficiency for each type of sample must be 
determined (see section 9.4 of this method).
    9.1.2 It is permissible to modify this method in order to improve 
separations or make other improvements, provided that all performance 
specifications are met. Each time a modification to the method is made 
it is necessary to repeat the calibration (section 10 of this method), 
the demonstration of method performance (section 9.2 of this method) and 
the recovery efficiency for each type of sample (section 9.4 of this 
method).
    9.1.3 Ongoing performance should be monitored by running a spiked 
rubber standard. If this test fails to demonstrate that the analysis is 
in control, then corrective action must be taken. This method is 
described in section 9.3 of this method.
    9.1.4 If new types of samples are being analyzed then recovery 
efficiency for each new type of sample must be determined. New type 
includes any change, such as polymer type, physical form or a 
significant change in the composition of the matrix.
    9.2 Initial demonstration of method capability to establish the 
accuracy and precision of the method. This is to be run following

[[Page 261]]

the calibration described in section 10 of this method.
    9.2.1 Prepare a series of identical spiked rubber standards as 
described in section 9.3 of this method. A sufficient number to 
determine statistical information on the test should be run. Ten may be 
a suitable number, depending on the quality control methodology used at 
the laboratory running the tests. These are run in the same manner as 
unknown samples (see section 11 of this method).
    9.2.2 Determine mean and standard deviation for the results. Use 
these to determine the capability of the method and to calculate 
suitable control limits for the ongoing performance check which will 
utilize the same standards.
    9.2.3 Prepare several additional spiked rubber standards and run 2 
each day to determine the suitability of storage of the samples for 24, 
48 and 72 hours or longer if longer storage times are desired.
    9.3 A spiked rubber standard should be run on a regular basis to 
verify system performance. This would probably be done daily if samples 
are run daily. This is prepared in the same manner as the calibration 
standards (section 10.1 of this method), except that only one 
concentration of toluene and styrene is prepared. Choose concentrations 
of toluene and styrene that fall in the middle of the range expected in 
the stripper crumb and then do not change these unless there is a major 
change in the composition of the unknowns. If it becomes necessary to 
change the composition of this standard the initial performance 
demonstration must be repeated with the new standard (section 9.2 of 
this method).
    9.3.1 Each day prepare one spiked rubber standard to be run the 
following day. The dry rubber may be prepared in bulk and stored for any 
length of time consistent with the shelf life of the product. The 
addition of water and hydrocarbons must be performed daily and all the 
steps described under section 10.1 of this method must be followed.
    9.3.2 Run the spiked rubber standard prepared the previous day. 
Record the results and plot on an appropriate control chart or other 
means of determining statistical control.
    9.3.3 If the results for the standard indicate that the test is out 
of control then corrective action must be taken. This may include a 
check on procedures, instrument settings, maintenance or recalibration. 
Samples may be stored (see section 8.2 of this method) until compliance 
is demonstrated.
    9.4 Recovery efficiency must be determined once for each sample type 
and whenever modifications are made to the method.
    9.4.1 For each sample type collect 12 samples from the process 
(section 8.1 of this method). This should be done when the process is 
operating in a normal manner and residual hydrocarbon levels are in the 
normal range. Half the vials and caps should be tared, labeled 
``spiked'' and numbered 1 through 6. The other vials are labeled 
``unspiked'' and need not be tared but are also numbered 1 through 6. 
Immediately on sampling, the vials should be capped to prevent loss of 
volatiles. Allow all the samples to cool completely to ambient 
temperature. Reweigh each of the vials labeled ``spiked'' to determine 
the weight of wet crumb inside.
    9.4.2 The dry weight of rubber present in the wet crumb is estimated 
by multiplying the weight of wet crumb by the fraction of nonvolatiles 
typical for the sample. If this is not known, an additional quantity of 
crumb may be sampled, weighed, dried in an oven and reweighed to 
determine the fraction of volatiles and nonvolatiles prior to starting 
this procedure.
    9.4.3 To the vials labeled ``spiked'' add an amount of a mixture of 
toluene and styrene that is between 40 and 60 % of the amount expected 
in the crumb. This is done by removing the cap, adding the mixture by 
syringe, touching the tip of the needle to the sample in order to remove 
the drop and then immediately recapping the vials. The mixture is not 
added through the septum, because a punctured septum may leak and vent 
vapors as the vial is heated. The weights of toluene and styrene added 
may be calculated from the volumes of the mixture added, its composition 
and density, or may be determined by the weight of the vials and caps 
prior to and after addition. The exact dry weight of rubber present and 
the concentration of residual toluene and styrene are not known at this 
time so an exact calculation of the concentration of hydrocarbons is not 
possible until the test is completed.
    9.4.4 Place all the vials onto a shaker or tumbler for 24  2 hours. This is essential in order for the 
hydrocarbons to be evenly distributed and completely absorbed into the 
rubber. If this is not followed the toluene and styrene will be mostly 
at the surface of the rubber and high results will be obtained.
    9.4.5 Remove the vials from the shaker and tap them so that all the 
crumb settles to the bottom of the vials. Allow them to stand for 1 hour 
prior to analysis to allow any liquid to drain fully to the bottom.
    9.4.6 Run the spiked and unspiked samples in the normal manner. 
Record the concentrations of toluene and styrene reported for each pair 
of spiked and unspiked samples with the same vial number.
    9.4.7 Open each of the vials labeled ``spiked'', remove all the 
rubber crumb and place it into a tarred drying pan. Place in a 100 deg C 
oven for two hours, cool and reweigh. Subtract the weight of the tare to 
give the dry weight of rubber in each spiked vial. Calculate the 
concentration of toluene and styrene spiked into each vial as percent of 
dry rubber weight. This will be slightly

[[Page 262]]

different for each vial since the weights of dry rubber will be 
different.
    9.4.8 For each hydrocarbon calculate the average recovery efficiency 
(R) using the following equations:

R=R--[Sigma](Pn)/6 (average of the 6 individual Rn 
values)

Where:
Rn=(Cns--Cnu) / Sn

Where:
n=vial number
Cns=concentration of compound measured in spiked sample number n.
Cnu=concentration of compound measured in unspiked sample number n.
Sn=theoretical concentration of compound spiked into sample n calculated 
in step 9.4.7

    9.4.9 A different R value should be obtained for each compound 
(styrene and toluene) and for each sample type.
    9.4.10 A value of R between 0.70 and 1.30 is acceptable.
    9.4.11 R is used to correct all reported results for each compound 
by dividing the measured results of each compound by the R for that 
compound for the same sample type (see section 12.2 of this method.)

                            10.0 Calibration

    10.1 Calibration standards are prepared by dosing known amounts of 
the hydrocarbons of interest into vials containing known amounts of 
rubber and water.
    10.1.1 Cut a sufficient quantity of dry rubber of the same type as 
will be analyzed into pieces about the same size as that of the crumb. 
Place these in a single layer on a piece of aluminum foil or other 
suitable surface and place into a forced air oven at 100 [deg]C for four 
hours. This is to remove any residual hydrocarbons that may be present. 
This step may be performed in advance.
    10.1.2 Into each of a series of vials add 3.0 g of the dry rubber.
    10.1.3 Into each vial add 1.0 ml distilled water or an amount that 
is close to the amount that will be present in the unknowns. The exact 
amount of water present does not have much effect on the analysis, but 
it is necessary to have a saturated environment. The water will also aid 
in the uniform distribution of the spiked hydrocarbons over the surface 
of the rubber after the vials are placed on the shaker (in step 10.1.5 
of this method).
    10.1.4 Into each vial add varying amounts of toluene and styrene by 
microliter syringe and cap the vials immediately to prevent loss. The 
tip of the needle should be carefully touched to the rubber in order to 
transfer the last drop to the rubber. Toluene and styrene may first be 
mixed together in suitable proportions and added together if desired. 
The weights of toluene and styrene added may be calculated from the 
volumes of the mixture added, its composition and density, or may be 
determined by the weight of the vials and caps prior to and after 
addition. Concentrations of added hydrocarbons are calculated as percent 
of the dry rubber weight. At least 5 standards should be prepared with 
the amounts of hydrocarbons added being calculated to cover the entire 
range possible in the unknowns. Retain two samples with no added 
hydrocarbons as blanks.
    10.1.5 Place all the vials onto a shaker or tumbler for 24  2 hours. This is essential in order for the 
hydrocarbons to be evenly distributed and completely absorbed into the 
rubber. If this is not followed the toluene and styrene will be mostly 
at the surface of the rubber and high results will be obtained.
    10.1.6 Remove the vials from the shaker and tap them so that all the 
crumb settles to the bottom of the vials. Allow them to stand for 1 hour 
prior to analysis to allow any liquid to drain fully to the bottom.
    10.2 Run the standards and blanks in the same manner as described 
for unknowns (section 11 of this method), starting with a blank, then in 
order of increasing hydrocarbon content and ending with the other blank.
    10.3 Verify that the blanks are sufficiently free from toluene and 
styrene or any interfering hydrocarbons.
    10.3.1 It is possible that trace levels may be present even in dry 
product. If levels are high enough that they will interfere with the 
calibration then the drying procedure in section 10.1.1 of this method 
should be reviewed and modified as needed to ensure that suitable 
standards can be prepared.
    10.3.2 It is possible that the final blank is contaminated by the 
previous standard. If this is the case review and modify the sampler 
parameters as needed to eliminate this problem. If necessary it is 
possible to run blank samples between regular samples in order to reduce 
this problem, though it should not be necessary if the sampler is 
properly set up.
    10.4 Enter the amounts of toluene and styrene added to each of the 
samples (as calculated in section 10.1.4 of this method) into the 
calibration table and perform a calibration utilizing the external 
standard method of analysis.
    10.5 At low concentrations the calibration should be close to 
linear. If a wide range of levels are to be determined it may be 
desirable to apply a nonlinear calibration to get the best fit.

                             11.0 Procedure

    11.1 Place the vials in the tray of the headspace sampler. Enter the 
starting and ending positions through the console of the sampler. For 
unknown samples each is run in duplicate to minimize the effect of 
variations in crumb composition. If excessive

[[Page 263]]

variation is noted it may be desirable to run more than two of each 
sample.
    11.2 Make sure the correct method is loaded on the Chemstation. Turn 
on the gas flows and light the FID flame.
    11.3 Start the sequence on the Chemstation. Press the START button 
on the headspace unit. The samples will be automatically injected after 
equilibrating for 30 minutes in the oven. As each sample is completed 
the Chemstation will calculate and print out the results as percent 
toluene and styrene in the crumb based on the dry weight of rubber.

                   12.0 Data Analysis and Calculations

    12.1 For each set of duplicate samples calculate the average of the 
measured concentration of toluene and styrene. If more than two 
replicates of each sample are run calculate the average over all 
replicates.
    12.2 For each sample correct the measured amounts of toluene and 
styrene using the following equation:

Corrected Result = Cm/R

Where:
Cm = Average measured concentration for that compound.
R = Recovery efficiency for that compound in the same sample type (see 
section 9.4 of this method)

    12.3 Report the recovery efficiency (R) and the corrected results of 
toluene and styrene for each sample.

                         13.0 Method Performance

    13.1 This method can be very sensitive and reproducible. The actual 
performance depends largely on the exact nature of the samples being 
analyzed. Actual performance must be determined by each laboratory for 
each sample type.
    13.2 The main source of variation is the actual variation in the 
composition of non homogeneous crumb in a stripping system and the small 
sample sizes employed here. It therefore is the responsibility of each 
laboratory to determine the optimum number of replicates of each sample 
required to obtain accurate results.

                        14.0 Pollution Prevention

    14.1 Samples should be kept sealed when possible in order to prevent 
evaporation of hydrocarbons.
    14.2 When drying of samples is required it should be done in an oven 
which vents into a suitable device that can trap the hydrocarbons 
released.
    14.3 Dispose of samples as described in section 15.

                          15.0 Waste Management

    15.1 Excess stripper crumb and water as well as the contents of the 
used sample vials should be properly disposed of in accordance with 
local and federal regulations.
    15.2 Preferably this will be accomplished by having a system of 
returning unused and spent samples to the process.

                             16.0 References

    16.1 ``HP 7694 Headspace Sampler--Operating and Service Manual'', 
Hewlett-Packard Company, publication number G1290-90310, June 1993.

   Method 313B--The Determination of Residual Hydrocarbon in Solution 
                Polymers by Capillary Gas Chromatography

                                1.0 Scope

    1.1 This method is applicable to solution polymerized polybutadiene 
(PBD).
    1.2 This method quantitatively determines n-hexane in wet crumb 
polymer at levels from 0.08 to 0.15% by weight.
    1.3 This method may be extended to the determination of other 
hydrocarbons in solution produced polymers with proper experimentation 
and documentation.

                         2.0 Principle of Method

    2.1 A weighed sample of polymer is dissolved in chloroform and the 
cement is coagulated with an isopropyl alcohol solution containing a 
specific amount of alpha-methyl styrene (AMS) as the internal standard. 
The extract of this coagulation is then injected into a gas 
chromatograph and separated into individual components. Quantification 
is achieved by the method of internal standardization.

                             3.0 Definitions

    3.1 The definitions are included in the text as needed.

                      4.0 Interferences. [Reserved]

                               5.0 Safety

    5.1 This method may involve hazardous materials, operations, and 
equipment. This method does not purport to address all of the safety 
problems associated with its use. It is the responsibility of the user 
of this method to establish appropriate safety and health practices and 
determine the applicability of regulatory limitations prior to use.

                       6.0 Equipment and Supplies

    6.1 Analytical balance, 160 g capacity, 0.1 mg resolution
    6.2 Bottles, 2-oz capacity with poly-cap screw lids
    6.3 Mechanical shaker
    6.4 Syringe, 10-ul capacity
    6.5 Syringe, 2.5-ml capacity, with 22 gauge 1.25 inch needle, PP/PE 
material, disposable

[[Page 264]]

    6.6 Gas chromatograph, Hewlett-Packard model 5890, or equivalent, 
configured with FID, split injector packed with silanized glass wool.
    6.6.1 Establish the following gas chromatographic conditions, and 
allow the system to thoroughly equilibrate before use.
    6.6.2 Injector parameters:

Injection technique=Split
Injector split flow=86 ml/min
Injector temperature=225 deg C

    6.6.3 Oven temperature program:
Initial temperature=40 deg C
Initial time=6 min
Program rate=10 deg C/min
Upper limit temperature=175 deg C
Upper limit interval=10 min

    6.6.4 Detector parameters:
Detector temperature=300 deg C
Hydrogen flow=30 ml/min
Air flow=350 ml/min
Nitrogen make up=26 ml/min

    6.7 Gas chromatographic columns: SE-54 (5%-phenyl) (1%-vinyl)-
methylpolysiloxane, 15 Mx0.53 mm ID with a 1.2 micron film thickness, 
and a Carbowax 20M (polyethylene glycol), 15 Mx0.53 mm ID with a 1.2 
micron film thickness.
    6.7.1 Column assembly: using a 0.53 mm ID butt connector union, join 
the 15 Mx0.53 mm SE-54 column to the 15 Mx0.53 mm Carbowax 20M. The SE-
54 column will be inserted into the injector and the Carbowax 20M 
inserted into the detector after they have been joined.
    6.7.2 Column parameters:

Helium flow=2.8 ml/min
Helium headpressure=2 psig

    6.8 Centrifuge
    6.9 Data collection system, Hewlett-Packard Model 3396, or 
equivalent
    6.10 Pipet, 25-ml capacity, automatic dispensing, and 2 liter 
reservoir
    6.11 Pipet, 2-ml capacity, volumetric delivery, class A
    6.12 Flasks, 100 and 1000-ml capacity, volumetric, class A
    6.13 Vial, serum, 50-ml capacity, red rubber septa and crimp ring 
seals
    6.14 Sample collection basket fabricated out of wire mesh to allow 
for drainage

                       7.0 Chemicals and Reagents

    CHEMICALS:
    7.1 alpha-Methyl Styrene, C9H10, 99+% purity, CAS 98-83-9
    7.2 n-Hexane, C6H14, 99+% purity, CAS 110-54-3
    7.3 Isopropyl alcohol, C3H8O 99.5+% purity, reagent grade, CAS 67-
63-0
    7.4 Chloroform, CHCl3, 99% min., CAS 67-66-3
    REAGENTS:
    7.5 Internal Standard Stock Solution: 10 mg/25 ml AMS in isopropyl 
alcohol.
    7.5.1 Into a 25-ml beaker, weigh 0.4 g of AMS to the nearest 0.1 mg.
    7.5.2 Quantitatively transfer this AMS into a 1-L volumetric flask. 
Dilute to the mark with isopropyl alcohol.
    7.5.3 Transfer this solution to the automatic dispensing pipet 
reservoir. This will be labeled the AMS STOCK SOLUTION.
    7.6 n-Hexane Stock Solution: 13mg/2ml hexane in isopropyl alcohol.
    7.6.1 Into a 100-ml volumetric flask, weigh 0.65 g of n-hexane to 
the nearest 0.1 mg.
    7.6.2 Dilute to the mark with isopropyl alcohol. This solution will 
be labeled the n-HEXANE STOCK SOLUTION.

             8.0 Sample Collection, Preservation and Storage

    8.1 A sampling device similar to Figure 1 is used to collect a non-
vented crumb rubber sample at a location that is after the stripping 
operation but before the sample is exposed to the atmosphere.
    8.2 The crumb rubber is allowed to cool before opening the sampling 
device and removing the sample.
    8.3 The sampling device is opened and the crumb rubber sample is 
collected in the sampling basket.
    8.4 One pound of crumb rubber sample is placed into a polyethylene 
bag. The bag is labeled with the time, date and sample location.
    8.5 The sample should be delivered to the laboratory for testing 
within one hour of sampling.
    8.6 Laboratory testing will be done within 3 hours of the sampling 
time.
    8.7 No special storage conditions are required unless the storage 
time exceeds 3 hours in which case refrigeration of the samples is 
recommended.

                           9.0 Quality Control

    9.1 For each sample type, 12 samples shall be obtained from the 
process for the recovery study. Half of the vials and caps shall be 
tared, labeled ``spiked'', and numbered 1 through 6. The other vials 
shall be labeled ``unspiked'' and need not be tared, but are also 
numbered 1 through 6.
    9.2 Determine the % moisture content of the crumb sample. After 
determining the % moisture content, the correction factor for 
calculating the dry crumb weight can be determined by using the equation 
in section 12.2 of this method.
    9.3 Run the spiked and unspiked samples in the normal manner. Record 
the concentrations of the n-hexane content of the mixed hexane reported 
for each pair of spiked and unspiked samples.
    9.4 For the recovery study, each sample of crumb shall be dissolved 
in chloroform containing a known amount of mixed hexane solvent.

[[Page 265]]

    9.5 For each hydrocarbon, calculate the recovery efficiency (R) 
using the following equations:

Mr=Ms-Mu
R=Mr/S

Where:
Mu=Measured amount of compound in the unspiked sample
Ms=Measured amount of compound in the spiked sample
Mr=Measured amount of the spiked compound
S=Amount of compound added to the spiked sample
R=Fraction of spiked compound recovered

    9.6 Normally a value of R between 0.70 and 1.30 is acceptable.
    9.7 R is used to correct all reported results for each compound by 
dividing the measured results of each compound by the R for that 
compound for the same sample type.

                            10.0 Calibration

    10.1 Using the AMS STOCK SOLUTION equipped with the automatic 
dispensing pipet (7.5.3 of this method), transfer 25.0 ml of the 
internal standard solution into an uncapped 50-ml serum vial.
    10.2 Using a 2.0 ml volumetric pipet, quantitatively transfer 2.0 ml 
of the n-HEXANE STOCK SOLUTION (7.6.2 of this method) into the 50-ml 
serum vial and cap. This solution will be labeled the CALIBRATION 
SOLUTION.
    10.3 Using the conditions prescribed (6.6 of this method), inject 1 
[mu]l of the supernate.
    10.4 Obtain the peak areas and calculate the response factor as 
described in the calculations section (12.1 of this method).

                             11.0 Procedure

    11.1 Determination of Dry Polymer Weight
    11.1.1 Remove wet crumb from the polyethylene bag and place on paper 
towels to absorb excess surface moisture.
    11.1.2 Cut small slices or cubes from the center of the crumb sample 
to improve sample uniformity and further eliminate surface moisture.
    11.1.3 A suitable gravimetric measurement should be made on a sample 
of this wet crumb to determine the correction factor needed to calculate 
the dry polymer weight.
    11.2 Determination of n-Hexane in Wet Crumb
    11.2.1 Remove wet crumb from the polyethylene bag and place on paper 
towels to absorb excess surface moisture.
    11.2.2 Cut small slices or cubes from the center of the crumb sample 
to improve sample uniformity and further eliminate surface moisture.
    11.2.3 Into a tared 2 oz bottle, weigh 1.5 g of wet polymer to the 
nearest 0.1 mg.
    11.2.4 Add 25 ml of chloroform to the 2 oz bottle and cap.
    11.2.5 Using a mechanical shaker, shake the bottle until the polymer 
dissolves.
    11.2.6 Using the autodispensing pipet, add 25.0 ml of the AMS STOCK 
SOLUTION (7.5.3 of this method) to the dissolved polymer solution and 
cap.
    11.2.7 Using a mechanical shaker, shake the bottle for 10 minutes to 
coagulate the dissolved polymer.
    11.2.8 Centrifuge the sample for 3 minutes at 2000 rpm.
    11.2.9 Using the conditions prescribed (6.6 of this method), 
chromatograph 1 [mu]l of the supernate.
    11.2.10 Obtain the peak areas and calculate the concentration of the 
component of interest as described in the calculations (12.2 of this 
method).

                            12.0 Calculations

    12.1 Calibration:

RFx=(Wx x Ais) / (Wis x 
Ax)

Where:
RFx=the relative response factor for n-hexane
Wx=the weight (g) of n-hexane in the CALIBRATION
SOLUTION
Ais=the area of AMS
Wis=the weight (g) of AMS in the CALIBRATION SOLUTION
Ax=the area of n-hexane

    12.2 Procedure:
    12.2.1 Correction Factor for calculating dry crumb weight.

F=1--(% moisture / 100)

Where:
F=Correction factor for calculating dry crumb weight
% moisture determined by appropriate method

    12.2.2 Moisture adjustment for chromatographic determination.

Ws=F x Wc

Where:
Ws=the weight (g) of the dry polymer corrected for moisture
F=Correction factor for calculating dry crumb weight
Wc=the weight (g) of the wet crumb in section 9.6

    12.2.3 Concentration (ppm) of hexane in the wet crumb.

ppmx=(Ax * RFx * Wis * 
10000) / (Ais * Ws)

Where:
ppmx=parts per million of n-hexane in the polymer
Ax=the area of n-hexane
RFx=the relative response factor for n-hexane
Wis=the weight (g) of AMS in the sample solution

[[Page 266]]

Ais=the area of AMS
Ws=the weight (g) of the dry polymer corrected for moisture

                         13.0 Method Performance

    13.1 Precision for the method was determined at the 0.08% level.

    The standard deviation was 0.01 and the percent relative standard 
deviation (RSD) was 16.3 % with five degrees of freedom.

                          14.0 Waste Generation

    14.1 Waste generation should be minimized where possible.

                          15.0 Waste Management

    15.1 Discard liquid chemical waste into the chemical waste drum.
    15.2 Discard polymer waste into the polymer waste container.

                             16.0 References

    16.1 This method is based on Goodyear Chemical Division Test Method 
E-964.

    Method 315--Determination of Particulate and Methylene Chloride 
  Extractable Matter (MCEM) From Selected Sources at Primary Aluminum 
                          Production Facilities

    Note: This method does not include all of the specifications (e.g., 
equipment and supplies) and procedures (e.g., sampling and analytical) 
essential to its performance. Some material is incorporated by reference 
from other methods in this part. Therefore, to obtain reliable results, 
persons using this method should have a thorough knowledge of at least 
the following additional test methods: Method 1, Method 2, Method 3, and 
Method 5 of 40 CFR part 60, appendix A.

                       1.0 Scope and Application.

    1.1 Analytes. Particulate matter (PM). No CAS number assigned. 
Methylene chloride extractable matter (MCEM). No CAS number assigned.
    1.2 Applicability. This method is applicable for the simultaneous 
determination of PM and MCEM when specified in an applicable regulation. 
This method was developed by consensus with the Aluminum Association and 
the U.S. Environmental Protection Agency (EPA) and has limited precision 
estimates for MCEM; it should have similar precision to Method 5 for PM 
in 40 CFR part 60, appendix A since the procedures are similar for PM.
    1.3 Data quality objectives. Adherence to the requirements of this 
method will enhance the quality of the data obtained from air pollutant 
sampling methods.

                         2.0 Summary of Method.

    Particulate matter and MCEM are withdrawn isokinetically from the 
source. PM is collected on a glass fiber filter maintained at a 
temperature in the range of l20  14 [deg]C (248 
25 [deg]F) or such other temperature as specified 
by an applicable subpart of the standards or approved by the 
Administrator for a particular application. The PM mass, which includes 
any material that condenses on the probe and is subsequently removed in 
an acetone rinse or on the filter at or above the filtration 
temperature, is determined gravimetrically after removal of uncombined 
water. MCEM is then determined by adding a methylene chloride rinse of 
the probe and filter holder, extracting the condensable hydrocarbons 
collected in the impinger water, adding an acetone rinse followed by a 
methylene chloride rinse of the sampling train components after the 
filter and before the silica gel impinger, and determining residue 
gravimetrically after evaporating the solvents.

                       3.0 Definitions. [Reserved]

                      4.0 Interferences. [Reserved]

                               5.0 Safety.

    This method may involve hazardous materials, operations, and 
equipment. This method does not purport to address all of the safety 
problems associated with its use. It is the responsibility of the user 
of this method to establish appropriate safety and health practices and 
determine the applicability of regulatory limitations prior to 
performing this test method.

                       6.0 Equipment and Supplies.

    Note: Mention of trade names or specific products does not 
constitute endorsement by the EPA.

    6.1 Sample collection. The following items are required for sample 
collection:
    6.1.1 Sampling train. A schematic of the sampling train used in this 
method is shown in Figure 5-1, Method 5, 40 CFR part 60, appendix A. 
Complete construction details are given in APTD-0581 (Reference 2 in 
section 17.0 of this method); commercial models of this train are also 
available. For changes from APTD-0581 and for allowable modifications of 
the train shown in Figure 5-1, Method 5, 40 CFR part 60, appendix A, see 
the following subsections.

    Note: The operating and maintenance procedures for the sampling 
train are described in APTD-0576 (Reference 3 in section 17.0 of this 
method). Since correct usage is important in obtaining valid results, 
all users should read APTD-0576 and adopt the operating and maintenance 
procedures outlined in it, unless otherwise specified herein. The use of 
grease for sealing sampling train components is not recommended because 
many

[[Page 267]]

greases are soluble in methylene chloride. The sampling train consists 
of the following components:

    6.1.1.1 Probe nozzle. Glass or glass lined with sharp, tapered 
leading edge. The angle of taper shall be <=30 [deg], and the taper 
shall be on the outside to preserve a constant internal diameter. The 
probe nozzle shall be of the button-hook or elbow design, unless 
otherwise specified by the Administrator. Other materials of 
construction may be used, subject to the approval of the Administrator. 
A range of nozzle sizes suitable for isokinetic sampling should be 
available. Typical nozzle sizes range from 0.32 to 1.27 cm (\1/8\ to \1/
2\ in.) inside diameter (ID) in increments of 0.16 cm (\1/16\ in.). 
Larger nozzle sizes are also available if higher volume sampling trains 
are used. Each nozzle shall be calibrated according to the procedures 
outlined in section 10.0 of this method.
    6.1.1.2 Probe liner. Borosilicate or quartz glass tubing with a 
heating system capable of maintaining a probe gas temperature at the 
exit end during sampling of 12014 [deg]C 
(24825 [deg]F), or such other temperature as 
specified by an applicable subpart of the standards or approved by the 
Administrator for a particular application. Because the actual 
temperature at the outlet of the probe is not usually monitored during 
sampling, probes constructed according to APTD-0581 and using the 
calibration curves of APTD-0576 (or calibrated according to the 
procedure outlined in APTD-0576) will be considered acceptable. Either 
borosilicate or quartz glass probe liners may be used for stack 
temperatures up to about 480 [deg]C (900 [deg]F); quartz liners shall be 
used for temperatures between 480 and 900 [deg]C (900 and 1,650 [deg]F). 
Both types of liners may be used at higher temperatures than specified 
for short periods of time, subject to the approval of the Administrator. 
The softening temperature for borosilicate glass is 820 [deg]C (1,500 
[deg]F) and for quartz glass it is 1,500 [deg]C (2,700 [deg]F).
    6.1.1.3 Pitot tube. Type S, as described in section 6.1 of Method 2, 
40 CFR part 60, appendix A, or other device approved by the 
Administrator. The pitot tube shall be attached to the probe (as shown 
in Figure 5-1 of Method 5, 40 CFR part 60, appendix A) to allow constant 
monitoring of the stack gas velocity. The impact (high pressure) opening 
plane of the pitot tube shall be even with or above the nozzle entry 
plane (see Method 2, Figure 2-6b, 40 CFR part 60, appendix A) during 
sampling. The Type S pitot tube assembly shall have a known coefficient, 
determined as outlined in section 10.0 of Method 2, 40 CFR part 60, 
appendix A.
    6.1.1.4 Differential pressure gauge. Inclined manometer or 
equivalent device (two), as described in section 6.2 of Method 2, 40 CFR 
part 60, appendix A. One manometer shall be used for velocity head (Dp) 
readings, and the other, for orifice differential pressure readings.
    6.1.1.5 Filter holder. Borosilicate glass, with a glass frit filter 
support and a silicone rubber gasket. The holder design shall provide a 
positive seal against leakage from the outside or around the filter. The 
holder shall be attached immediately at the outlet of the probe (or 
cyclone, if used).
    6.1.1.6 Filter heating system. Any heating system capable of 
maintaining a temperature around the filter holder of 12014 [deg]C (24825 [deg]F) during 
sampling, or such other temperature as specified by an applicable 
subpart of the standards or approved by the Administrator for a 
particular application. Alternatively, the tester may opt to operate the 
equipment at a temperature lower than that specified. A temperature 
gauge capable of measuring temperature to within 3 [deg]C (5.4 [deg]F) 
shall be installed so that the temperature around the filter holder can 
be regulated and monitored during sampling. Heating systems other than 
the one shown in APTD-0581 may be used.
    6.1.1.7 Temperature sensor. A temperature sensor capable of 
measuring temperature to within 3 [deg]C (5.4 
[deg]F) shall be installed so that the sensing tip of the temperature 
sensor is in direct contact with the sample gas, and the temperature 
around the filter holder can be regulated and monitored during sampling.
    6.1.1.8 Condenser. The following system shall be used to determine 
the stack gas moisture content: four glass impingers connected in series 
with leak-free ground glass fittings. The first, third, and fourth 
impingers shall be of the Greenburg-Smith design, modified by replacing 
the tip with a 1.3 cm (1/2 in.) ID glass tube extending to about 1.3 cm 
(1/2 in.) from the bottom of the flask. The second impinger shall be of 
the Greenburg-Smith design with the standard tip. The first and second 
impingers shall contain known quantities of water (section 8.3.1 of this 
method), the third shall be empty, and the fourth shall contain a known 
weight of silica gel or equivalent desiccant. A temperature sensor 
capable of measuring temperature to within 1 [deg]C (2 [deg]F) shall be 
placed at the outlet of the fourth impinger for monitoring.
    6.1.1.9 Metering system. Vacuum gauge, leak-free pump, temperature 
sensors capable of measuring temperature to within 3 [deg]C (5.4 
[deg]F), dry gas meter (DGM) capable of measuring volume to within 2 
percent, and related equipment, as shown in Figure 5-1 of Method 5, 40 
CFR part 60, appendix A. Other metering systems capable of maintaining 
sampling rates within 10 percent of isokinetic and of determining sample 
volumes to within 2 percent may be used, subject to the approval of the 
Administrator. When the metering system is used in conjunction with a 
pitot tube, the system shall allow periodic checks of isokinetic rates.

[[Page 268]]

    6.1.1.10 Sampling trains using metering systems designed for higher 
flow rates than that described in APTD-0581 or APTD-0576 may be used 
provided that the specifications of this method are met.
    6.1.2 Barometer. Mercury, aneroid, or other barometer capable of 
measuring atmospheric pressure to within 2.5 mm (0.1 in.) Hg.

    Note: The barometric reading may be obtained from a nearby National 
Weather Service station. In this 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 made at a rate of minus 2.5 mm (0.1 in) Hg per 30 m (100 ft) 
elevation increase or plus 2.5 mm (0.1 in) Hg per 30 m (100 ft) 
elevation decrease.

    6.1.3 Gas density determination equipment. Temperature sensor and 
pressure gauge, as described in sections 6.3 and 6.4 of Method 2, 40 CFR 
part 60, appendix A, and gas analyzer, if necessary, as described in 
Method 3, 40 CFR part 60, appendix A. The temperature sensor shall, 
preferably, be permanently attached to the pitot tube or sampling probe 
in a fixed 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-
4, 40 CFR part 60, appendix A). As a second alternative, if a difference 
of not more than 1 percent in the average velocity measurement is to be 
introduced, the temperature sensor need not be attached to the probe or 
pitot tube. (This alternative is subject to the approval of the 
Administrator.)
    6.2 Sample recovery. The following items are required for sample 
recovery:
    6.2.1 Probe-liner and probe-nozzle brushes. Nylon or Teflon[reg] 
bristle brushes with stainless steel wire handles. The probe brush shall 
have extensions (at least as long as the probe) constructed of stainless 
steel, nylon, Teflon[reg], or similarly inert material. The brushes 
shall be properly sized and shaped to brush out the probe liner and 
nozzle.
    6.2.2 Wash bottles. Glass wash bottles are recommended. Polyethylene 
or tetrafluoroethylene (TFE) wash bottles may be used, but they may 
introduce a positive bias due to contamination from the bottle. It is 
recommended that acetone not be stored in polyethylene or TFE bottles 
for longer than a month.
    6.2.3 Glass sample storage containers. Chemically resistant, 
borosilicate glass bottles, for acetone and methylene chloride washes 
and impinger water, 500 ml or 1,000 ml. Screw-cap liners shall either be 
rubber-backed Teflon[reg] or shall be constructed so as to be leak-free 
and resistant to chemical attack by acetone or methylene chloride. 
(Narrow-mouth glass bottles have been found to be less prone to 
leakage.) Alternatively, polyethylene bottles may be used.
    6.2.4 Petri dishes. For filter samples, glass, unless otherwise 
specified by the Administrator.
    6.2.5 Graduated cylinder and/or balance. To measure condensed water, 
acetone wash and methylene chloride wash used during field recovery of 
the samples, 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 such balance is suitable 
for use here and in section 6.3.4 of this method.
    6.2.6 Plastic storage containers. Air-tight containers to store 
silica gel.
    6.2.7 Funnel and rubber policeman. To aid in transfer of silica gel 
to container; not necessary if silica gel is weighed in the field.
    6.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
    6.3 Sample analysis. The following equipment is required for sample 
analysis:
    6.3.1 Glass or Teflon[reg] weighing dishes.
    6.3.2 Desiccator. It is recommended that fresh desiccant be used to 
minimize the chance for positive bias due to absorption of organic 
material during drying.
    6.3.3 Analytical balance. To measure to within 0.l mg.
    6.3.4 Balance. To measure to within 0.5 g.
    6.3.5 Beakers. 250 ml.
    6.3.6 Hygrometer. To measure the relative humidity of the laboratory 
environment.
    6.3.7 Temperature sensor. To measure the temperature of the 
laboratory environment.
    6.3.8 Buchner fritted funnel. 30 ml size, fine (<50 micron)-porosity 
fritted glass.
    6.3.9 Pressure filtration apparatus.
    6.3.10 Aluminum dish. Flat bottom, smooth sides, and flanged top, 18 
mm deep and with an inside diameter of approximately 60 mm.

                       7.0 Reagents and Standards.

    7.l Sample collection. The following reagents are required for 
sample collection:
    7.1.1 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 shall be conducted in accordance with ASTM Method D 2986-95A 
(incorporated by reference in Sec. 63.841 of this part). Test data from 
the supplier's quality control program are sufficient for this purpose. 
In sources containing S02 or S03, the filter 
material must be of a type that is unreactive to S02 or 
S03. Reference 10 in section 17.0 of this method may be used 
to select the appropriate filter.

[[Page 269]]

    7.1.2 Silica gel. Indicating type, 6 to l6 mesh. If previously used, 
dry at l75 [deg]C (350 [deg]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.
    7.1.3 Water. When analysis of the material caught in the impingers 
is required, deionized distilled water shall be used. Run blanks prior 
to field use to eliminate a high blank on test samples.
    7.1.4 Crushed ice.
    7.1.5 Stopcock grease. Acetone-insoluble, heat-stable silicone 
grease. This is not necessary if screw-on connectors with Teflon'' 
sleeves, or similar, are used. Alternatively, other types of stopcock 
grease may be used, subject to the approval of the Administrator. 
[Caution: Many stopcock greases are methylene chloride-soluble. Use 
sparingly and carefully remove prior to recovery to prevent 
contamination of the MCEM analysis.]
    7.2 Sample recovery. The following reagents are required for sample 
recovery:
    7.2.1 Acetone. Acetone with blank values < 1 ppm, by weight residue, 
is required. Acetone blanks may be run prior to field use, and only 
acetone with low blank values may be used. In no case shall a blank 
value of greater than 1E-06 of the weight of acetone used be subtracted 
from the sample weight.

    Note: This is more restrictive than Method 5, 40 CFR part 60, 
appendix A. At least one vendor (Supelco Incorporated located in 
Bellefonte, Pennsylvania) lists <1 mg/l as residue for its Environmental 
Analysis Solvents.

    7.2.2 Methylene chloride. Methylene chloride with a blank value <1.5 
ppm, by weight, residue. Methylene chloride blanks may be run prior to 
field use, and only methylene chloride with low blank values may be 
used. In no case shall a blank value of greater than 1.6E-06 of the 
weight of methylene chloride used be subtracted from the sample weight.

    Note: A least one vendor quotes <1 mg/l for Environmental Analysis 
Solvents-grade methylene chloride.

    7.3 Sample analysis. The following reagents are required for sample 
analysis:
    7.3.l Acetone. Same as in section 7.2.1 of this method.
    7.3.2 Desiccant. Anhydrous calcium sulfate, indicating type. 
Alternatively, other types of desiccants may be used, subject to the 
approval of the Administrator.
    7.3.3 Methylene chloride. Same as in section 7.2.2 of this method.

      8.0 Sample Collection, Preservation, Storage, and Transport.

    Note: The complexity of this method is such that, in order to obtain 
reliable results, testers should be trained and experienced with the 
test procedures.

    8.11 Pretest preparation. It is suggested that sampling equipment be 
maintained according to the procedures described in APTD-0576.
    8.1.1 Weigh several 200 g to 300 g portions of silica gel in 
airtight containers to the nearest 0.5 g. Record on each container the 
total weight of the silica gel plus 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.
    8.1.2 A batch of glass fiber filters, no more than 50 at a time, 
should placed in a soxhlet extraction apparatus and extracted using 
methylene chloride for at least 16 hours. After extraction, check 
filters visually against light for irregularities, flaws, or pinhole 
leaks. Label the shipping containers (glass or plastic petri dishes), 
and keep the filters in these containers at all times except during 
sampling and weighing.
    8.1.3 Desiccate the filters at 20 5.6 [deg]C 
(68 10 [deg]F) and ambient pressure for at least 
24 hours and weigh at intervals 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 longer than 2 minutes and a relative 
humidity above 50 percent. Alternatively (unless otherwise specified by 
the Administrator), the filters may be oven-dried at 104 [deg]C (220 
[deg]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.
    8.2 Preliminary determinations.
    8.2.1 Select the sampling site and the minimum number of sampling 
points according to Method 1, 40 CFR part 60, appendix A or as specified 
by the Administrator. Determine the stack pressure, temperature, and the 
range of velocity heads using Method 2, 40 CFR part 60, appendix A; it 
is recommended that a leak check of the pitot lines (see section 8.1 of 
Method 2, 40 CFR part 60, appendix A) be performed. Determine the 
moisture content using Approximation Method 4 (section 1.2 of Method 4, 
40 CFR part 60, appendix A) or its alternatives to make isokinetic 
sampling rate settings. Determine the stack gas dry molecular weight, as 
described in section 8.6 of Method 2, 40 CFR part 60, appendix A; 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 particulate sample run.
    8.2.2 Select a nozzle size based on the range of velocity heads such 
that it is not necessary to change the nozzle size in order

[[Page 270]]

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 8.2 of 
Method 2, 40 CFR part 60, appendix A).
    8.2.3 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 required probe length.
    8.2.4 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 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.
    8.2.5 The sampling time at each point shall be the same. 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 eliminate 
timekeeping errors.
    8.2.6 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.
    8.3 Preparation of sampling train.
    8.3.1 During preparation and assembly of the sampling train, keep 
all openings where contamination can occur covered until just prior to 
assembly or until sampling is about to begin. Place l00 ml of water in 
each of the first two impingers, 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 
recorded.
    8.3.2 Using a tweezer or clean disposable surgical 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 to prevent the sample gas stream from circumventing the filter. Check 
the filter for tears after assembly is completed.
    8.3.3 When glass liners are used, install the selected nozzle using 
a Viton A 0-ring when stack temperatures are less than 260 [deg]C (500 
[deg]F) and an asbestos string gasket when temperatures are higher. See 
APTD-0576 for details. Mark the probe with heat-resistant tape or by 
some other method to denote the proper distance into the stack or duct 
for each sampling point.
    8.3.4 Set up the train as in Figure 5-1 of Method 5, 40 CFR part 60, 
appendix A, using (if necessary) a very light coat of silicone grease on 
all ground glass joints, greasing only the outer portion (see APTD-0576) 
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 particulate catch is expected 
to exceed 100 mg or when water droplets are present in the stack gas.
    8.3.5 Place crushed ice around the impingers.
    8.4 Leak-check procedures.
    8.4.1 Leak check of metering system shown in Figure 5-1 of Method 5, 
40 CFR part 60, appendix A. 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 recorded than is actually sampled. The following procedure 
is suggested (see Figure 5-2 of Method 5, 40 CFR part 60, appendix A): 
Close the main valve on the meter box. Insert a one-hole rubber stopper 
with rubber 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 (5 to 7 in.) water 
column by blowing into the rubber tubing. Pinch off the tubing, and 
observe the manometer for 1 minute. A loss of pressure on the manometer 
indicates a leak in the meter box; leaks, if present, must be corrected.
    8.4.2 Pretest leak check. A pretest leak-check is recommended but 
not required. If the pretest leak-check is conducted, the following 
procedure should be used.
    8.4.2.1 After the sampling train has been assembled, turn on and set 
the filter and probe heating systems to the desired operating 
temperatures. Allow time for the temperatures to stabilize. If a Viton A 
0-ring or other leak-free connection is used in assembling the probe 
nozzle to the probe liner, leak-check the train at the sampling site by 
plugging the nozzle and pulling a 380 mm (15 in.) Hg vacuum.

    Note: A lower vacuum may be used, provided that it is not exceeded 
during the test.

    8.4.2.2 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 (15 in.) Hg vacuum. (See NOTE in section 8.4.2.1 of 
this method). Then connect the probe to the train and perform the leak 
check at approximately 25 mm (1 in.) Hg vacuum; alternatively, the probe 
may be leak-checked with the rest of the sampling train,

[[Page 271]]

in one step, at 380 mm (15 in.) Hg vacuum. Leakage rates in excess of 4 
percent of the average sampling rate or 0.00057 m\3\/min (0.02 cfm), 
whichever is less, are unacceptable.
    8.4.2.3 The following leak check instructions for the sampling train 
described in APTD-0576 and APTD-058l may be helpful. Start the pump with 
the bypass valve fully open and the 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 the 
direction of the bypass valve, as this will cause water to back up into 
the filter holder. If the desired vacuum is exceeded, either leak-check 
at this higher vacuum or end the leak check as shown below and start 
over.
    8.4.2.4 When the leak check is completed, first slowly remove the 
plug from the inlet to the probe, filter holder, or cyclone (if 
applicable) and immediately turn off the vacuum pump. This prevents the 
water in the impingers from being forced backward into the filter holder 
and the silica gel from being entrained backward into the third 
impinger.
    8.4.3 Leak checks during sample run. If, during the sampling run, a 
component (e.g., filter assembly or impinger) 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 8.4.2 of this method, 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\3\/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, either record the leakage rate and plan to 
correct the sample volume as shown in section 12.3 of this method or 
void the sample run.

    Note: Immediately after component changes, leak checks are optional; 
if such leak checks are done, the procedure outlined in section 8.4.2 of 
this method should be used.

    8.4.4 Post-test leak check. A leak check is mandatory at the 
conclusion of each sampling run. The leak check shall be performed in 
accordance with the procedures outlined in section 8.4.2 of this method, 
except that it shall be conducted at a vacuum equal to or greater than 
the maximum value reached during the sampling run. If the leakage rate 
is found to be no greater than 0.00057 m\3\/min (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, either 
record the leakage rate and correct the sample volume, as shown in 
section 12.4 of this method, or void the sampling run.
    8.5 Sampling train operation. During the sampling run, maintain an 
isokinetic sampling rate (within l0 percent of true isokinetic unless 
otherwise specified by the Administrator) and a temperature around the 
filter of 120 14 [deg]C (248 25 [deg]F), or such other temperature as 
specified by an applicable subpart of the standards or approved by the 
Administrator.
    8.5.1 For each run, record the data required on a data sheet such as 
the one shown in Figure 5-2 of Method 5, 40 CFR part 60, appendix A. Be 
sure to record the initial reading. Record the DGM 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 indicated by Figure 5-2 of Method 5, 40 CFR 
part 60, appendix A at least once at each sample point during each time 
increment and additional readings when significant changes (20 percent 
variation in velocity 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.
    8.5.2 Clean the portholes prior to the test run to minimize the 
chance of sampling deposited material. To begin sampling, remove the 
nozzle cap and verify that the filter and probe heating systems are up 
to temperature and that the pitot tube and probe are properly 
positioned. Position the nozzle at the first traverse point with the tip 
pointing directly into the gas stream. Immediately start the pump and 
adjust the flow to isokinetic conditions. Nomographs are available, 
which aid in the rapid adjustment of the isokinetic sampling rate 
without excessive computations. These nomographs are designed for use 
when the Type S pitot tube coefficient (Cp) is 0.85  
0.02 and the stack gas equivalent density (dry molecular weight) is 29 
 4. APTD-0576 details the procedure for using the 
nomographs. If Cp and Md are outside the above-
stated ranges, do not use the nomographs unless appropriate steps (see 
Reference 7 in section 17.0 of this method) are taken to compensate for 
the deviations.
    8.5.3 When the stack is under significant negative pressure (height 
of impinger stem), close the coarse adjust valve before inserting the 
probe into the stack to prevent water from backing into the filter 
holder. If necessary, the pump may be turned on with the coarse adjust 
valve closed.
    8.5.4 When the probe is in position, block off the openings around 
the probe and porthole to prevent unrepresentative dilution of the gas 
stream.
    8.5.5 Traverse the stack cross-section, as required by Method 1, 40 
CFR part 60, appendix A or as specified by the Administrator,

[[Page 272]]

being careful not to bump the probe nozzle into the stack walls when 
sampling near the walls or when removing or inserting the probe through 
the portholes; this minimizes the chance of extracting deposited 
material.
    8.5.6 During the test run, make periodic adjustments to keep the 
temperature around the filter holder at the proper level; add more ice 
and, if necessary, salt to maintain a temperature of less than 20 [deg]C 
(68 [deg]F) at the condenser/silica gel outlet. Also, periodically check 
the level and zero of the manometer.
    8.5.7 If the pressure drop across the filter becomes too high, 
making isokinetic sampling difficult to maintain, the filter may be 
replaced in the midst of the sample run. It is recommended that another 
complete filter assembly be used rather than attempting to change the 
filter itself. Before a new filter assembly is installed, conduct a leak 
check (see section 8.4.3 of this method). The total PM weight shall 
include the summation of the filter assembly catches.
    8.5.8 A single train shall be used for the entire sample run, except 
in cases where simultaneous 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: When two or more trains are used, separate analyses of the 
front-half and (if applicable) impinger catches from each train shall be 
performed, unless identical nozzle sizes were used in all trains, in 
which case the front-half catches from the individual trains may be 
combined (as may the impinger catches) and one analysis of the front-
half catch and one analysis of the impinger catch may be performed.

    8.5.9 At the end of the sample run, turn off the coarse adjust 
valve, remove the probe and nozzle from the stack, turn off the pump, 
record the final DGM reading, and then conduct a post-test leak check, 
as outlined in section 8.4.4 of this method. Also leak-check the pitot 
lines as described in section 8.1 of Method 2, 40 CFR part 60, appendix 
A. The lines must pass this leak check in order to validate the velocity 
head data.
    8.6 Calculation of percent isokinetic. Calculate percent isokinetic 
(see Calculations, section 12.12 of this method) to determine whether a 
run was valid or another test run should be made. If there was 
difficulty in maintaining isokinetic rates because of source conditions, 
consult the Administrator for possible variance on the isokinetic rates.
    8.7 Sample recovery.
    8.7.1 Proper cleanup procedure begins as soon as the probe is 
removed from the stack at the end of the sampling period. Allow the 
probe to cool.
    8.7.2 When the probe can be safely handled, wipe off all external PM 
near the tip of the probe nozzle and place a cap over it to prevent 
losing or gaining PM. Do not cap off the probe tip tightly while the 
sampling train is cooling down. This would create a vacuum in the filter 
holder, thus drawing water from the impingers into the filter holder.
    8.7.3 Before moving the sample train to the cleanup site, remove the 
probe from the sample train, wipe off the silicone 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 filter inlet 
where the probe was fastened and cap it. Remove the umbilical cord from 
the last impinger and cap the impinger. If a flexible line is used 
between the first impinger or condenser and the filter holder, 
disconnect the line at the filter holder and let any condensed water or 
liquid drain into the impingers or condenser. After wiping off the 
silicone grease, cap off the filter holder outlet and impinger inlet. 
Ground-glass stoppers, plastic caps, or serum caps may be used to close 
these openings.
    8.7.4 Transfer the probe and filter-impinger assembly 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.
    8.7.5 Save a portion of the acetone and methylene chloride used for 
cleanup as blanks. Take 200 ml of each solvent directly from the wash 
bottle being used and place it in glass sample containers labeled 
``acetone blank'' and ``methylene chloride blank,'' respectively.
    8.7.6 Inspect the train prior to and during disassembly and note any 
abnormal conditions. Treat the samples as follows:
    8.7.6.1 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 PM 
cake is inside the fold. Using a dry nylon bristle brush and/or a sharp-
edged blade, carefully transfer to the petri dish any PM and/or filter 
fibers that adhere to the filter holder gasket. Seal the container.
    8.7.6.2 Container No. 2. Taking care to see that dust on the outside 
of the probe or other exterior surfaces does not get into the sample, 
quantitatively recover PM or any condensate from the probe nozzle, probe 
fitting, probe liner, and front half of the filter holder by washing 
these components with acetone and placing the wash in a glass container. 
Perform the acetone rinse as follows:
    8.7.6.2.1 Carefully remove the probe nozzle and clean the inside 
surface by rinsing with acetone from a wash bottle and brushing with a 
nylon bristle brush. Brush until the acetone rinse shows no visible 
particles,

[[Page 273]]

after which make a final rinse of the inside surface with acetone.
    8.7.6.2.2 Brush and rinse the inside parts of the Swagelok fitting 
with acetone in a similar way until no visible particles remain.
    8.7.6.2.3 Rinse the probe liner with acetone by tilting and rotating 
the probe while squirting acetone into its upper end so that all inside 
surfaces are wetted with acetone. Let the acetone drain from the lower 
end into the sample container. A funnel (glass or polyethylene) may be 
used to aid in transferring liquid washes to the container. Follow the 
acetone rinse with a probe brush. Hold the probe in an inclined 
position, squirt acetone into the upper end as the probe brush is being 
pushed with a twisting action through the probe, hold a sample container 
under the lower end of the probe, and catch any acetone and PM that is 
brushed from the probe. Run the brush through the probe three times or 
more until no visible PM is carried out with the acetone or until none 
remains in the probe liner on visual inspection. With stainless steel or 
other metal probes, run the brush through in the above-described manner 
at least six times, since metal probes have small crevices in which PM 
can be entrapped. Rinse the brush with acetone and quantitatively 
collect these washings in the sample container. After the brushing, make 
a final acetone rinse of the probe as described above.
    8.7.6.2.4 It is recommended that two people clean the probe to 
minimize sample losses. Between sampling runs, keep brushes clean and 
protected from contamination.
    8.7.6.2.5 After ensuring that all joints have been wiped clean of 
silicone grease, 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 times or more if needed to remove 
visible particulate. Make a final rinse of the brush and filter holder. 
Carefully rinse out the glass cyclone also (if applicable).
    8.7.6.2.6 After rinsing the nozzle, probe, and front half of the 
filter holder with acetone, repeat the entire procedure with methylene 
chloride and save in a separate No. 2M container.
    8.7.6.2.7 After acetone and methylene chloride washings and PM have 
been collected in the proper sample containers, tighten the lid on the 
sample containers so that acetone and methylene chloride 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 each 
container to identify clearly its contents.
    8.7.6.3 Container No. 3. 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 container. A funnel may make it 
easier to pour the silica gel without spilling. A rubber policeman may 
be used as an aid in removing 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, follow the procedure for Container No. 3 in section 11.2.3 
of this method.
    8.7.6.4 Impinger water. Treat the impingers as follows:
    8.7.6.4.1 Make a notation of any color or film in the liquid catch. 
Measure the liquid that is in the 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 the effluent gas.
    8.7.6.4.2 Following the determination of the volume of liquid 
present, rinse the back half of the train with water, add it to the 
impinger catch, and store it in a container labeled 3W (water).
    8.7.6.4.3 Following the water rinse, rinse the back half of the 
train with acetone to remove the excess water to enhance subsequent 
organic recovery with methylene chloride and quantitatively recover to a 
container labeled 3S (solvent) followed by at least three sequential 
rinsings with aliquots of methylene chloride. Quantitatively recover to 
the same container labeled 3S. Record separately the amount of both 
acetone and methylene chloride used to the nearest 1 ml or 0.5g.

    Note: Because the subsequent analytical finish is gravimetric, it is 
okay to recover both solvents to the same container. This would not be 
recommended if other analytical finishes were required.

    8.8 Sample transport. Whenever possible, containers should be 
shipped in such a way that they remain upright at all times.

                          9.0 Quality Control.

    9.1 Miscellaneous quality control measures.

------------------------------------------------------------------------
                                    Quality control
             Section                    measure             Effect
------------------------------------------------------------------------
8.4, 10.1-10.6..................  Sampling and        Ensure accurate
                                   equipment leak      measurement of
                                   check and           stack gas flow
                                   calibration.        rate, sample
                                                       volume.
------------------------------------------------------------------------

    9.2 Volume metering system checks. The following quality control 
procedures are suggested to check the volume metering system

[[Page 274]]

calibration values at the field test site prior to sample collection. 
These procedures are optional.
    9.2.1 Meter orifice check. Using the calibration data obtained 
during the calibration procedure described in section 10.3 of this 
method, determine the [Delta]Ha for the metering system 
orifice. The [Delta]Ha is the orifice pressure differential 
in units of in. H20 that correlates to 0.75 cfm of air at 528 
[deg]R and 29.92 in. Hg. The [Delta]Ha is calculated as 
follows:
[GRAPHIC] [TIFF OMITTED] TR07OC97.008

Where

0.0319 = (0.0567 in. Hg/ [deg]R)(0.75 cfm)\2\;
[Delta]H = Average pressure differential across the orifice meter, in. 
H20;
Tm = Absolute average DGM temperature, [deg]R;
[Theta] = Total sampling time, min;
Pbar = Barometric pressure, in. Hg;
Y = DGM calibration factor, dimensionless;
Vm = Volume of gas sample as measured by DGM, dcf.

    9.2.1.1 Before beginning the field test (a set of three runs usually 
constitutes a field test), operate the metering system (i.e., pump, 
volume meter, and orifice) at the [Delta]Ha pressure 
differential for 10 minutes. Record the volume collected, the DGM 
temperature, and the barometric pressure. Calculate a DGM calibration 
check value, Yc, as follows:
[GRAPHIC] [TIFF OMITTED] TR07OC97.009

Where

Yc = DGM calibration check value, dimensionless;
10 = Run time, min.

    9.2.1.2 Compare the Yc value with the dry gas meter 
calibration factor Y to determine that: 0.97 Y < Yc < 1.03Y. 
If the Yc value is not within this range, the volume metering 
system should be investigated before beginning the test.
    9.2.2 Calibrated critical orifice. A calibrated critical orifice, 
calibrated against a wet test meter or spirometer and designed to be 
inserted at the inlet of the sampling meter box, may be used as a 
quality control check by following the procedure of section 16.2 of this 
method.

                  10.0 Calibration and Standardization.

    Note: Maintain a laboratory log of all calibrations.

    10.1 Probe nozzle. Probe nozzles shall be calibrated before their 
initial use in the field. Using a micrometer, measure the ID 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 (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.
    10.2 Pitot tube assembly. The Type S pitot tube assembly shall be 
calibrated according to the procedure outlined in section 10.1 of Method 
2, 40 CFR part 60, appendix A.
    10.3 Metering system.
    10.3.1 Calibration prior to use. Before its initial use in the 
field, the metering system shall be calibrated as follows: Connect the 
metering system inlet to the outlet of a wet test meter that is accurate 
to within 1 percent. Refer to Figure 5-5 of Method 5, 40 CFR part 60, 
appendix A. The wet test meter should have a capacity of 30 liters/
revolution (1 ft3/rev). A spirometer of 400 liters (14 
ft3) or more capacity, or equivalent, may be used for this 
calibration, although a wet test meter is usually more practical. The 
wet test meter should be periodically calibrated with a spirometer or a 
liquid displacement meter to ensure the accuracy of the wet test meter. 
Spirometers or wet test meters of other sizes may be used, provided that 
the specified accuracies of the procedure are maintained. Run the 
metering system pump for about 15 minutes with the orifice manometer 
indicating a median reading, as expected in field use, to allow the pump 
to warm up and to permit the interior surface of the wet test meter to 
be thoroughly wetted. Then, at each of a minimum of three orifice 
manometer settings, pass an exact quantity of gas through the wet test 
meter and note the gas volume indicated by the DGM. Also note the 
barometric pressure and the temperatures of the wet test meter, the 
inlet of the DGM, and the outlet of the DGM. Select the highest and 
lowest orifice settings to bracket the expected field operating range of 
the orifice. Use a minimum volume of 0.15 m3 (5 cf) at all 
orifice settings. Record all the data on a form similar to Figure 5-6 of 
Method 5, 40 CFR part 60, appendix A, and calculate Y (the DGM 
calibration factor) and [Delta]Ha (the

[[Page 275]]

orifice calibration factor) at each orifice setting, as shown on Figure 
5-6 of Method 5, 40 CFR part 60, appendix A. Allowable tolerances for 
individual Y and [Delta]Ha values are given in Figure 5-6 of 
Method 5, 40 CFR part 60, appendix A. Use the average of the Y values in 
the calculations in section 12 of this method.
    10.3.1.1 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 m3/min 
(0.02 cfm); at the end of the run, take the difference of the measured 
wet test meter and DGM volumes; divide the difference by 10 to get the 
leak rate. The leak rate should not exceed 0.00057 m3/min 
(0.02 cfm).
    10.3.2 Calibration after use. 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 DGM calibration factor. If the value has changed by more than 5 
percent, recalibrate the meter over the full range of orifice settings, 
as previously detailed.

    Note: Alternative procedures, e.g., rechecking the orifice meter 
coefficient, may be used, subject to the approval of the Administrator.

    10.3.3 Acceptable variation in calibration. If the DGM coefficient 
values obtained before and after a test series differ by more than 5 
percent, either the test series shall 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.
    10.4 Probe heater calibration. Use a heat source to generate air 
heated to selected temperatures that approximate those expected to occur 
in the sources to be sampled. Pass this air through the probe at a 
typical sample flow rate while measuring the probe inlet and outlet 
temperatures at various probe heater settings. For each air temperature 
generated, construct a graph of probe heating system setting versus 
probe outlet temperature. The procedure outlined in APTD-0576 can also 
be used. Probes constructed according to APTD-0581 need not be 
calibrated if the calibration curves in APTD-0576 are used. Also, probes 
with outlet temperature monitoring capabilities do not require 
calibration.

    Note: The probe heating system shall be calibrated before its 
initial use in the field.

    10.5 Temperature sensors. Use the procedure in section 10.3 of 
Method 2, 40 CFR part 60, appendix A to calibrate in-stack temperature 
sensors. Dial thermometers, such as are used for the DGM and condenser 
outlet, shall be calibrated against mercury-in-glass thermometers.
    10.6 Barometer. Calibrate against a mercury barometer.

                       11.0 Analytical Procedure.

    11.1 Record the data required on a sheet such as the one shown in 
Figure 315-1 of this method.
    11.2 Handle each sample container as follows:
    11.2.1 Container No. 1.
    11.2.1.1 PM analysis. Leave the contents in the shipping container 
or transfer the filter and any loose PM from the sample container to a 
tared glass weighing dish. Desiccate for 24 hours in a desiccator 
containing anhydrous calcium sulfate. Weigh to a constant weight and 
report the results to the nearest 0.1 mg. For purposes of this section, 
the term ``constant weight'' means a difference 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 (overnight desiccation is a common 
practice). If a third weighing is required and it agrees within 0.5 mg, then the results of the second weighing should 
be used. For quality assurance purposes, record and report each 
individual weighing; if more than three weighings are required, note 
this in the results for the subsequent MCEM results.
    11.2.1.2 MCEM analysis. Transfer the filter and contents 
quantitatively into a beaker. Add 100 ml of methylene chloride and cover 
with aluminum foil. Sonicate for 3 minutes then allow to stand for 20 
minutes. Set up the filtration apparatus. Decant the solution into a 
clean Buchner fritted funnel. Immediately pressure filter the solution 
through the tube into another clean, dry beaker. Continue decanting and 
pressure filtration until all the solvent is transferred. Rinse the 
beaker and filter with 10 to 20 ml methylene chloride, decant into the 
Buchner fritted funnel and pressure filter. Place the beaker on a low-
temperature hot plate (maximum 40 [deg]C) and slowly evaporate almost to 
dryness. Transfer the remaining last few milliliters of solution 
quantitatively from the beaker (using at least three aliquots of 
methylene chloride rinse) to a tared clean dry aluminum dish and 
evaporate to complete dryness. Remove from heat once solvent is 
evaporated. Reweigh the dish after a 30-minute equilibrium in the 
balance room and determine the weight to the nearest 0.1 mg. Conduct a 
methylene chloride blank run in an identical fashion.
    11.2.2 Container No. 2.

[[Page 276]]

    11.2.2.1 PM analysis. Note the level of liquid in the container, and 
confirm on the analysis sheet whether 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 gravimetrically to 
10.5 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.
    11.2.2.2 MCEM analysis. Add 25 ml methylene chloride to the beaker 
and cover with aluminum foil. Sonicate for 3 minutes then allow to stand 
for 20 minutes; combine with contents of Container No. 2M and pressure 
filter and evaporate as described for Container 1 in section 11.2.1.2 of 
this method.

                         Notes for MCEM Analysis

    1. Light finger pressure only is necessary on 24/40 adaptor. A 
Chemplast adapter 15055-240 has been found satisfactory.
    2. Avoid aluminum dishes made with fluted sides, as these may 
promote solvent ``creep,'' resulting in possible sample loss.
    3. If multiple samples are being run, rinse the Buchner fritted 
funnel twice between samples with 5 ml solvent using pressure 
filtration. After the second rinse, continue the flow of air until the 
glass frit is completely dry. Clean the Buchner fritted funnels 
thoroughly after filtering five or six samples.

    11.2.3 Container No. 3. 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.
    11.2.4 Container 3W (impinger water).
    11.2.4.1 MCEM analysis. Transfer the solution into a 1,000 ml 
separatory funnel quantitatively with methylene chloride washes. Add 
enough solvent to total approximately 50 ml, if necessary. Shake the 
funnel for 1 minute, allow the phases to separate, and drain the solvent 
layer into a 250 ml beaker. Repeat the extraction twice. Evaporate with 
low heat (less than 40 [deg]C) until near dryness. Transfer the 
remaining few milliliters of solvent quantitatively with small solvent 
washes into a clean, dry, tared aluminum dish and evaporate to dryness. 
Remove from heat once solvent is evaporated. Reweigh the dish after a 
30-minute equilibration in the balance room and determine the weight to 
the nearest 0.1 mg.

    11.2.5 Container 3S (solvent).
    11.2.5.1 MCEM analysis. Transfer the mixed solvent to 250 ml 
beaker(s). Evaporate and weigh following the procedures detailed for 
container 3W in section 11.2.4 of this method.
    11.2.6 Blank containers. Measure the distilled water, acetone, or 
methylene chloride in each container either volumetrically or 
gravimetrically. Transfer the ``solvent'' to a tared 250 ml beaker, and 
evaporate to dryness at ambient temperature and pressure. (Conduct a 
solvent blank on the distilled deionized water blank in an identical 
fashion to that described in section 11.2.4.1 of this method.) Desiccate 
for 24 hours, and weigh to a constant weight. Report the results to the 
nearest 0.l mg.

    Note: The contents of Containers No. 2, 3W, and 3M as well as the 
blank containers may be evaporated at temperatures higher than ambient. 
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 and methylene chloride are highly flammable 
and have a low flash point.

                  12.0 Data Analysis and Calculations.

    12.1 Carry out calculations, retaining 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.
    12.2 Nomenclature.

An = Cross-sectional area of nozzle, m3 
(ft3).
Bws = Water vapor in the gas stream, proportion by volume.
Ca = Acetone blank residue concentration, mg/g.
Cs = Concentration of particulate matter in stack gas, dry 
basis, corrected to standard conditions, g/dscm (g/dscf).
I = Percent of isokinetic sampling.
La = Maximum acceptable leakage rate for either a pretest 
leak check or for a leak check following a component change; equal to 
0.00057 m3/min (0.02 cfm) or 4 percent of the average 
sampling rate, whichever is less.
Li = Individual leakage rate observed during the leak check 
conducted prior to the ``ith'' component change (I = l, 2, 
3...n), m3/min (cfm).
Lp = Leakage rate observed during the post-test leak check, 
m3/min (cfm).
ma = Mass of residue of acetone after evaporation, mg.
mn = Total amount of particulate matter collected, mg.
Mw = Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-
mole).
Pbar = Barometric pressure at the sampling site, mm Hg (in 
Hg).
Ps = Absolute stack gas pressure, mm Hg (in. Hg).

[[Page 277]]

Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R = Ideal gas constant, 0.06236 [(mm Hg)(m3)]/[( [deg]K) (g-
mole)] '61' 21.85 [(in. Hg)(ft3)]/[( [deg]R)(lb-mole)'61' ].
Tm = Absolute average dry gas meter (DGM) temperature (see 
Figure 5-2 of Method 5, 40 CFR part 60, appendix A), [deg]K ( [deg]R).
Ts = Absolute average stack gas temperature (see Figure 5-2 
of Method 5, 40 CFR part 60, appendix A), [deg]K( [deg]R).
Tstd = Standard absolute temperature, 293 [deg]K (528 
[deg]R).
Va = Volume of acetone blank, ml.
Vaw = Volume of acetone used in wash, ml.
Vt = Volume of methylene chloride blank, ml.
Vtw = Volume of methylene chloride used in wash, ml.
Vlc = Total volume liquid collected in impingers and silica 
gel (see Figure 5-3 of Method 5, 40 CFR part 60, appendix A), ml.
Vm = Volume of gas sample as measured by dry gas meter, dcm 
(dcf).
Vm(std) = Volume of gas sample measured by the dry gas meter, 
corrected to standard conditions, dscm (dscf).
Vw(std) = Volume of water vapor in the gas sample, corrected 
to standard conditions, scm (scf).
Vs = Stack gas velocity, calculated by Equation 2-9 in Method 
2, 40 CFR part 60, appendix A, using data obtained from Method 5, 40 CFR 
part 60, appendix A, m/sec (ft/sec).
Wa = Weight of residue in acetone wash, mg.
Y = Dry gas meter calibration factor.
[Delta]H = Average pressure differential across the orifice meter (see 
Figure 5-2 of Method 5, 40 CFR part 60, appendix A), mm H2O 
(in H2O).
[rho]a = Density of acetone, 785.1 mg/ml (or see label on 
bottle).
[rho]w = Density of water, 0.9982 g/ml (0.00220l lb/ml).
[rho]t = Density of methylene chloride, 1316.8 mg/ml (or see 
label on bottle).
[Theta] = Total sampling time, min.
[Theta]1 = Sampling time interval, from the beginning of a 
run until the first component change, min.
[Theta]1 = Sampling time interval, between two successive 
component changes, beginning with the interval between the first and 
second changes, min.
[Theta]p = Sampling time interval, from the final 
(nth) component change until the end of the sampling run, 
min.
13.6 = Specific gravity of mercury.
60 = Sec/min.
100 = Conversion to percent.

    12.3 Average dry gas meter temperature and average orifice pressure 
drop. See data sheet (Figure 5-2 of Method 5, 40 CFR part 60, appendix 
A).
    12.4 Dry gas volume. Correct the sample volume measured by the dry 
gas meter to standard conditions (20 [deg]C, 760 mm Hg or 68 [deg]F, 
29.92 in Hg) by using Equation 315-1.
[GRAPHIC] [TIFF OMITTED] TR07OC97.010

Where

Kl = 0.3858 [deg]K/mm Hg for metric units,
= 17.64 [deg]R/in Hg for English units.

    Note: Equation 315-1 can be used as written unless the leakage rate 
observed during any of the mandatory leak checks (i.e., the post-test 
leak check or leak checks conducted prior to component changes) exceeds 
La. If Lp or Li exceeds La, 
Equation 315-1 must be modified as follows:
    (a) Case I. No component changes made during sampling run. In this 
case, replace Vm in Equation 315-1 with the expression:

[Vm--(Lp--La) [Theta]]

    (b) Case II. One or more component changes made during the sampling 
run. In this case, replace Vm in Equation 315-1 by the 
expression:
[GRAPHIC] [TIFF OMITTED] TR07OC97.011

and substitute only for those leakage rates (Li or 
Lp) which exceed La.
    12.5 Volume of water vapor condensed.

[[Page 278]]

[GRAPHIC] [TIFF OMITTED] TR07OC97.012

Where

K2 = 0.001333 m3/ml for metric units;
= 0.04706 ft3/ml for English units.

12.6 Moisture content.
[GRAPHIC] [TIFF OMITTED] TR07OC97.013

    Note: In saturated or water droplet-laden gas streams, two 
calculations of the moisture content of the stack gas shall be made, one 
from the impinger analysis (Equation 315-3), and a second from the 
assumption of saturated conditions. The lower of the two values of 
Bws shall be considered correct. The procedure for 
determining the moisture content based upon assumption of saturated 
conditions is given in section 4.0 of Method 4, 40 CFR part 60, appendix 
A. For the purposes of this method, the average stack gas temperature 
from Figure 5-2 of Method 5, 40 CFR part 60, appendix A may be used to 
make this determination, provided that the accuracy of the in-stack 
temperature sensor is 1 [deg]C (2 [deg]F).

    12.7 Acetone blank concentration.
    [GRAPHIC] [TIFF OMITTED] TR07OC97.014
    
    12.8 Acetone wash blank.

Wa = Ca Vaw [rho]a Eq. 315-5

    12.9 Total particulate weight. Determine the total PM catch from the 
sum of the weights obtained from Containers l and 2 less the acetone 
blank associated with these two containers (see Figure 315-1).

    Note: Refer to section 8.5.8 of this method to assist in calculation 
of results involving two or more filter assemblies or two or more 
sampling trains.

    12.10 Particulate concentration.

cs = K3 mn/Vm(std) Eq. 315-6

where

K = 0.001 g/mg for metric units;
= 0.0154 gr/mg for English units.

    12.11 Conversion factors.

------------------------------------------------------------------------
              From                       To              Multiply by
------------------------------------------------------------------------
ft \3\.........................  m \3\............  0.02832
gr.............................  mg...............  64.80004
gr/ft\3\.......................  mg/m\3\..........  2288.4
mg.............................  g................  0.001
gr.............................  lb...............  1.429x10-4
------------------------------------------------------------------------

    12.12 Isokinetic variation.
    12.12.1 Calculation from raw data.
    [GRAPHIC] [TIFF OMITTED] TR07OC97.015
    
where

K4 = 0.003454 [(mm Hg)(m3)]/[(m1)( [deg]K)] for 
metric units;
= 0.002669 [(in Hg)(ft3)]/[(m1)( [deg]R)] for English units.

    12.12.2 Calculation from intermediate values.
    [GRAPHIC] [TIFF OMITTED] TR07OC97.016
    
where

K5 = 4.320 for metric units;
= 0.09450 for English units.

    12.12.3 Acceptable results. If 90 percent <= I <= 110 percent, the 
results are acceptable. If

[[Page 279]]

the PM or MCEM results are low in comparison to the standard, and ``I'' 
is over 110 percent or less than 90 percent, the Administrator may opt 
to accept the results. Reference 4 in the Bibliography may be used to 
make acceptability judgments. If ``I'' is judged to be unacceptable, 
reject the results, and repeat the test.
    12.13 Stack gas velocity and volumetric flow rate. Calculate the 
average stack gas velocity and volumetric flow rate, if needed, using 
data obtained in this method and the equations in sections 5.2 and 5.3 
of Method 2, 40 CFR part 60, appendix A.
    12.14 MCEM results. Determine the MCEM concentration from the 
results from Containers 1, 2, 2M, 3W, and 3S less the acetone, methylene 
chloride, and filter blanks value as determined in the following 
equation:

mmcem = Smtotal - wa - wt - fb

    13.0 Method Performance. [Reserved]
    14.0 Pollution Prevention. [Reserved]
    15.0 Waste Management. [Reserved]
    16.0 Alternative Procedures.
    16.1 Dry gas meter as a calibration standard. A DGM may be used as a 
calibration standard for volume measurements in place of the wet test 
meter specified in section 16.1 of this method, provided that it is 
calibrated initially and recalibrated periodically as follows:
    16.1.1 Standard dry gas meter calibration.
    16.1.1.1. The DGM to be calibrated and used as a secondary reference 
meter should be of high quality and have an appropriately sized 
capacity, e.g., 3 liters/rev (0.1 ft \3\/rev). A spirometer (400 liters 
or more capacity), or equivalent, may be used for this calibration, 
although a wet test meter is usually more practical. The wet test meter 
should have a capacity of 30 liters/rev (1 ft \3\/rev) and be capable of 
measuring volume to within 1.0 percent; wet test meters should be 
checked against a spirometer or a liquid displacement meter to ensure 
the accuracy of the wet test meter. Spirometers or wet test meters of 
other sizes may be used, provided that the specified accuracies of the 
procedure are maintained.
    16.1.1.2 Set up the components as shown in Figure 5-7 of Method 5, 
40 CFR part 60, appendix A. A spirometer, or equivalent, may be used in 
place of the wet test meter in the system. Run the pump for at least 5 
minutes at a flow rate of about 10 liters/min (0.35 cfm) to condition 
the interior surface of the wet test meter. The pressure drop indicated 
by the manometer at the inlet side of the DGM should be minimized (no 
greater than 100 mm H2O [4 in. H2O] at a flow rate 
of 30 liters/min [1 cfm]). This can be accomplished by using large-
diameter tubing connections and straight pipe fittings.
    16.1.1.3 Collect the data as shown in the example data sheet (see 
Figure 5-8 of Method 5, 40 CFR part 60, appendix A). Make triplicate 
runs at each of the flow rates and at no less than five different flow 
rates. The range of flow rates should be between 10 and 34 liters/min 
(0.35 and 1.2 cfm) or over the expected operating range.
    16.1.1.4 Calculate flow rate, Q, for each run using the wet test 
meter volume, Vw, and the run time, q. Calculate the DGM 
coefficient, Yds, for each run. These calculations are as 
follows:
[GRAPHIC] [TIFF OMITTED] TR07OC97.017

[GRAPHIC] [TIFF OMITTED] TR07OC97.018

Where

K1 = 0.3858 for international system of units (SI); 17.64 for 
English units;
Pbar = Barometric pressure, mm Hg (in Hg);
Vw = Wet test meter volume, liter (ft\3\);
tw = Average wet test meter temperature, [deg]C ( [deg]F);
tstd = 273 [deg]C for SI units; 460 [deg]F for English units;
[Theta] = Run time, min;
tds = Average dry gas meter temperature, [deg]C ( [deg]F);
Vds = Dry gas meter volume, liter (ft\3\);
[Delta]p = Dry gas meter inlet differential pressure, mm H2O 
(in H2O).

    16.1.1.5 Compare the three Yds values at each of the flow 
rates and determine the maximum and minimum values. The difference 
between the maximum and minimum values at each flow rate should be no 
greater than 0.030. Extra sets of triplicate runs may be made in order 
to complete this requirement. In addition, the meter coefficients

[[Page 280]]

should be between 0.95 and 1.05. If these specifications cannot be met 
in three sets of successive triplicate runs, the meter is not suitable 
as a calibration standard and should not be used as such. If these 
specifications are met, average the three Yds values at each 
flow rate resulting in five average meter coefficients, Yds.
    16.1.1.6 Prepare a curve of meter coefficient, Yds, 
versus flow rate, Q, for the DGM. This curve shall be used as a 
reference when the meter is used to calibrate other DGMs and to 
determine whether recalibration is required.
    16.1.2 Standard dry gas meter recalibration.
    16.1.2.1 Recalibrate the standard DGM against a wet test meter or 
spirometer annually or after every 200 hours of operation, whichever 
comes first. This requirement is valid provided the standard DGM is kept 
in a laboratory and, if transported, cared for as any other laboratory 
instrument. Abuse to the standard meter may cause a change in the 
calibration and will require more frequent recalibrations.
    16.1.2.2 As an alternative to full recalibration, a two-point 
calibration check may be made. Follow the same procedure and equipment 
arrangement as for a full recalibration, but run the meter at only two 
flow rates (suggested rates are 14 and 28 liters/min [0.5 and 1.0 cfm]). 
Calculate the meter coefficients for these two points, and compare the 
values with the meter calibration curve. If the two coefficients are 
within 1.5 percent of the calibration curve values at the same flow 
rates, the meter need not be recalibrated until the next date for a 
recalibration check.
    6.2 Critical orifices as calibration standards. Critical orifices 
may be used as calibration standards in place of the wet test meter 
specified in section 10.3 of this method, provided that they are 
selected, calibrated, and used as follows:
    16.2.1 Selection of critical orifices.
    16.2.1.1 The procedure that follows describes the use of hypodermic 
needles or stainless steel needle tubing that has been found suitable 
for use as critical orifices. Other materials and critical orifice 
designs may be used provided the orifices act as true critical orifices; 
i.e., a critical vacuum can be obtained, as described in section 
7.2.2.2.3 of Method 5, 40 CFR part 60, appendix A. Select five critical 
orifices that are appropriately sized to cover the range of flow rates 
between 10 and 34 liters/min or the expected operating range. Two of the 
critical orifices should bracket the expected operating range. A minimum 
of three critical orifices will be needed to calibrate a Method 5 DGM; 
the other two critical orifices can serve as spares and provide better 
selection for bracketing the range of operating flow rates. The needle 
sizes and tubing lengths shown in Table 315-1 give the approximate flow 
rates indicated in the table.
    16.2.1.2 These needles can be adapted to a Method 5 type sampling 
train as follows: Insert a serum bottle stopper, 13x20 mm sleeve type, 
into a 0.5 in Swagelok quick connect. Insert the needle into the stopper 
as shown in Figure 5-9 of Method 5, 40 CFR part 60, appendix A.
    16.2.2 Critical orifice calibration. The procedure described in this 
section uses the Method 5 meter box configuration with a DGM as 
described in section 6.1.1.9 of this method to calibrate the critical 
orifices. Other schemes may be used, subject to the approval of the 
Administrator.
    16.2.2.1 Calibration of meter box. The critical orifices must be 
calibrated in the same configuration as they will be used; i.e., there 
should be no connections to the inlet of the orifice.
    16.2.2.1.1 Before calibrating the meter box, leak-check the system 
as follows: Fully open the coarse adjust valve and completely close the 
bypass valve. Plug the inlet. Then turn on the pump and determine 
whether there is any leakage. The leakage rate shall be zero; i.e., no 
detectable movement of the DGM dial shall be seen for 1 minute.
    16.2.2.1.2 Check also for leakages in that portion of the sampling 
train between the pump and the orifice meter. See section 5.6 of Method 
5, 40 CFR part 60, appendix A for the procedure; make any corrections, 
if necessary. If leakage is detected, check for cracked gaskets, loose 
fittings, worn 0-rings, etc. and make the necessary repairs.
    16.2.2.1.3 After determining that the meter box is leakless, 
calibrate the meter box according to the procedure given in section 5.3 
of Method 5, 40 CFR part 60, appendix A. Make sure that the wet test 
meter meets the requirements stated in section 7.1.1.1 of Method 5, 40 
CFR part 60, appendix A. Check the water level in the wet test meter. 
Record the DGM calibration factor, Y.
    16.2.2.2 Calibration of critical orifices. Set up the apparatus as 
shown in Figure 5-10 of Method 5, 40 CFR part 60, appendix A.
    16.2.2.2.1 Allow a warm-up time of 15 minutes. This step is 
important to equilibrate the temperature conditions through the DGM.
    16.2.2.2.2 Leak-check the system as in section 7.2.2.1.1 of Method 
5, 40 CFR part 60, appendix A. The leakage rate shall be zero.
    16.2.2.2.3 Before calibrating the critical orifice, determine its 
suitability and the appropriate operating vacuum as follows: turn on the 
pump, fully open the coarse adjust valve, and adjust the bypass valve to 
give a vacuum reading corresponding to about half of atmospheric 
pressure. Observe the meter box orifice manometer reading, DH. Slowly 
increase the vacuum reading until a stable reading is obtained on the 
meter box orifice manometer. Record the critical vacuum for

[[Page 281]]

each orifice. Orifices that do not reach a critical value shall not be 
used.
    16.2.2.2.4 Obtain the barometric pressure using a barometer as 
described in section 6.1.2 of this method. Record the barometric 
pressure, Pbar, in mm Hg (in. Hg).
    16.2.2.2.5 Conduct duplicate runs at a vacuum of 25 to 50 mm Hg (1 
to 2 in. Hg) above the critical vacuum. The runs shall be at least 5 
minutes each. The DGM volume readings shall be in increments of complete 
revolutions of the DGM. As a guideline, the times should not differ by 
more than 3.0 seconds (this includes allowance for changes in the DGM 
temperatures) to achieve 0.5 percent in K'. Record 
the information listed in Figure 5-11 of Method 5, 40 CFR part 60, 
appendix A.
    16.2.2.2.6 Calculate K' using Equation 315-11.
    [GRAPHIC] [TIFF OMITTED] TR07OC97.019
    
where

K' = Critical orifice coefficient, [m\3\)( [deg]K)1/2]/[(mm 
Hg)(min)] '61' [(ft\3\)( [deg]R)1/2)]/[(in. Hg)(min)]'61'
Tamb = Absolute ambient temperature, [deg]K ( [deg]R).

    16.2.2.2.7 Average the K' values. The individual K' values should 
not differ by more than 0.5 percent from the 
average.
    16.2.3 Using the critical orifices as calibration standards.
    16.2.3.1 Record the barometric pressure.
    16.2.3.2 Calibrate the metering system according to the procedure 
outlined in sections 7.2.2.2.1 to 7.2.2.2.5 of Method 5, 40 CFR part 60, 
appendix A. Record the information listed in Figure 5-12 of Method 5, 40 
CFR part 60, appendix A.
    16.2.3.3 Calculate the standard volumes of air passed through the 
DGM and the critical orifices, and calculate the DGM calibration factor, 
Y, using the equations below:

Vm(std) = K1 Vm [Pbar + 
([Delta]H/13.6)]/Tm Eq. 315-12
Vcr(std) = K' (Pbar [Theta])/
Tamb1/2 Eq. 315-13
Y = Vcr(std)/Vm(std) Eq. 315-14
where

Vcr(std) = Volume of gas sample passed through the critical 
orifice, corrected to standard conditions, dscm (dscf).
K' = 0.3858 [deg]K/mm Hg for metric units
= 17.64 [deg]R/in Hg for English units.

    16.2.3.4 Average the DGM calibration values for each of the flow 
rates. The calibration factor, Y, at each of the flow rates should not 
differ by more than 2 percent from the average.
    16.2.3.5 To determine the need for recalibrating the critical 
orifices, compare the DGM Y factors obtained from two adjacent orifices 
each time a DGM is calibrated; for example, when checking orifice 13/
2.5, use orifices 12/10.2 and 13/5.1. If any critical orifice yields a 
DGM Y factor differing by more than 2 percent from the others, 
recalibrate the critical orifice according to section 7.2.2.2 of Method 
5, 40 CFR part 60, appendix A.
    17.0 References.
    1. Addendum to Specifications for Incinerator Testing at Federal 
Facilities. PHS, NCAPC. December 6, 1967.
    2. Martin, Robert M. Construction Details of Isokinetic Source-
Sampling Equipment. Environmental Protection Agency. Research Triangle 
Park, NC. APTD-0581. April 1971.
    3. Rom, Jerome J. Maintenance, Calibration, and Operation of 
Isokinetic Source Sampling Equipment. Environmental Protection Agency. 
Research Triangle Park, NC. 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 Control Association, St. Louis, MO. June 
14-19, 1970.
    5. Smith, W.S., et al. Stack Gas Sampling Improved and Simplified 
With New Equipment. APCA Paper No. 67-119. 1967.
    6. Specifications for Incinerator Testing at Federal Facilities. 
PHS, NCAPC. 1967.
    7. Shigehara, R.T. Adjustment 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 Commercially Available Instrumentation 
for the Measurement of Low-Range Gas Velocities. U.S. Environmental 
Protection Agency, Emission Measurement Branch. Research Triangle Park, 
NC. November 1976 (unpublished paper).
    9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels; Coal and 
Coke; Atmospheric Analysis. American Society for Testing and Materials. 
Philadelphia, PA. 1974. pp. 617-622.
    10. Felix, L.G., G.I. Clinard, G.E. Lacy, and J.D. McCain. Inertial 
Cascade Impactor Substrate Media for Flue Gas Sampling. U.S. 
Environmental Protection Agency. Research

[[Page 282]]

Triangle Park, NC 27711. Publication No. EPA-600/7-77-060. June 1977. 83 
p.
    11. Westlin, P.R., and R.T. Shigehara. Procedure for Calibrating and 
Using Dry Gas Volume Meters as Calibration Standards. Source Evaluation 
Society Newsletter. 3(1):17-30. February 1978.
    12. Lodge, J.P., Jr., J.B. Pate, B.E. Ammons, and G.A. Swanson. The 
Use of Hypodermic Needles as Critical Orifices in Air Sampling. J. Air 
Pollution Control Association. 16:197-200. 1966.
    18.0 Tables, Diagrams, Flowcharts, and Validation Data

                       TABLE 315-1. Flow Rates for Various Needle Sizes and Tube Lengths.
----------------------------------------------------------------------------------------------------------------
                                                 Flow rate                                            Flow rate
              Gauge/length  (cm)                  (liters/             Gauge/length  (cm)              (liters/
                                                    min)                                                 min)
----------------------------------------------------------------------------------------------------------------
12/7.6........................................        32.56  14/2.5................................        19.54
12/10.2.......................................        30.02  14/5.1................................        17.27
13/2.5........................................        25.77  14/7.6................................        16.14
13/5.1........................................        23.50  15/3.2................................        14.16
13/7.6........................................        22.37  15/7.6................................        11.61
13/10.2.......................................        20.67  115/10.2..............................        10.48
----------------------------------------------------------------------------------------------------------------


               Figure 315-1. Particulate and MCEM Analyses
------------------------------------------------------------------------
 
------------------------------------------------------------------------
                          Particulate Analysis
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½
Plant............................  .....................................
Date.............................  .....................................
Run No...........................  .....................................
Filter No........................  .....................................
Amount liquid lost during          .....................................
 transport.
Acetone blank volume (ml)........  .....................................
Acetone blank concentration (Eq.   .....................................
 315-4) (mg/mg).
Acetone wash blank (Eq. 315-5)     .....................................
 (mg).
------------------------------------------------------------------------


 
                                Final weight   Tare weight   Weight gain
                                    (mg)           (mg)          (mg)
------------------------------------------------------------------------
Container No. 1..............  .............
Container No. 2..............  .............
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½                .............
Less Acetone blank...........  .............
Weight of particulate matter.  .............
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½                 Final volume    Initial
                                                   (mg)      volume (mg)
      Moisture Analysis
------------------------------ Note 1         Note 1
Silica gel...................  .............
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½                .............
 Note 1: Convert volume of
 water to weight by
 multiplying by the density
 of water (1 g/ml).
------------------------------------------------------------------------



 
                                                 Tare of                                            Methylene
          Container No.              Final       aluminum      Weight gain      Acetone wash      chloride wash
                                  weight (mg)   dish (mg)                        volume (ml)       volume (ml)
----------------------------------------------------------------------------------------------------------------
                                                  MCEM Analysis
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½
1...............................  ...........
2+2M............................  ...........
3W..............................  ...........
3S..............................  ...........
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½              ...........  ................  [sum3]mtotal      <3-ln-grk-S>Vaw
----------------------------------------------------------------------------------------------------------------


Less acetone wash blank (mg) (not to exceed 1 mg/l of   wa = capa [sum3]Vaw
 acetone used).
 

[[Page 283]]

 
Less methylene chloride wash blank (mg) (not to exceed  wt = ctpt [sum3]Vtw
 1.5 mg/l of methylene chloride used).
 
Less filter blank (mg) (not to exceed . . . (mg/        Fb
 filter).
 
MCEM weight (mg)......................................  mMCEOM = [sum3]mtotal - wa - wt- fb

   Method 316--Sampling and Analysis for Formaldehyde Emissions From 
  Stationary Sources in the Mineral Wool and Wool Fiberglass Industries

                            1.0 Introduction

    This method is applicable to the determination of formaldehyde, CAS 
Registry number 50-00-0, from stationary sources in the mineral wool and 
wool fiber glass industries. High purity water is used to collect the 
formaldehyde. The formaldehyde concentrations in the stack samples are 
determined using the modified pararosaniline method. Formaldehyde can be 
detected as low as 8.8 x 1010 lbs/cu ft (11.3 ppbv) or as 
high as 1.8 x 103 lbs/cu ft (23,000,000 ppbv), at standard 
conditions over a 1 hour sampling period, sampling approximately 30 cu 
ft.

                          2.0 Summary of Method

    Gaseous and particulate pollutants are withdrawn isokinetically from 
an emission source and are collected in high purity water. Formaldehyde 
present in the emissions is highly soluble in high purity water. The 
high purity water containing formaldehyde is then analyzed using the 
modified pararosaniline method. Formaldehyde in the sample reacts with 
acidic pararosaniline, and the sodium sulfite, forming a purple 
chromophore. The intensity of the purple color, measured 
spectrophotometrically, provides an accurate and precise measure of the 
formaldehyde concentration in the sample.

                             3.0 Definitions

    See the definitions in the General Provisions of this Subpart.

                            4.0 Interferences

    Sulfite and cyanide in solution interfere with the pararosaniline 
method. A procedure to overcome the interference by each compound has 
been described by Miksch, et al.

                         5.0 Safety. (Reserved)

                       6.0 Apparatus and Materials

    6.1 A schematic of the sampling train is shown in Figure 1. This 
sampling train configuration is adapted from EPA Method 5, 40 CFR part 
60, appendix A, procedures.

[[Page 284]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.050

    The sampling train consists of the following components: probe 
nozzle, probe liner, pitot tube, differential pressure gauge, impingers, 
metering system, barometer, and gas density determination equipment.
    6.1.1 Probe Nozzle: Quartz, glass, or stainless steel with sharp, 
tapered (30 [deg] angle) leading edge. The taper shall be on the outside 
to preserve a constant inner diameter. The nozzle shall be buttonhook or 
elbow design. A range of nozzle sizes suitable for isokinetic sampling 
should be available in increments of 0.15 cm (\1/16\ in), e.g., 0.32 to 
1.27 cm (\1/8\ to \1/2\ in), or larger if higher volume sampling trains 
are used. Each nozzle shall be calibrated according to the procedure 
outlined in Section 10.1.
    6.1.2 Probe Liner: Borosilicate glass or quartz shall be used for 
the probe liner. The probe shall be maintained at a temperature of 120 
[deg]C  14 [deg]C (248 [deg]F  25 [deg]F).
    6.1.3 Pitot Tube: The pitot tube shall be Type S, as described in 
Section 2.1 of EPA Method 2, 40 CFR part 60, appendix A, or any other 
appropriate device. The pitot tube shall be attached to the probe to 
allow constant monitoring of the stack gas velocity. The impact (high 
pressure) opening plane of the pitot tube shall be even with or above 
the nozzle entry plane (see Figure 2-6b, EPA Method 2, 40 CFR part 60, 
appendix A) during sampling. The Type S pitot tube assembly shall have a 
known coefficient, determined as outlined in Section 4 of EPA Method 2, 
40 CFR part 60, appendix A.
    6.1.4 Differential Pressure Gauge: The differential pressure gauge 
shall be an inclined manometer or equivalent device as described in 
Section 2.2 of EPA Method 2, 40 CFR part 60, appendix A. One manometer 
shall be used for velocity-head reading and the other for orifice 
differential pressure readings.
    6.1.5 Impingers: The sampling train requires a minimum of four 
impingers, connected as shown in Figure 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 diameters (\1/2\ in) glass tube extending to 1.3 cm 
(\1/2\ in) from the bottom of the flask. For the second impinger, use a 
Greenburg-Smith impinger with the standard tip. Place a thermometer 
capable of measuring temperature

[[Page 285]]

to within 1 [deg]C (2 [deg]F) at the outlet of the fourth impinger for 
monitoring purposes.
    6.1.6 Metering System: The necessary components are a vacuum gauge, 
leak-free pump, thermometers capable of measuring temperatures within 3 
[deg]C (5.4 [deg]F), dry-gas meter capable of measuring volume to within 
1 percent, and related equipment as shown in Figure 1. At a minimum, the 
pump should be capable of 4 cfm free flow, and the dry gas meter should 
have a recording capacity of 0-999.9 cu ft with a resolution of 0.005 cu 
ft. Other metering systems may be used which are capable of maintaining 
sample volumes to within 2 percent. The metering system may be used in 
conjunction with a pitot tube to enable checks of isokinetic sampling 
rates.
    6.1.7 Barometer: The barometer may be mercury, aneroid, or other 
barometer 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) is requested and an 
adjustment for elevation differences between the weather station and 
sampling point is applied at a rate of minus 2.5 mm Hg (0.1 in Hg) per 
30 m (100 ft) elevation increase (rate is plus 2.5 mm Hg per 30 m (100 
ft) of elevation decrease).
    6.1.8 Gas Density Determination Equipment: Temperature sensor and 
pressure gauge (as described in Sections 2.3 and 2.3 of EPA Method 2, 40 
CFR part 60, appendix A), and gas analyzer, if necessary (as described 
in EPA Method 3, 40 CFR part 60, appendix A). The temperature sensor 
ideally should be permanently attached to the pitot tube or sampling 
probe in a fixed configuration such that the top 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 openings (see Figure 2-7, EPA Method 2, 
40 CFR part 60, appendix A). As a second alternative, if a difference of 
no 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.

                           6.2 Sample Recovery

    6.2.1 Probe Liner: Probe nozzle and brushes; bristle brushes with 
stainless steel wire handles are required. The probe brush shall have 
extensions of stainless steel, Teflon TM, or inert material 
at least as long as the probe. The brushes shall be properly sized and 
shaped to brush out the probe liner, the probe nozzle, and the 
impingers.
    6.2.2 Wash Bottles: One wash bottle is required. Polyethylene, 
Teflon TM, or glass wash bottles may be used for sample 
recovery.
    6.2.3 Graduated Cylinder and/or Balance: A graduated cylinder or 
balance is required to measure condensed water to the nearest 1 ml or 1 
g. Graduated cylinders shall have division not 2 ml. 
Laboratory balances capable of weighing to  0.5 g 
are required.
    6.2.4 Polyethylene Storage Containers: 500 ml wide-mouth 
polyethylene bottles are required to store impinger water samples.
    6.2.5 Rubber Policeman and Funnel: A rubber policeman and funnel are 
required to aid the transfer of material into and out of containers in 
the field.

                           6.3 Sample Analysis

    6.3.1 Spectrophotometer--B&L 70, 710, 2000, etc., or equivalent; 1 
cm pathlength cuvette holder.
    6.3.2 Disposable polystyrene cuvettes, pathlengh 1 cm, volume of 
about 4.5 ml.
    6.3.3 Pipettors--Fixed-volume Oxford pipet (250 [mu]l; 500 [mu]l; 
1000 [mu]l); adjustable volume Oxford or equivalent pipettor 1-5 ml 
model, set to 2.50 ml.
    6.3.4 Pipet tips for pipettors above.
    6.3.5 Parafilm, 2 [deg] wide; cut into about 1'' squares.

                              7.0 Reagents

    7.1 High purity water: All references to water in this method refer 
to high purity water (ASTM Type I water or equivalent). The water purity 
will dictate the lower limits of formaldehyde quantification.
    7.2 Silica Gel: Silica gel shall be indicting type, 6-16 mesh. If 
the silica gel has been used previously, dry at 175 [deg]C (350 [deg]F) 
for 2 hours before using. New silica gel may be used as received. 
Alternatively, other types of desiccants (equivalent or better) may be 
used.
    7.3 Crushed Ice: Quantities ranging from 10-50 lbs may be necessary 
during a sampling run, depending upon ambient temperature. Samples which 
have been taken must be stored and shipped cold; sufficient ice for this 
purpose must be allowed.
    7.4 Quaternary ammonium compound stock solution: Prepare a stock 
solution of dodecyltrimethylammonium chloride (98 percent minimum assay, 
reagent grade) by dissolving 1.0 gram in 1000 ml water. This solution 
contains nominally 1000 [mu]g/ml quaternary ammonium compound, and is 
used as a biocide for some sources which are prone to microbial 
contamination.
    7.5 Pararosaniline: Weigh 0.16 grams pararosaniline (free base; 
assay of 95 percent or greater, C.I. 42500; Sigma P7632 has been found 
to be acceptable) into a 100 ml flask. Exercise care, since 
pararosaniline is a dye and will stain. Using a wash bottle with

[[Page 286]]

high-purity water, rinse the walls of the flask. Add no more than 25 ml 
water. Then, carefully add 20 ml of concentrated hydrochloric acid to 
the flask. The flask will become warm after the addition of acid. Add a 
magnetic stir bar to the flask, cap, and place on a magnetic stirrer for 
approximately 4 hours. Then, add additional water so the total volume is 
100 ml. This solution is stable for several months when stored tightly 
capped at room temperature.
    7.6 Sodium sulfite: Weigh 0.10 grams anhydrous sodium sulfite into a 
100 ml flask. Dilute to the mark with high purity water. Invert 15-20 
times to mix and dissolve the sodium sulfite. This solution must be 
prepared fresh every day.
    7.7 Formaldehyde standard solution: Pipet exactly 2.70 ml of 37 
percent formaldehyde solution into a 1000 ml volumetric flask which 
contains about 500 ml of high-purity water. Dilute to the mark with 
high-purity water. This solution contains nominally 1000 [mu]g/ml of 
formaldehyde, and is used to prepare the working formaldehyde standards. 
The exact formaldehyde concentration may be determined if needed by 
suitable modification of the sodium sulfite method (Reference: J.F. 
Walker, Formaldehyde (Third Edition), 1964.). The 1000 [mu]g/ml 
formaldehyde stock solution is stable for at least a year if kept 
tightly closed, with the neck of the flask sealed with Parafilm. Store 
at room temperature.
    7.8 Working formaldehyde standards: Pipet exactly 10.0 ml of the 
1000 [mu]g/ml formaldehyde stock solution into a 100 ml volumetric flask 
which is about half full of high-purity water. Dilute to the mark with 
high-purity water, and invert 15-20 times to mix thoroughly. This 
solution contains nominally 100 [mu]g/ml formaldehyde. Prepare the 
working standards from this 100 [mu]g/ml standard solution and using the 
Oxford pipets:

------------------------------------------------------------------------
                                                              Volumetric
                                                                flask
                                                  [mu]L or      volume
           Working standard, [mu]/mL             100 [mu]g/   (dilute to
                                                mL solution   mark with
                                                                water)
------------------------------------------------------------------------
0.250.........................................          250          100
0.500.........................................          500          100
1.00..........................................         1000          100
2.00..........................................         2000          100
3.00..........................................         1500           50
------------------------------------------------------------------------

The 100 [mu]g/ml stock solution is stable for 4 weeks if kept 
refrigerated between analyses. The working standards (0.25-3.00 [mu]g/
ml) should be prepared fresh every day, consistent with good laboratory 
practice for trace analysis. If the laboratory water is not of 
sufficient purity, it may be necessary to prepare the working standards 
every day. The laboratory must establish that the working standards are 
stable--DO NOT assume that your working standards are stable for more 
than a day unless you have verified this by actual testing for several 
series of working standards.

                          8.0 Sample Collection

    8.1 Because of the complexity of this method, field personnel should 
be trained in and experienced with the test procedures in order to 
obtain reliable results.

                       8.2 Laboratory Preparation

    8.2.1 All the components shall be maintained and calibrated 
according to the procedure described in APTD-0576, unless otherwise 
specified.
    8.2.2 Weigh several 200 to 300 g portions of silica gel in airtight 
containers to the nearest 0.5 g. Record on each container the total 
weight of the silica gel plus containers. As an alternative to 
preweighing the silica gel, it may instead be weighed directly in the 
impinger or sampling holder just prior to train assembly.

                  8.3 Preliminary Field Determinations

    8.3.1 Select the sampling site and the minimum number of sampling 
points according to EPA Method 1, 40 CFR part 60, appendix A, or other 
relevant criteria. Determine the stack pressure, temperature, and range 
of velocity heads using EPA Method 2, 40 CFR part 60, appendix A. A 
leak-check of the pitot lines according to Section 3.1 of EPA Method 2, 
40 CFR part 60, appendix A, must be performed. Determine the stack gas 
moisture content using EPA Approximation Method 4,40 CFR part 60, 
appendix A, or its alternatives to establish estimates of isokinetic 
sampling rate settings. Determine the stack gas dry molecular weight, as 
described in EPA Method 2, 40 CFR part 60, appendix A, Section 3.6. If 
integrated EPA Method 3, 40 CFR part 60, appendix A, 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 
sample run.
    8.3.2 Select a nozzle size based on the range of velocity heads so 
that it is not necessary to change the nozzle size in order to maintain 
isokinetic sampling rates below 28 l/min (1.0 cfm). During the run do 
not change the nozzle. Ensure that the proper differential pressure 
gauge is chosen for the range of velocity heads encountered (see Section 
2.2 of EPA Method 2, 40 CFR part 60, appendix A).
    8.3.3 Select a suitable probe liner and probe length so that all 
traverse points can be sampled. For large stacks, to reduce the length 
of the probe, consider sampling from opposite sides of the stack.
    8.3.4 A minimum of 30 cu ft of sample volume is suggested for 
emission sources with stack concentrations not greater than 23,000,000 
ppbv. Additional sample volume

[[Page 287]]

shall be collected as necessitated by the capacity of the water reagent 
and analytical detection limit constraint. Reduced sample volume may be 
collected as long as the final concentration of formaldehyde in the 
stack sample is greater than 10 (ten) times the detection limit.
    8.3.5 Determine the total length of sampling time needed to obtain 
the identified minimum volume by comparing the anticipated average 
sampling rate with the volume requirement. Allocate the same time to all 
traverse points defined by EPA Method 1, 40 CFR part 60, appendix A. To 
avoid timekeeping errors, the length of time sampled at each traverse 
point should be an integer or an integer plus 0.5 min.
    8.3.6 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-volume samples. In these cases, careful documentation must be 
maintained in order to allow accurate calculations of concentrations.

                   8.4 Preparation of Collection Train

    8.4.1 During preparation and assembly of the sampling train, keep 
all openings where contamination can occur covered with 
TeflonTM film or aluminum foil until just prior to assembly 
or until sampling is about to begin.
    8.4.2 Place 100 ml of water in each of the first two impingers, and 
leave the third impinger empty. If additional capacity is required for 
high expected concentrations of formaldehyde in the stack gas, 200 ml of 
water per impinger may be used or additional impingers may be used for 
sampling. Transfer approximately 200 to 300 g of pre-weighed silica gel 
from its container to the fourth impinger. Care should be taken to 
ensure that the silica gel is not entrained and carried out from the 
impinger during sampling. Place the silica gel 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 
recorded.
    8.4.3 With a glass or quartz liner, install the selected nozzle 
using a Viton-A O-ring when stack temperatures are <260 [deg]C (500 
[deg]F) and a woven glass-fiber gasket when temperatures are higher. See 
APTD-0576 for details. Other connection systems utilizing either 316 
stainless steel or TeflonTM ferrules may be used. Mark the 
probe with heat-resistant tape or by some other method to denote the 
proper distance into the stack or duct for each sampling point.
    8.4.4 Assemble the train as shown in Figure 1. During assembly, a 
very light coating of silicone grease may be used on ground-glass joints 
of the impingers, but the silicone grease should be limited to the outer 
portion (see APTD-0576) of the ground-glass joints to minimize silicone 
grease contamination. If necessary, TeflonTM tape may be used 
to seal leaks. Connect all temperature sensors to an appropriate 
potentiometer/display unit. Check all temperature sensors at ambient 
temperatures.
    8.4.5 Place crushed ice all around the impingers.
    8.4.6 Turn on and set the probe heating system at the desired 
operating temperature. Allow time for the temperature to stabilize.

                        8.5 Leak-Check Procedures

    8.5.1 Pre-test Leak-check: Recommended, but not required. If the 
tester elects to conduct the pre-test leak-check, the following 
procedure shall be used.
    8.5.1.1 After the sampling train has been assembled, turn on and set 
probe heating system at the desired operating temperature. Allow time 
for the temperature to stabilize. If a Viton-a O-ring or other leak-free 
connection is used in assembling the probe nozzle to the probe liner, 
leak-check the train at the sampling site by plugging the nozzle and 
pulling a 381 mm Hg (15 in Hg) vacuum.

    Note: A lower vacuum may be used, provided that the lower vacuum is 
not exceeded during the test.

    If a woven glass fiber gasket is used, do not connect the probe to 
the train during the leak-check. Instead, leak-check the train by first 
attaching a carbon-filled leak-check impinger to the inlet and then 
plugging the inlet and pulling a 381 mm Hg (15 in Hg) vacuum. (A lower 
vacuum may be used if this lower vacuum is not exceeded during the 
test.) Next connect the probe to the train and leak-check at about 25 mm 
Hg (1 in Hg) vacuum. Alternatively, leak-check the probe with the rest 
of the sampling train in one step at 381 mm Hg (15 in Hg) vacuum. 
Leakage rates in excess of (a) 4 percent of the average sampling rate or 
(b) 0.00057 m3/min (0.02 cfm), whichever is less, are 
unacceptable.
    8.5.1.2 The following leak-check instructions for the sampling train 
described in APTD-0576 and APTD-0581 may be helpful. Start the pump with 
the fine-adjust valve fully open and coarse-valve completely closed. 
Partially open the coarse-adjust valve and slowly close the fine-adjust 
valve until the desired vacuum is reached. Do not reverse direction of 
the fine-adjust valve, as liquid will back up into the train. If the 
desired vacuum is exceeded, either perform the leak-check at this higher 
vacuum or end the leak-check, as described below, and start over.
    8.5.1.3 When the leak-check is completed, first slowly remove the 
plug from the inlet to the probe. When the vacuum drops to 127 mm (5 in) 
Hg or less, immediately close the coarse-adjust valve. Switch off the 
pumping system and reopen the fine-adjust valve. Do not reopen the fine-
adjust valve until the

[[Page 288]]

coarse-adjust valve has been closed to prevent the liquid in the 
impingers from being forced backward in the sampling line and silica gel 
from being entrained backward into the third impinger.
    8.5.2 Leak-checks During Sampling Run:
    8.5.2.1 If, during the sampling run, a component change (e.g., 
impinger) becomes necessary, a leak-check shall be conducted immediately 
after the interruption of sampling and before the change is made. The 
leak-check shall be done according to the procedure described in Section 
10.3.3, except that it shall be done at a vacuum greater than or equal 
to the maximum value recorded up to that point in the test. If the 
leakage rate is found to be no greater than 0.0057 m3/min 
(0.02 cfm) or 4 percent of the average sampling rate (whichever is 
less), the results are acceptable. If a higher leakage rate is obtained, 
the tester must void the sampling run.

    Note: Any correction of the sample volume by calculation reduces the 
integrity of the pollutant concentration data generated and must be 
avoided.

    8.5.2.2 Immediately after component changes, leak-checks are 
optional. If performed, the procedure described in section 8.5.1.1 shall 
be used.
    8.5.3 Post-test Leak-check:
    8.5.3.1 A leak-check is mandatory at the conclusion of each sampling 
run. The leak-check shall be done with the same procedures as the pre-
test leak-check, except that the post-test leak-check shall be conducted 
at a vacuum greater than or equal to the maximum value reached during 
the sampling run. If the leakage rate is found to be no greater than 
0.00057 m3/min (0.02 cfm) or 4 percent of the average 
sampling rate (whichever is less), the results are acceptable. If, 
however, a higher leakage rate is obtained, the tester shall record the 
leakage rate and void the sampling run.

                      8.6 Sampling Train Operation

    8.6.1 During the sampling run, maintain an isokinetic sampling rate 
to within 10 percent of true isokinetic, below 28 l/min (1.0 cfm). 
Maintain a temperature around the probe of 120 [deg]C  14 [deg]C (248 [deg]  25 [deg]F).
    8.6.2 For each run, record the data on a data sheet such as the one 
shown in Figure 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 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 2 at least once at each sample point during each time 
increment and additional readings when significant adjustments (20 
percent variation in velocity 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.

[[Page 289]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.051


[[Page 290]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                Gas sample                   Temperature
                                                                                      Pressure              temperature at dry                  of gas
                                                              Stack      Velocity   differential     Gas         gas meter         Filter      leaving
                                       Sampling   Vacuum   temperature     head        across      sample  --------------------    holder     condenser
        Traverse point number            time      mm Hg       (T )     ([Delta]P)     orifice     volume                       temperature    or last
                                       (e) min.  (in. Hg)    [deg]C (    mm  (in)     meter  mm      m3       Inlet    Outlet      [deg]C (    impinger
                                                             [deg]F)        H2O       H2O  (in.     (ft3)   [deg]C (  [deg]C (    [deg]F)      [deg]C (
                                                                                        H2O)                 [deg]F)   [deg]F)                 [deg]F)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                       ........  ........  ...........  ..........  ............  ........  ........  ........  ...........  ...........
                                       ........  ........  ...........  ..........  ............  ........  ........  ........  ...........  ...........
                                       ........  ........  ...........  ..........  ............  ........  ........  ........  ...........  ...........
                                       ........  ........  ...........  ..........  ............  ........  ........  ........  ...........  ...........
                                       ........  ........  ...........  ..........  ............  ........  ........  ........  ...........  ...........
    Total............................  ........  ........  ...........  ..........  ............  ........      Avg.      Avg.  ...........  ...........
                                                                                                           --------------------
Average..............................  ........  ........  ...........  ..........  ............  ........      Avg.  ........  ...........  ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------

    8.6.3 Clean the stack access ports prior to the test run to 
eliminate the chance of sampling deposited material. To begin sampling, 
remove the nozzle cap, verify that the probe heating system are at the 
specified temperature, and verify that the pitot tube and probe are 
properly positioned. Position the nozzle at the first traverse point, 
with the tip pointing directly into the gas stream. Immediately start 
the pump and adjust the flow to isokinetic conditions. Nomographs, which 
aid in the rapid adjustment of the isokinetic sampling rate without 
excessive computations, are available. These nomographs are designed for 
use when the Type S pitot tube coefficient is 0.84  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 the stack gas 
molecular weight and the pitot tube coefficient are outside the above 
ranges, do not use the nomographs unless appropriate steps are taken to 
compensate for the deviations.
    8.6.4 When the stack is under significant negative pressure 
(equivalent to the height of the impinger stem), take care to close the 
coarse-adjust valve before inserting the probe into the stack in order 
to prevent liquid from backing up through the train. If necessary, a low 
vacuum on the train may have to be started prior to entering the stack.
    8.6.5 When the probe is in position, block off the openings around 
the probe and stack access port to prevent unrepresentative dilution of 
the gas stream.
    8.6.6 Traverse the stack cross section, as required by EPA Method 1, 
40 CFR part 60, appendix A, being careful not to bump the probe nozzle 
into the stack walls when sampling near the walls or when removing or 
inserting the probe through the access port, in order to minimize the 
chance of extracting deposited material.
    8.6.7 During the test run, make periodic adjustments to keep the 
temperature around the probe at the proper levels. Add more ice and, if 
necessary, salt, to maintain a temperature of <20 [deg]C (68 [deg]F) at 
the silica gel outlet.
    8.6.8 A single train shall be used for the entire sampling run, 
except in cases where simultaneous 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. An additional train or trains may also be used for sampling when 
the capacity of a single train is exceeded.
    8.6.9 When two or more trains are used, separate analyses of 
components from each train shall be performed. If multiple trains have 
been used because the capacity of a single train would be exceeded, 
first impingers from each train may be combined, and second impingers 
from each train may be combined.
    8.6.10 At the end of the sampling run, turn off the coarse-adjust 
valve, remove the probe and nozzle from the stack, turn off the pump, 
record the final dry gas meter reading, and conduct a post-test leak-
check. Also, check the pitot lines as described in EPA Method 2, 40 CFR 
part 60, appendix A. The lines must pass this leak-check in order to 
validate the velocity-head data.
    8.6.11 Calculate percent isokineticity (see Method 2) to determine 
whether the run was valid or another test should be made.

                  8.7 Sample Preservation and Handling

    8.7.1 Samples from most sources applicable to this method have 
acceptable holding times using normal handling practices (shipping 
samples iced, storing in refrigerator at 2 [deg]C until analysis). 
However, forming section stacks and other sources using waste water 
sprays may be subject to microbial contamination. For these sources, a 
biocide (quaternary ammonium compound solution) may be added to 
collected samples to improve sample stability and method ruggedness.
    8.7.2 Sample holding time: Samples should be analyzed within 14 days 
of collection. Samples must be refrigerated/kept cold

[[Page 291]]

for the entire period preceding analysis. After the samples have been 
brought to room temperature for analysis, any analyses needed should be 
performed on the same day. Repeated cycles of warming the samples to 
room temperature/refrigerating/rewarming, then analyzing again, etc., 
have not been investigated in depth to evaluate if analyte levels remain 
stable for all sources.
    8.7.3 Additional studies will be performed to evaluate whether 
longer sample holding times are feasible for this method.

                           8.8 Sample Recovery

    8.8.1 Preparation:
    8.8.1.1 Proper cleanup procedure begins as soon as the probe is 
removed from the stack at the end of the sampling period. Allow the 
probe to cool. When the probe can be handled safely, wipe off all 
external particulate matter near the tip of the probe nozzle and place a 
cap over the tip to prevent losing or gaining particulate matter. Do not 
cap the probe tightly while the sampling train is cooling because a 
vacuum will be created, drawing liquid from the impingers back through 
the sampling train.
    8.8.1.2 Before moving the sampling train to the cleanup site, remove 
the probe from the sampling train and cap the open outlet, being careful 
not to lose any condensate that might be present. Remove the umbilical 
cord from the last impinger and cap the impinger. If a flexible line is 
used, let any condensed water or liquid drain into the impingers. Cap 
off any open impinger inlets and outlets. Ground glass stoppers, Teflon 
TM caps, or caps of other inert materials may be used to seal 
all openings.
    8.8.1.3 Transfer the probe and impinger assembly to an area that is 
clean and protected from wind so that the chances of contaminating or 
losing the sample are minimized.
    8.8.1.4 Inspect the train before and during disassembly, and note 
any abnormal conditions.
    8.8.1.5 Save a portion of the washing solution (high purity water) 
used for cleanup as a blank.
    8.8.2 Sample Containers:
    8.8.2.1 Container 1: Probe and Impinger Catches. Using a graduated 
cylinder, measure to the nearest ml, and record the volume of the 
solution in the first three impingers. Alternatively, the solution may 
be weighed to the nearest 0.5 g. Include any condensate in the probe in 
this determination. Transfer the combined impinger solution from the 
graduated cylinder into the polyethylene bottle. Taking care that dust 
on the outside of the probe or other exterior surfaces does not get into 
the sample, clean all surfaces to which the sample is exposed (including 
the probe nozzle, probe fitting, probe liner, first three impingers, and 
impinger connectors) with water. Use less than 400 ml for the entire 
waste (250 ml would be better, if possible). Add the rinse water to the 
sample container.
    8.8.2.1.1 Carefully remove the probe nozzle and rinse the inside 
surface with water from a wash bottle. Brush with a bristle brush and 
rinse until the rinse shows no visible particles, after which make a 
final rinse of the inside surface. Brush and rinse the inside parts of 
the Swagelok (or equivalent) fitting with water in a similar way.
    8.8.2.1.2 Rinse the probe liner with water. While squirting the 
water into the upper end of the probe, tilt and rotate the probe so that 
all inside surfaces will be wetted with water. Let the water drain from 
the lower end into the sample container. The tester may use a funnel 
(glass or polyethylene) to aid in transferring the liquid washes to the 
container. Follow the rinse with a bristle brush. Hold the probe in an 
inclined position, and squirt water into the upper end as the probe 
brush is being pushed with a twisting action through the probe. Hold the 
sample container underneath the lower end of the probe, and catch any 
water and particulate matter that is brushed from the probe. Run the 
brush through the probe three times or more. Rinse the brush with water 
and quantitatively collect these washings in the sample container. After 
the brushing, make a final rinse of the probe as describe above.

    Note: Two people should clean the probe in order to minimize sample 
losses. Between sampling runs, brushes must be kept clean and free from 
contamination.

    8.8.2.1.3 Rinse the inside surface of each of the first three 
impingers (and connecting tubing) three separate times. Use a small 
portion of water for each rinse, and brush each surface to which the 
sample is exposed with a bristle brush to ensure recovery of fine 
particulate matter. Make a final rinse of each surface and of the brush, 
using water.
    8.8.2.1.4 After all water washing and particulate matter have been 
collected in the sample container, tighten the lid so the sample will 
not leak out when the container 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.
    8.8.2.1.5 If the first two impingers are to be analyzed separately 
to check for breakthrough, separate the contents and rinses of the two 
impingers into individual containers. Care must be taken to avoid 
physical carryover from the first impinger to the second. Any physical 
carryover of collected moisture into the second impinger will invalidate 
a breakthrough assessment.
    8.8.2.2 Container 2: Sample Blank. Prepare a blank by using a 
polyethylene container and adding a volume of water equal to the total 
volume in Container 1. Process the blank in the same manner as Container 
1.

[[Page 292]]

    8.8.2.3 Container 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. The impinger containing the silica gel may be 
used as a sample transport container with both ends sealed with tightly 
fitting caps or plugs. Ground-glass stoppers or TeflonTM caps 
maybe used. The silica gel impinger should then be labeled, covered with 
aluminum foil, and packaged on ice for transport to the laboratory. If 
the silica gel is removed from the impinger, 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 water or other liquids to transfer the silica 
gel. If a balance is available in the field, the spent silica gel (or 
silica gel plus impinger) may be weighed to the nearest 0.5 g.
    8.8.2.4 Sample containers should be placed in a cooler, cooled by 
(although not in contact with) ice. Putting sample bottles in Zip-
LockTM bags can aid in maintaining the integrity of the 
sample labels. Sample containers should be placed vertically to avoid 
leakage during shipment. Samples should be cooled during shipment so 
they will be received cold at the laboratory. It is critical that 
samples be chilled immediately after recovery. If the source is 
susceptible to microbial contamination from wash water (e.g. forming 
section stack), add biocide as directed in section 8.2.5.
    8.8.2.5 A quaternary ammonium compound can be used as a biocide to 
stabilize samples against microbial degradation following collection. 
Using the stock quaternary ammonium compound (QAC) solution; add 2.5 ml 
QAC solution for every 100 ml of recovered sample volume (estimate of 
volume is satisfactory) immediately after collection. The total volume 
of QAC solution must be accurately known and recorded, to correct for 
any dilution caused by the QAC solution addition.
    8.8.3 Sample Preparation for Analysis 8.8.3.1 The sample should be 
refrigerated if the analysis will not be performed on the day of 
sampling. Allow the sample to warm at room temperature for about two 
hours (if it has been refrigerated) prior to analyzing.
    8.8.3.2 Analyze the sample by the pararosaniline method, as 
described in Section 11. If the color-developed sample has an absorbance 
above the highest standard, a suitable dilution in high purity water 
should be prepared and analyzed.

                           9.0 Quality Control

    9.1 Sampling: See EPA Manual 600/4-77-02b for Method 5 quality 
control.
    9.2 Analysis: The quality assurance program required for this method 
includes the analysis of the field and method blanks, and procedure 
validations. The positive identification and quantitation of 
formaldehyde are dependent on the integrity of the samples received and 
the precision and accuracy of the analytical methodology. Quality 
assurance procedures for this method are designed to monitor the 
performance of the analytical methodology and to provide the required 
information to take corrective action if problems are observed in 
laboratory operations or in field sampling activities.
    9.2.1 Field Blanks: Field blanks must be submitted with the samples 
collected at each sampling site. The field blanks include the sample 
bottles containing aliquots of sample recover water, and water reagent. 
At a minimum, one complete sampling train will be assembled in the field 
staging area, taken to the sampling area, and leak-checked at the 
beginning and end of the testing (or for the same total number of times 
as the actual sampling train). The probe of the blank train must be 
heated during the sample test. The train will be recovered as if it were 
an actual test sample. No gaseous sample will be passed through the 
blank sampling train.
    9.2.2 Blank Correction: The field blank formaldehyde concentrations 
will be subtracted from the appropriate sample formaldehyde 
concentrations. Blank formaldehyde concentrations above 0.25 [mu]g/ml 
should be considered suspect, and subtraction from the sample 
formaldehyde concentrations should be performed in a manner acceptable 
to the Administrator.
    9.2.3 Method Blanks: A method blank must be prepared for each set of 
analytical operations, to evaluate contamination and artifacts that can 
be derived from glassware, reagents, and sample handling in the 
laboratory.

                             10 Calibration

    10.1 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 
measurements at three separate places across the diameter and obtain the 
average of the measurements. The difference between the high and low 
numbers shall not exceed 0.1 mm (0.004 in). When the nozzle becomes 
nicked or corroded, it shall be repaired and calibrated, or replaced 
with a calibrated nozzle before use. Each nozzle must be permanently and 
uniquely identified.
    10.2 Pitot Tube: The Type S pitot tube assembly shall be calibrated 
according to the procedure outlined in Section 4 of EPA Method 2, or 
assigned a nominal coefficient of 0.84 if it is not visibly nicked or 
corroded and if it meets design and intercomponent spacing 
specifications.

[[Page 293]]

                          10.3 Metering System

    10.3.1 Before its initial use in the field, the metering system 
shall be calibrated according to the procedure outlined in APTD-0576. 
Instead of physically adjusting the dry-gas meter dial readings to 
correspond to the wet-test meter readings, calibration factors may be 
used to correct the gas meter dial readings mathematically to the 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 delete leakages with the pump. 
For these cases, the following leak-check procedure will apply: Make a 
ten-minute calibration run at 0.00057 m3/min (0.02 cfm). At 
the end of the run, take the difference of the measured wet-test and 
dry-gas meter volumes and divide the difference by 10 to get the leak 
rate. The leak rate should not exceed 0.00057 m3/min (0.02 
cfm).
    10.3.2 After each field use, check the calibration of the metering 
system by performing three calibration runs at a single intermediate 
orifice setting (based on the previous field test). Set the vacuum 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 
calibration has changed by more than 5 percent, recalibrate the meter 
over the full range of orifice settings, as outlined in APTD-0576.
    10.3.3 Leak-check of metering system: The portion of the sampling 
train from the pump to the orifice meter (see Figure 1) 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. 
Use the following procedure: Close the main valve on the meter box. 
Insert a one-hole rubber stopper with rubber 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 
13-18 cm (5-7 in) water column by blowing into the rubber tubing. Pinch 
off the tubing and observe the manometer for 1 min. A loss of pressure 
on the manometer indicates a leak in the meter box. Leaks must be 
corrected.

    Note: If the dry-gas meter coefficient values obtained before and 
after a test series differ by 5 percent, either the test 
series must be voided or calculations for test series must be performed 
using whichever meter coefficient value (i.e., before or after) gives 
the lower value of total sample volume.

    10.4 Probe Heater: The probe heating system must 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.
    10.5 Temperature gauges: Use the procedure in section 4.3 of USEPA 
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 mercury-in-glass thermometers.
    10.6 Barometer: Adjust the barometer initially and before each test 
series to agree to within 2.5 mm Hg (0.1 in Hg) of 
the mercury barometer. Alternately, if a National Weather Service 
Station (NWSS) is located at the same altitude above sea level as the 
test site, the barometric pressure reported by the NWSS may be used.
    10.7 Balance: Calibrate the balance before each test series, using 
Class S standard weights. The weights must be within 0.5 percent of the standards, or the balance must be 
adjusted to meet these limits.

                      11.0 Procedure for Analysis.

    The working formaldehyde standards (0.25, 0.50, 1.0, 2.0, and 3.0 
[mu]g/ml) are analyzed and a calibration curve is calculated for each 
day's analysis. The standards should be analyzed first to ensure that 
the method is working properly prior to analyzing the samples. In 
addition, a sample of the high-purity water should also be analyzed and 
used as a ``0'' formaldehyde standard.
    The procedure for analysis of samples and standards is identical: 
Using the pipet set to 2.50 ml, pipet 2.50 ml of the solution to be 
analyzed into a polystyrene cuvette. Using the 250 [mu]l pipet, pipet 
250 [mu]l of the pararosaniline reagent solution into the cuvette. Seal 
the top of the cuvette with a Parafilm square and shake at least 30 
seconds to ensure the solution in the cuvette is well-mixed. Peel back a 
corner of the Parafilm so the next reagent can be added. Using the 250 
[mu]l pipet, pipet 250 [mu]l of the sodium sulfite reagent solution into 
the cuvette. Reseal the cuvette with the Parafilm, and again shake for 
about 30 seconds to mix the solution in the cuvette. Record the time of 
addition of the sodium sulfite and let the color develop at room 
temperature for 60 minutes. Set the spectrophotometer to 570 nm and set 
to read in Absorbance Units. The spectrophotometer should be equipped 
with a holder for the 1-cm pathlength cuvettes. Place cuvette(s) 
containing high-purity water in the spectrophotometer and adjust to read 
0.000 AU.
    After the 60 minutes color development period, read the standard and 
samples in the spectrophotometer. Record the absorbance reading for each 
cuvette. The calibration curve is calculated by linear regression, with 
the formaldehyde concentration as the ``x'' coordinate of the pair, and 
the absorbance reading as the ``y'' coordinate. The procedure

[[Page 294]]

is very reproducible, and typically will yield values similar to these 
for the calibration curve:

Correlation Coefficient: 0.9999
Slope: 0.50
Y-Intercept: 0.090

The formaldehyde concentration of the samples can be found by using the 
trend-line feature of the calculator or computer program used for the 
linear regression. For example, the TI-55 calculators use the ``X'' key 
(this gives the predicted formaldehyde concentration for the value of 
the absorbance you key in for the sample). Multiply the formaldehyde 
concentration from the sample by the dilution factor, if any, for the 
sample to give the formaldehyde concentration of the original, 
undiluted, sample (units will be micrograms/ml).

               11.1 Notes on the Pararosaniline Procedure

    11.1.1 The pararosaniline method is temperature-sensitive. However, 
the small fluctuations typical of a laboratory will not significantly 
affect the results.
    11.1.2 The calibration curve is linear to beyond 4 ``[mu]g/ml'' 
formaldehyde, however, a research-grade spectrophotometer is required to 
reproducibly read the high absorbance values. Consult your instrument 
manual to evaluate the capability of the spectrophotometer.
    11.1.3 The quality of the laboratory water used to prepare standards 
and make dilutions is critical. It is important that the cautions given 
in the Reagents section be observed. This procedure allows quantitation 
of formaldehyde at very low levels, and thus it is imperative to avoid 
contamination from other sources of formaldehyde and to exercise the 
degree of care required for trace analyses.
    11.1.4 The analyst should become familiar with the operation of the 
Oxford or equivalent pipettors before using them for an analysis. Follow 
the instructions of the manufacturer; one can pipet water into a tared 
container on any analytical balance to check pipet accuracy and 
precision. This will also establish if the proper technique is being 
used. Always use a new tip for each pipetting operation.
    11.1.5 This procedure follows the recommendations of ASTM Standard 
Guide D 3614, reading all solutions versus water in the reference cell. 
This allows the absorbance of the blank to be tracked on a daily basis. 
Refer to ASTM D 3614 for more information.

                            12.0 Calculations

    Carry out calculations, retaining at least one extra decimal figure 
beyond that of the acquired data. Round off figures after final 
calculations.

                 12.1 Calculations of Total Formaldehyde

    12.1.1 To determine the total formaldehyde in mg, use the following 
equation if biocide was not used:
    Total mg formaldehyde=
    [GRAPHIC] [TIFF OMITTED] TR14JN99.043
    
Where:

Cd = measured conc. formaldehyde, [mu]g/ml
V = total volume of stack sample, ml
DF = dilution factor

    12.1.2 To determine the total formaldehyde in mg, use the following 
equation if biocide was used:
    Total mg formaldehyde=
    [GRAPHIC] [TIFF OMITTED] TR14JN99.044
    
Where:

Cd = measured conc. formaldehyde, [mu]g/ml
V = total volume of stack sample, ml
B = total volume of biocide added to sample, ml
DF = dilution factor

    12.2 Formaldehyde concentration (mg/m3) in stack gas. 
Determine the formaldehyde concentration (mg/m3) in the stack 
gas using the following equation: Formaldehyde concentration (mg/
m3) =
[GRAPHIC] [TIFF OMITTED] TR14JN99.045

Where:

K = 35.31 cu ft/m3 for Vm(std) in English units, 
or
K = 1.00 m3/m3 for Vm(std) in metric 
units
Vm(std) = volume of gas sample measured by a dry gas meter, 
corrected to standard conditions, dscm (dscf)

    12.3 Average dry gas meter temperature and average orifice pressure 
drop are obtained from the data sheet.
    12.4 Dry Gas Volume: Calculate Vm(std) and adjust for 
leakage, if necessary, using the equation in Section 6.3 of EPA Method 
5, 40 CFR part 60, appendix A.
    12.5 Volume of Water Vapor and Moisture Content: Calculated the 
volume of water vapor and moisture content from equations 5-2 and 5-3 of 
EPA Method 5.

                         13.0 Method Performance

    The precision of this method is estimated to be better than 5 percent, expressed as  the 
percent relative standard deviation.

[[Page 295]]

                  14.0 Pollution Prevention. (Reserved)

                    15.0 Waste Management. (Reserved)

                             16.0 References

R.R. Miksch, et al., Analytical Chemistry, November 1981, 53 pp. 2118-
2123.
J.F. Walker, Formaldehyde, Third Edition, 1964.
US EPA 40 CFR, part 60, Appendix A, Test Methods 1-5

Method 318--Extractive FTIR Method for the Measurement of Emissions From 
             the Mineral Wool and Wool Fiberglass Industries

                        1.0 Scope and Application

    This method has been validated and approved for mineral wool and 
wool fiberglass sources. This method may not be applied to other source 
categories without validation and approval by the Administrator 
according to the procedures in Test Method 301, 40 CFR part 63, appendix 
A. For sources seeking to apply FTIR to other source categories, Test 
Method 320 (40 CFR part 63, appendix A) may be utilized.
    1.1 Scope. The analytes measured by this method and their CAS 
numbers are:

Carbon Monoxide 630-08-0
Carbonyl Sulfide 463-58-1
Formaldehyde 50-00-0
Methanol 1455-13-6
Phenol 108-95-2

                            1.2 Applicability

    1.2.1 This method is applicable for the determination of 
formaldehyde, phenol, methanol, carbonyl sulfide (COS) and carbon 
monoxide (CO) concentrations in controlled and uncontrolled emissions 
from manufacturing processes using phenolic resins. The compounds are 
analyzed in the mid-infrared spectral region (about 400 to 4000 cm-1 or 
25 to 2.5 [mu]m). Suggested analytical regions are given below (Table 
1). Slight deviations from these recommended regions may be necessary 
due to variations in moisture content and ammonia concentration from 
source to source.

                                       Table 1--Example Analytical Regions
----------------------------------------------------------------------------------------------------------------
             Compound                Analytical region (cm-1)  FLm - FUm           Potential interferants
----------------------------------------------------------------------------------------------------------------
Formaldehyde.....................  2840.93-2679.83.......................  Water, Methane.
Phenol...........................  1231.32-1131.47.......................  Water, Ammonia, Methane.
Methanol.........................  1041.56-1019.95.......................  Water, Ammonia.
COSa.............................  2028.4-2091.9.........................  Water, CO2, CO.
COa..............................  2092.1-2191.8.........................  Water, CO2, COS.
----------------------------------------------------------------------------------------------------------------
a Suggested analytical regions assume about 15 percent moisture and CO2, and that COS and CO have about the same
  absorbance (in the range of 10 to 50 ppm). If CO and COS are hundreds of ppm or higher, then CO2 and moisture
  interference is reduced. If CO or COS is present at high concentration and the other at low concentration,
  then a shorter cell pathlength may be necessary to measure the high concentration component.

1.2.2 This method does not apply when: (a) Polymerization of 
formaldehyde occurs, (b) moisture condenses in either the sampling 
system or the instrumentation, and (c) when moisture content of the gas 
stream is so high relative to the analyte concentrations that it causes 
severe spectral interference.

                    1.3 Method Range and Sensitivity

    1.3.1 The analytical range is a function of instrumental design and 
composition of the gas stream. Theoretical detection limits depend, in 
part, on (a) the absorption coefficient of the compound in the 
analytical frequency region, (b) the spectral resolution, (c) 
interferometer sampling time, (d) detector sensitivity and response, and 
(e) absorption pathlength.
    1.3.2 Practically, there is no upper limit to the range. The 
practical lower detection limit is usually higher than the theoretical 
value, and depends on (a) moisture content of the flue gas, (b) presence 
of interferants, and (c) losses in the sampling system. In general, a 22 
meter pathlength cell in a suitable sampling system can achieve 
practical detection limits of 1.5 ppm for three compounds (formaldehyde, 
phenol, and methanol) at moisture levels up to 15 percent by volume. 
Sources with uncontrolled emissions of CO and COS may require a 4 meter 
pathlength cell due to high concentration levels. For these two 
compounds, make sure absorbance of highest concentration component is 
<1.0.

                       1.4 Data Quality Objectives

1.4.1 In designing or configuring the system, the analyst first sets the 
data quality objectives, i.e., the desired lower detection limit 
(DLi) and the desired analytical uncertainty (AUi) 
for each compound. The instrumental parameters (factors b, c, d, and e 
in Section 1.3.1) are then chosen to meet these requirements, using 
Appendix D of the FTIR Protocol.
1.4.2 Data quality for each application is determined, in part, by 
measuring the RMS (Root Mean Square) noise level in each analytical 
spectral region (Appendix C of the FTIR Protocol). The RMS noise is 
defined as

[[Page 296]]

the RMSD (Root Mean Square Deviation) of the absorbance values in an 
analytical region from the mean absorbance value of the region. Appendix 
D of the FTIR Protocol defines the MAUim (minimum analyte 
uncertainty of the ith analyte in the mth 
analytical region). The MAU is the minimum analyte concentration for 
which the analytical uncertainty limit (AUi) can be 
maintained: if the measured analyte concentration is less than 
MAUi, then data quality is unacceptable. Table 2 gives some 
example DL and AU values along with calculated areas and MAU values 
using the protocol procedures.

                                 Table 2--Example Pre-Test Protocol Calculations
----------------------------------------------------------------------------------------------------------------
                                                                                                    Protocol
          Protocol value                  Form               Phenol             Methanol            appendix
----------------------------------------------------------------------------------------------------------------
Reference concentration a (ppm-    3.016               3.017               5.064               .................
 meters)/K.
Reference Band Area..............  8.2544              16.6417             4.9416              B
DL (ppm-meters)/K................  0.1117              0.1117              0.1117              B
AU...............................  0.2                 0.2                 0.2                 B
CL...............................  0.02234             0.02234             0.02234             B
FL...............................  2679.83             1131.47             1019.95             B
FU...............................  2840.93             1231.32             1041.56             B
FC...............................  2760.38             1181.395            1030.755            B
AAI (ppm-meters)/K...............  0.18440             0.01201             0.00132             B
RMSD.............................  2.28E-03            1.21E-03            1.07E-03            C
MAU (ppm-meters)/K...............  4.45E-02            7.26E-03            4.68E-03            D
MAU (ppm at 22)..................  0.0797              0.0130              0.0084              D
----------------------------------------------------------------------------------------------------------------
a Concentration units are: ppm concentration of the reference sample (ASC), times the path length of the FTIR
  cell used when the reference spectrum was measured (meters), divided by the absolute temperature of the
  reference sample in Kelvin (K), or (ppm-meters)/K.

                          2.0 Summary of Method

                              2.1 Principle

    2.1.1 Molecules are composed of chemically bonded atoms, which are 
in constant motion. The atomic motions result in bond deformations (bond 
stretching and bond-angle bending). The number of fundamental (or 
independent) vibrational motions depends on the number of atoms (N) in 
the molecule. At typical testing temperatures, most molecules are in the 
ground-state vibrational state for most of their fundamental vibrational 
motions. A molecule can undergo a transition from its ground state (for 
a particular vibration) to the first excited state by absorbing a 
quantum of light at a frequency characteristic of the molecule and the 
molecular motion. Molecules also undergo rotational transitions by 
absorbing energies in the far-infrared or microwave spectral regions. 
Rotational transition absorbencies are superimposed on the vibrational 
absorbencies to give a characteristic shape to each rotational-
vibrational absorbance ``band.''
    2.1.2 Most molecules exhibit more than one absorbance band in 
several frequency regions to produce an infrared spectrum (a 
characteristic pattern of bands or a ``fingerprint'') that is unique to 
each molecule. The infrared spectrum of a molecule depends on its 
structure (bond lengths, bond angles, bond strengths, and atomic 
masses). Even small differences in structure can produce significantly 
different spectra.
    2.1.3 Spectral band intensities vary with the concentration of the 
absorbing compound. Within constraints, the relationship between 
absorbance and sample concentration is linear. Sample spectra are 
compared to reference spectra to determine the species and their 
concentrations.

                        2.2 Sampling and Analysis

    2.2.1 Flue gas is continuously extracted from the source, and the 
gas or a portion of the gas is conveyed to the FTIR gas cell, where a 
spectrum of the flue gas is recorded. Absorbance band intensities are 
related to sample concentrations by Beer's Law.
[GRAPHIC] [TIFF OMITTED] TR14JN99.046

Where:

An = absorbance of the ith component at the given frequency, 
[nu].
a = absorption coefficient of the ith component at the 
frequency, [nu].
b = path length of the cell.
c = concentration of the ith compound in the sample at 
frequency [nu].

    2.2.2 After identifying a compound from the infrared spectrum, its 
concentration is determined by comparing band intensities in the sample 
spectrum to band intensities in ``reference spectra'' of the 
formaldehyde, phenol, methanol, COS and CO. These reference spectra are 
available in a permanent soft copy from the EPA spectral library on the 
EMTIC bulletin board. The source may also prepare reference spectra 
according to Section 4.5 of the FTIR Protocol.

    Note: Reference spectra not prepared according to the FTIR Protocol 
are not acceptable for use in this test method. Documentation detailing 
the FTIR Protocol steps used

[[Page 297]]

in preparing any non-EPA reference spectra shall be included in each 
test report submitted by the source.

    2.3 Operator Requirements. The analyst must have some knowledge of 
source sampling and of infrared spectral patterns to operate the 
sampling system and to choose a suitable instrument configuration. The 
analyst should also understand FTIR instrument operation well enough to 
choose an instrument configuration consistent with the data quality 
objectives.

                             3.0 Definitions

    See Appendix A of the FTIR Protocol.

                            4.0 Interferences

    4.1 Analytical (or Spectral) Interferences. Water vapor. High 
concentrations of ammonia (hundreds of ppm) may interfere with the 
analysis of low concentrations of methanol (1 to 5 ppm). For CO, carbon 
dioxide and water may be interferants. In cases where COS levels are low 
relative to CO levels, CO and water may be interferants.
    4.2 Sampling System Interferences. Water, if it condenses, and 
ammonia, which reacts with formaldehyde.

                               5.0 Safety

    5.1 Formaldehyde is a suspected carcinogen; therefore, exposure to 
this compound must be limited. Proper monitoring and safety precautions 
must be practiced in any atmosphere with potentially high concentrations 
of CO.
    5.2 This method may involve sampling at locations having high 
positive or negative pressures, high temperatures, elevated heights, 
high concentrations of hazardous or toxic pollutants, or other diverse 
sampling conditions. It is the responsibility of the tester(s) to ensure 
proper safety and health practices, and to determine the applicability 
of regulatory limitations before performing this test method.

                       6.0 Equipment and Supplies

    The equipment and supplies are based on the schematic of a sampling 
train shown in Figure 1. Either the evacuated or purged sampling 
technique may be used with this sampling train. Alternatives may be 
used, provided that the data quality objectives of this method are met.
    6.1 Sampling Probe. Glass, stainless steel, or other appropriate 
material of sufficient length and physical integrity to sustain heating, 
prevent adsorption of analytes, and to reach gas sampling point.
    6.2 Particulate Filters. A glass wool plug (optional) inserted at 
the probe tip (for large particulate removal) and a filter rated at 1-
micron (e.g., BalstonTM) for fine particulate removal, placed 
immediately after the heated probe.
    6.3 Sampling Line/Heating System. Heated (maintained at 250  25 degrees F) stainless steel, TeflonTM, or 
other inert material that does not adsorb the analytes, to transport the 
sample to analytical system.
    6.4 Stainless Steel Tubing. Type 316, e.g., \3/8\ in. diameter, and 
appropriate length for heated connections.
    6.5 Gas Regulators. Appropriate for individual gas cylinders.

[[Page 298]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.052

    6.6 TeflonTM Tubing. Diameter (e.g., \3/8\ in.) and 
length suitable to connect cylinder regulators.
    6.7 Sample Pump. A leak-free pump (e.g., KNF TM), with 
by-pass valve, capable of pulling sample through entire sampling system 
at a rate of about 10 to 20 L/min. If placed before the analytical 
system, heat the pump and use a pump fabricated from materials non-
reactive to the target pollutants. If the pump is located after the 
instrument, systematically record the sample pressure in the gas cell.
    6.8 Gas Sample Manifold. A heated manifold that diverts part of the 
sample stream to the analyzer, and the rest to the by-pass discharge 
vent or other analytical instrumentation.
    6.9 Rotameter. A calibrated 0 to 20 L/min range rotameter.
    6.10 FTIR Analytical System. Spectrometer and detector, capable of 
measuring formaldehyde, phenol, methanol, COS and CO to the 
predetermined minimum detectable level. The system shall include a 
personal computer with compatible software that provides real-time 
updates of the spectral profile during sample collection and spectral 
collection.
    6.11 FTIR Cell Pump. Required for the evacuated sampling technique, 
capable of evacuating the FTIR cell volume within 2 minutes. The FTIR 
cell pump should allow the operator to obtain at least 8 sample spectra 
in 1 hour.
    6.12 Absolute Pressure Gauge. Heatable and capable of measuring 
pressure from 0 to 1000 mmHg to within 2.5 mmHg 
(e.g., BaratronTM).
    6.13 Temperature Gauge. Capable of measuring the cell temperature to 
within 2 [deg]C.

[[Page 299]]

                       7.0 Reagents and Standards

    7.1 Ethylene (Calibration Transfer Standard). Obtain NIST traceable 
(or Protocol) cylinder gas.
    7.2 Nitrogen. Ultra high purity (UHP) grade.
    7.3 Reference Spectra. Obtain reference spectra for the target 
pollutants at concentrations that bracket (in ppm-meter/K) the emission 
source levels. Also, obtain reference spectra for SF6 and 
ethylene. Suitable concentrations are 0.0112 to 0.112 (ppm-meter)/K for 
SF6 and 5.61 (ppm-meter)/K or less for ethylene. The 
reference spectra shall meet the criteria for acceptance outlined in 
Section 2.2.2. The optical density (ppm-meters/K) of the reference 
spectrum must match the optical density of the sample spectrum within 
(less than) 25 percent.

            8.0 Sample Collection, Preservation, and Storage

    Sampling should be performed in the following sequence: Collect 
background, collect CTS spectrum, collect samples, collect post-test CTS 
spectrum, verify that two copies of all data were stored on separate 
computer media.
    8.1 Pretest Preparations and Evaluations. Using the procedure in 
Section 4.0 of the FTIR Protocol, determine the optimum sampling system 
configuration for sampling the target pollutants. Table 2 gives some 
example values for AU, DL, and MAU. Based on a study (Reference 1), an 
FTIR system using 1 cm-1 resolution, 22 meter path length, 
and a broad band MCT detector was suitable for meeting the requirements 
in Table 2. Other factors that must be determined are:
    a. Test requirements: AUi, CMAXi, 
DLi, OFUi, and tAN for each.
    b. Interferants: See Table 1.
    c. Sampling system: LS', Pmin, PS', 
TS', tSS, VSS; fractional error, MIL.
    d. Analytical regions: 1 through Nm, FLm, 
FCm, and FUm, plus interferants, FFUm, 
FFLm, wavenumber range FNU to FNL. See Tables 1 and 2.
    8.1.1 If necessary, sample and acquire an initial spectrum. Then 
determine the proper operational pathlength of the instrument to obtain 
non-saturated absorbances of the target analytes.
    8.1.2 Set up the sampling train as shown in Figure 1.
    8.2 Sampling System Leak-check. Leak-check from the probe tip to 
pump outlet as follows: Connect a 0- to 250-mL/min rate meter (rotameter 
or bubble meter) to the outlet of the pump. Close off the inlet to the 
probe, and note the leakage rate. The leakage rate shall be <=200 mL/
min.
    8.3 Analytical System Leak-check.
    8.3.1 For the evacuated sample technique, close the valve to the 
FTIR cell, and evacuate the absorption cell to the minimum absolute 
pressure Pmin. Close the valve to the pump, and determine the 
change in pressure [Delta]Pv after 2 minutes.
    8.3.2 For both the evacuated sample and purging techniques, 
pressurize the system to about 100 mmHg above atmospheric pressure. 
Isolate the pump and determine the change in pressure 
[Delta]Pp after 2 minutes.
    8.3.3 Measure the barometric pressure, Pb in mmHg.
    8.3.4 Determine the percent leak volume %VL for the 
signal integration time tSS and for [Delta]Pmax, 
i.e., the larger of [Delta]Pv or [Delta]Pp, as 
follows:
[GRAPHIC] [TIFF OMITTED] TR14JN99.047

Where:

50 = 100% divided by the leak-check time of 2 minutes.

    8.3.5 Leak volumes in excess of 4 percent of the sample system 
volume VSS are unacceptable.
    8.4 Background Spectrum. Evacuate the gas cell to <=5 mmHg, and fill 
with dry nitrogen gas to ambient pressure. Verify that no significant 
amounts of absorbing species (for example water vapor and 
CO2) are present. Collect a background spectrum, using a 
signal averaging period equal to or greater than the averaging period 
for the sample spectra. Assign a unique file name to the background 
spectrum. Store the spectra of the background interferogram and 
processed single-beam background spectrum on two separate computer media 
(one is used as the back-up). If continuous sampling will be used during 
sample collection, collect the background spectrum with nitrogen gas 
flowing through the cell at the same pressure and temperature as will be 
used during sampling.
    8.5 Pre-Test Calibration Transfer Standard. Evacuate the gas cell to 
<=5 mmHg absolute pressure, and fill the FTIR cell to atmospheric 
pressure with the CTS gas. Or, purge the cell with 10 cell volumes of 
CTS gas. Record the spectrum. If continuous sampling will be used during 
sample collection, collect the CTS spectrum with CTS gas flowing through 
the cell at the same pressure and temperature as will be used during 
sampling.

                               8.6 Samples

    8.6.1 Evacuated Samples. Evacuate the absorbance cell to <=5 mmHg 
absolute pressure. Fill the cell with flue gas to ambient pressure and 
record the spectrum. Before taking the next sample, evacuate the cell 
until no further evidence of absorption exists. Repeat this procedure to 
collect at least 8 separate spectra (samples) in 1 hour.
    8.6.2 Purge Sampling. Purge the FTIR cell with 10 cell volumes of 
flue gas and at least for about 10 minutes. Discontinue the gas

[[Page 300]]

cell purge, isolate the cell, and record the sample spectrum and the 
pressure. Before taking the next sample, purge the cell with 10 cell 
volumes of flue gas.
    8.6.3 Continuous Sampling. Spectra can be collected continuously 
while the FTIR cell is being purged. The sample integration time, 
tss, the sample flow rate through the FTIR gas cell, and the 
total run time must be chosen so that the collected data consist of at 
least 10 spectra with each spectrum being of a separate cell volume of 
flue gas. More spectra can be collected over the run time and the total 
run time (and number of spectra) can be extended as well.

               8.7 Sampling QA, Data Storage and Reporting

    8.7.1 Sample integration times should be sufficient to achieve the 
required signal-to-noise ratios. Obtain an absorbance spectrum by 
filling the cell with nitrogen. Measure the RMSD in each analytical 
region in this absorbance spectrum. Verify that the number of scans is 
sufficient to achieve the target MAU (Table 2).
    8.7.2 Identify all sample spectra with unique file names.
    8.7.3 Store on two separate computer media a copy of sample 
interferograms and processed spectra. The data shall be available to the 
Administrator on request for the length of time specified in the 
applicable regulation.
    8.7.4 For each sample spectrum, document the sampling conditions, 
the sampling time (while the cell was being filled), the time the 
spectrum was recorded, the instrumental conditions (path length, 
temperature, pressure, resolution, integration time), and the spectral 
file name. Keep a hard copy of these data sheets.
    8.8 Signal Transmittance. While sampling, monitor the signal 
transmittance through the instrumental system. If signal transmittance 
(relative to the background) drops below 95 percent in any spectral 
region where the sample does not absorb infrared energy, obtain a new 
background spectrum.
    8.9 Post-run CTS. After each sampling run, record another CTS 
spectrum.

                            8.10 Post-test QA

    8.10.1 Inspect the sample spectra immediately after the run to 
verify that the gas matrix composition was close to the expected 
(assumed) gas matrix.
    8.10.2 Verify that the sampling and instrumental parameters were 
appropriate for the conditions encountered. For example, if the moisture 
is much greater than anticipated, it will be necessary to use a shorter 
path length or dilute the sample.
    8.10.3 Compare the pre and post-run CTS spectra. They shall agree to 
within -5 percent. See FTIR Protocol, Appendix E.

                           9.0 Quality Control

    Follow the quality assurance procedures in the method, including the 
analysis of pre and post-run calibration transfer standards (Sections 
8.5 and 8.9) and the post-test quality assurance procedures in Section 
8.10.

                  10.0 Calibration and Standardization

    10.1 Signal-to-Noise Ratio (S/N). The S/N shall be sufficient to 
meet the MAU in each analytical region.
    10.2 Absorbance Pathlength. Verify the absorbance path length by 
comparing CTS spectra to reference spectra of the calibration gas(es). 
See FTIR Protocol, Appendix E.
    10.3 Instrument Resolution. Measure the line width of appropriate 
CTS band(s) and compare to reference CTS spectra to verify instrumental 
resolution.
    10.4 Apodization Function. Choose appropriate apodization function. 
Determine any appropriate mathematical transformations that are required 
to correct instrumental errors by measuring the CTS. Any mathematical 
transformations must be documented and reproducible.
    10.5 FTIR Cell Volume. Evacuate the cell to <=5 mmHg. Measure the 
initial absolute temperature (Ti) and absolute pressure 
(Pi). Connect a wet test meter (or a calibrated dry gas 
meter), and slowly draw room air into the cell. Measure the meter volume 
(Vm), meter absolute temperature (Tm), and meter 
absolute pressure (Pm), and the cell final absolute 
temperature (Tf) and absolute pressure (Pf). 
Calculate the FTIR cell volume Vss, including that of the 
connecting tubing, as follows:
[GRAPHIC] [TIFF OMITTED] TR14JN99.048

As an alternative to the wet test meter/calibrated dry gas meter 
procedure, measure the inside dimensions of the cell cylinder and 
calculate its volume.

                             11.0 Procedure

    Refer to Sections 4.6-4.11, Sections 5, 6, and 7, and the appendices 
of the FTIR Protocol.

                   12.0 Data Analysis and Calculations

    a. Data analysis is performed using appropriate reference spectra 
whose concentrations can be verified using CTS spectra. Various 
analytical programs are available to relate sample absorbance to a 
concentration standard. Calculated concentrations should be verified by 
analyzing spectral baselines after mathematically subtracting scaled 
reference spectra from the sample spectra. A

[[Page 301]]

full description of the data analysis and calculations may be found in 
the FTIR Protocol (Sections 4.0, 5.0, 6.0 and appendices).
    b. Correct the calculated concentrations in sample spectra for 
differences in absorption pathlength between the reference and sample 
spectra by:
[GRAPHIC] [TIFF OMITTED] TR14JN99.049

Where:

Ccorr = The pathlength corrected concentration.
Ccalc = The initial calculated concentration (output of the 
Multicomp program designed for the compound).
Lr = The pathlength associated with the reference spectra.
Ls = The pathlength associated with the sample spectra.
Ts = The absolute temperature (K) of the sample gas.
Tr = The absolute gas temperature (K) at which reference 
spectra were recorded.

                    13.0 Reporting and Recordkeeping

    All interferograms used in determining source concentration shall be 
stored for the period of time required in the applicable regulation. The 
Administrator has the option of requesting the interferograms recorded 
during the test in electronic form as part of the test report.

                         14.0 Method Performance

    Refer to the FTIR Protocol.

                  15.0 Pollution Prevention. [Reserved]

                          16.0 Waste Management

    Laboratory standards prepared from the formaldehyde and phenol are 
handled according to the instructions in the materials safety data 
sheets (MSDS).

                             17.0 References

    (1) ``Field Validation Test Using Fourier Transform Infrared (FTIR) 
Spectrometry To Measure Formaldehyde, Phenol and Methanol at a Wool 
Fiberglass Production Facility.'' Draft. U.S. Environmental Protection 
Agency Report, Entropy, Inc., EPA Contract No. 68D20163, Work Assignment 
I-32, December 1994 (docket item II-A-13).
    (2) ``Method 301--Field Validation of Pollutant Measurement Methods 
from Various Waste Media,'' 40 CFR part 63, appendix A.

 Method 319--Determination of Filtration Efficiency for Paint Overspray 
                                Arrestors

                       1.0 Scope and Application.

    1.1 This method applies to the determination of the initial, 
particle size dependent, filtration efficiency for paint arrestors over 
the particle diameter range from 0.3 to 10 [mu]m. The method applies to 
single and multiple stage paint arrestors or paint arrestor media. The 
method is applicable to efficiency determinations from 0 to 99 percent. 
Two test aerosols are used--one liquid phase and one solid phase. Oleic 
acid, a low-volatility liquid (CAS Number 112-80-1), is used to simulate 
the behavior of wet paint overspray. The solid-phase aerosol is 
potassium chloride salt (KCl, CAS Number 7447-40-7) and is used to 
simulate the behavior of a dry overspray. The method is limited to 
determination of the initial, clean filtration efficiency of the 
arrestor. Changes in efficiency (either increase or decrease) due to the 
accumulation of paint overspray on and within the arrestor are not 
evaluated.
    1.2 Efficiency is defined as 1--Penetration (e.g., 70 percent 
efficiency is equal to 0.30 penetration). Penetration is based on the 
ratio of the downstream particle concentration to the upstream 
concentration. It is often more useful, from a mathematical or 
statistical point of view, to discuss the upstream and downstream counts 
in terms of penetration rather than the derived efficiency value. Thus, 
this document uses both penetration and efficiency as appropriate.
    1.3 For a paint arrestor system or subsystem which has been tested 
by this method, adding additional filtration devices to the system or 
subsystem shall be assumed to result in an efficiency of at least that 
of the original system without the requirement for additional testing. 
(For example, if the final stage of a three-stage paint arrestor system 
has been tested by itself, then the addition of the other two stages 
shall be assumed to maintain, as a minimum, the filtration efficiency 
provided by the final stage alone. Thus, in this example, if the final 
stage has been shown to meet the filtration requirements of Table 1 of 
Sec. 63.745 of subpart GG, then the final stage in combination with any 
additional paint arrestor stages also passes the filtration 
requirements.)

                         2.0 Summary of Method.

    2.1 This method applies to the determination of the fractional 
(i.e., particle-size dependent) aerosol penetration of several types of 
paint arrestors. Fractional penetration is computed from aerosol 
concentrations measured upstream and downstream of an arrestor installed 
in a laboratory test rig. The aerosol concentrations upstream and 
downstream of the arrestors are measured with an

[[Page 302]]

aerosol analyzer that simultaneously counts and sizes the particles in 
the aerosol stream. The aerosol analyzer covers the particle diameter 
size range from 0.3 to 10 [mu]m in a minimum of 12 contiguous sizing 
channels. Each sizing channel covers a narrow range of particle 
diameters. For example, Channel 1 may cover from 0.3 to 0.4 [mu]m, 
Channel 2 from 0.4 to 0.5 [mu]m, * * * By taking the ratio of the 
downstream to upstream counts on a channel by channel basis, the 
penetration is computed for each of the sizing channels.
    2.2 The upstream and downstream aerosol measurements are made while 
injecting the test aerosol into the air stream upstream of the arrestor 
(ambient aerosol is removed with HEPA filters on the inlet of the test 
rig). This test aerosol spans the particle size range from 0.3 to 10 
[mu]m and provides sufficient upstream concentration in each of the 
optical particle counter (OPC) sizing channels to allow accurate 
calculation of penetration, down to penetrations of approximately 0.01 
(i.e., 1 percent penetration; 99 percent efficiency). Results are 
presented as a graph and a data table showing the aerodynamic particle 
diameter and the corresponding fractional efficiency.

                            3.0 Definitions.

    Aerodynamic Diameter--diameter of a unit density sphere having the 
same aerodynamic properties as the particle in question.
    Efficiency is defined as equal to 1--Penetration.
    Optical Particle Counter (OPC)--an instrument that counts particles 
by size using light scattering. An OPC gives particle diameters based on 
size, index of refraction, and shape.
    Penetration--the fraction of the aerosol that penetrates the filter 
at a given particle diameter. Penetration equals the downstream 
concentration divided by the upstream concentration.

                           4.0 Interferences.

    4.1 The influence of the known interferences (particle losses) are 
negated by correction of the data using blanks.

                               5.0 Safety.

    5.1 There are no specific safety precautions for this method above 
those of good laboratory practice. This standard does not purport to 
address all of the safety problems, if any, associated with its use. It 
is the responsibility of the user of this method to establish 
appropriate safety and health practices and determine the applicability 
of regulatory limitations prior to use.

                       6.0 Equipment and Supplies.

    6.1 Test Facility. A schematic diagram of a test duct used in the 
development of the method is shown in Figure 319-1.

[[Page 303]]

[GRAPHIC] [TIFF OMITTED] TR27MR98.008

    6.1.1 The test section, paint spray section, and attached 
transitions are constructed of stainless and galvanized steel. The 
upstream and downstream ducting is 20 cm diameter polyvinyl chloride 
(PVC). The upstream transition provides a 7 [deg] angle of expansion to 
provide a uniform air flow distribution to the paint arrestors. Aerosol 
concentration is

[[Page 304]]

measured upstream and downstream of the test section to obtain the 
challenge and penetrating aerosol concentrations, respectively. Because 
the downstream ducting runs back under the test section, the challenge 
and penetrating aerosol taps are located physically near each other, 
thereby facilitating aerosol sampling and reducing sample-line length. 
The inlet nozzles of the upstream and downstream aerosol probes are 
designed to yield isokinetic sampling conditions.
    6.1.2 The configuration and dimensions of the test duct can deviate 
from those of Figure 319-1 provided that the following key elements are 
maintained: the test duct must meet the criteria specified in Table 319-
1; the inlet air is HEPA filtered; the blower is on the upstream side of 
the duct thereby creating a positive pressure in the duct relative to 
the surrounding room; the challenge air has a temperature between 50 
[deg] and 100 [deg]F and a relative humidity of less than 65 percent; 
the angle of the upstream transition (if used) to the paint arrestor 
must not exceed 7 [deg]; the angle of the downstream transition (if 
used) from the paint arrestor must not exceed 30 [deg]; the test duct 
must provide a means for mixing the challenge aerosol with the upstream 
flow (in lieu of any mixing device, a duct length of 15 duct diameters 
fulfills this requirement); the test duct must provide a means for 
mixing any penetrating aerosol with the downstream flow (in lieu of any 
mixing device, a duct length of 15 duct diameters fulfills this 
requirement); the test section must provide a secure and leak-free 
mounting for single and multiple stage arrestors; and the test duct may 
utilize a 180 [deg] bend in the downstream duct.

                     Table 319-1--QC Control Limits
------------------------------------------------------------------------
                                  Frequency and
                                   description         Control limits
------------------------------------------------------------------------
OPC zero count..............  Each Test. OPC        <50 counts per
                               samples HEPA-         minute.
                               filtered air.
OPC sizing accuracy check...  Daily. Sample         Peak of distribution
                               aerosolized PSL       should be in
                               spheres.              correct OPC
                                                     channel.
Minimum counts per channel    Each Test...........  Minimum total of 500
 for challenge aerosol.                              particle counts per
                                                     channel.
Maximum particle              Each Test. Needed to  <10% of
 concentration.                ensure OPC is not     manufacturer's
                               overloaded.           claimed upper limit
                                                     corresponding to a
                                                     10% count error.
Standard Deviation of         Computed for each     <0.10 for 0.3 to 3
 Penetration.                  test based on the     [mu]m diameter.
                               CV of the upstream   <0.30 for 3 [mu]m
                               counts.               diameter.
0% Penetration..............  Monthly.............  <0.01.
100% Penetration--KCl.......  Triplicate tests      0.3 to 1 [mu]m: 0.90
                               performed             to 1.10.
                               immediately before,  1 to 3 [mu]m: 0.75
                               during, or after      to 1.25.
                               triplicate arrestor  3 to 10 [mu]m: 0.50
                               tests.                to 1.50.
100% Penetration--Oleic Acid  Triplicate tests      0.3 to 1 [mu]m: 0.90
                               performed             to 1.10.
                               immediately before,  1 to 3 [mu]m: 0.75
                               during, or after      to 1.25.
                               triplicate arrestor  3 to 10 [mu]m: 0.50
                               tests.                to 1.50.
------------------------------------------------------------------------

    6.2 Aerosol Generator. The aerosol generator is used to produce a 
stable aerosol covering the particle size range from 0.3 to 10 [mu]m 
diameter. The generator used in the development of this method consists 
of an air atomizing nozzle positioned at the top of a 0.30-m (12-in.) 
diameter, 1.3-m (51-in.) tall, acrylic, transparent, spray tower. This 
tower allows larger sized particles, which would otherwise foul the test 
duct and sample lines, to fall out of the aerosol. It also adds drying 
air to ensure that the KCl droplets dry to solid salt particles. After 
generation, the aerosol passes through an aerosol neutralizer (Kr85 
radioactive source) to neutralize any electrostatic charge on the 
aerosol (electrostatic charge is an unavoidable consequence of most 
aerosol generation methods). To improve the mixing of the aerosol with 
the air stream, the aerosol is injected counter to the airflow. 
Generators of other designs may be used, but they must produce a stable 
aerosol concentration over the 0.3 to 10 [mu]m diameter size range; 
provide a means of ensuring the complete drying of the KCl aerosol; and 
utilize a charge neutralizer to neutralize any electrostatic charge on 
the aerosol. The resultant challenge aerosol must meet the minimum count 
per channel and maximum concentration criteria of Table 319-1.
    6.3 Installation of Paint Arrestor. The paint arrestor is to be 
installed in the test duct in a manner that precludes air bypassing the 
arrestor. Since arrestor media are often sold unmounted, a mounting 
frame may be used to provide back support for the media in addition to 
sealing it into the duct. The mounting frame for 20 in.x20 in. arrestors 
will have minimum open internal dimensions of 18 in. square. Mounting 
frames for 24 in.x24 in. arrestors will have minimum open internal 
dimensions of 22 in. square. The open internal dimensions of the 
mounting frame shall not be less than 75 percent of the approach duct 
dimensions.

[[Page 305]]

    6.4 Optical Particle Counter. The upstream and downstream aerosol 
concentrations are measured with a high-resolution optical particle 
counter (OPC). To ensure comparability of test results, the OPC shall 
utilize an optical design based on wide-angle light scattering and 
provided a minimum of 12 contiguous particle sizing channels from 0.3 to 
10[mu]m diameter (based on response to PSL) where, for each channel, the 
ratio of the diameter corresponding to the upper channel bound to the 
lower channel bound must not exceed 1.5.
    6.5 Aerosol Sampling System. The upstream and downstream sample 
lines must be made of rigid electrically-grounded metallic tubing having 
a smooth inside surface, and they must be rigidly secured to prevent 
movement during testing. The upstream and downstream sample lines are to 
be nominally identical in geometry. The use of a short length (100 mm 
maximum) of straight flexible tubing to make the final connection to the 
OPC is acceptable. The inlet nozzles of the upstream and downstream 
probes must be sharp-edged and of appropriate entrance diameter to 
maintain isokinetic sampling within 20 percent of the air velocity.
    6.5.1 The sampling system may be designed to acquire the upstream 
and downstream samples using (a) sequential upstream-downstream sampling 
with a single OPC, (b) simultaneous upstream and downstream sampling 
with two OPC's, or (c) sequential upstream-downstream sampling with two 
OPC's.
    6.5.2 When two particle counters are used to acquire the upstream 
and downstream counts, they must be closely matched in flowrate and 
optical design.
    6.6 Airflow Monitor. The volumetric airflow through the system shall 
be measured with a calibrated orifice plate, flow nozzle, or laminar 
flow element. The measurement device must have an accuracy of 5 percent 
or better.
    7.0 Reagents and Standards.
    7.1 The liquid test aerosol is reagent grade, 98 percent pure, oleic 
acid (Table 319-2). The solid test aerosol is KCl aerosolized from a 
solution of KCl in water. In addition to the test aerosol, a calibration 
aerosol of monodisperse polystyrene latex (PSL) spheres is used to 
verify the calibration of the OPC.

                          Table 319-2--Properties of the Test and Calibration Aerosols
----------------------------------------------------------------------------------------------------------------
                                                                  Density,  g/
                                        Refractive index             cm \3\                  Shape
----------------------------------------------------------------------------------------------------------------
Oleic Acid (liquid-phase       1.46 nonabsorbing................         0.89  Spherical.
 challenge aerosol).
KCl (solid-phase challenge     1.49.............................         1.98  Cubic or agglomerated cubes.
 aerosol).
PSL (calibration aerosol)....  1.59 nonabsorbing................         1.05  Spherical.
----------------------------------------------------------------------------------------------------------------

            8.0 Sample Collection, Preservation, and Storage.

    8.1 In this test, all sampling occurs in real-time, thus no samples 
are collected that require preservation or storage during the test. The 
paint arrestors are shipped and stored to avoid structural damage or 
soiling. Each arrestor may be shipped in its original box from the 
manufacturer or similar cardboard box. Arrestors are stored at the test 
site in a location that keeps them clean and dry. Each arrestor is 
clearly labeled for tracking purposes.

                          9.0 Quality Control.

    9.1 Table 319-1 lists the QC control limits.
    9.2 The standard deviation ([sigma]) of the penetration (P) for a 
given test at each of the 15 OPC sizing channels is computed from the 
coefficient of variation (CV, the standard deviation divided by the 
mean) of the upstream and downstream measurements as:
[GRAPHIC] [TIFF OMITTED] TR27MR98.009

For a properly operating system, the standard deviation of the 
penetration is < 0.10 at particle diameters from 0.3 to 3 [mu]m and less 
than 0.30 at diameters  3 [mu]m.
    9.3 Data Quality Objectives (DQO).
    9.3.1 Fractional Penetration. From the triplicate tests of each 
paint arrestor model, the standard deviation for the penetration 
measurements at each particle size (i.e., for each sizing channel of the 
OPC) is computed as:

[[Page 306]]

[GRAPHIC] [TIFF OMITTED] TR27MR98.010

where Pi represents an individual penetration measurement, 
and P the average of the 3 (n = 3) individual measurements.

    9.3.2 Bias of the fractional penetration values is determined from 
triplicate no-filter and HEPA filter tests. These tests determine the 
measurement bias at 100 percent penetration and 0 percent penetration, 
respectively.
    9.3.3 PSL-Equivalent Light Scattering Diameter. The precision and 
bias of the OPC sizing determination are based on sampling a known 
diameter of PSL and noting whether the particle counts peak in the 
correct channel of the OPC. This is a pass/fail measurement with no 
calculations involved.
    9.3.4 Airflow. The precision of the measurement must be within 5 
percent of the set point.

                  10.0 Calibration and Standardization.

    10.1 Optical Particle Counter. The OPC must have an up-to-date 
factory calibration. Check the OPC zero at the beginning and end of each 
test by sampling HEPA-filtered air. Verify the sizing accuracy on a 
daily basis (for days when tests are performed) with 1-size PSL spheres.
    10.2 Airflow Measurement. Airflow measurement devices must have an 
accuracy of 5 percent or better. Manometers used in conjunction with the 
orifice plate must be inspected prior to use for proper level, zero, and 
mechanical integrity. Tubing connections to the manometer must be free 
from kinks and have secure connections.
    10.3 Pressure Drop. Measure pressure drop across the paint arrestor 
with an inclined manometer readable to within 0.01 in. H2O. 
Prior to use, the level and zero of the manometer, and all tubing 
connections, must be inspected and adjusted as needed.

                             11.0 Procedure.

    11.1 Filtration Efficiency. For both the oleic acid and KCl 
challenges, this procedure is performed in triplicate using a new 
arrestor for each test.
    11.1.1 General Information and Test Duct Preparation
    11.1.1.1 Use the ``Test Run Sheet'' form (Figure 319-2) to record 
the test information.

                                Run Sheet

                       Part 1. General Information

Date and Time:__________________________________________________________

Test Operator:__________________________________________________________

Test :_________________________________________________________

Paint Arrestor:
 Brand/Model____________________________________________________________

 Arrestor Assigned ID _________________________________________
    Condition of arrestor (i.e., is there any damage? Must be new 
condition to proceed):

________________________________________________________________________
    Manometer zero and level confirmed?

________________________________________________________________________

                      Part 2. Clean Efficiency Test

Date and Time:__________________________________________________________
Optical Particle Counter:
 20 min. warm up________________________________________________________

 Zero count (< 50 counts/min)___________________________________________

 Daily PSL check________________________________________________________

PSL Diam: ------ [mu]m

 File name for OPC data:________________________________________________

Test Conditions:
Air Flow: ------

Temp & RH: Temp ------ [deg]F RH ------ %

Atm. Pressure: ------in. Hg
(From mercury barometer)

Aerosol Generator: (record all operating parameters)

________________________________________________________________________

________________________________________________________________________

________________________________________________________________________

________________________________________________________________________

Test Aerosol:
 (Oleic acid or KCl)____________________________________________________
Arrestor:
Pressure drop: at start ------ in. H2O

at end ------ in. H2O

    Condition of arrestor at end of test (note any physical 
deterioration):

________________________________________________________________________

________________________________________________________________________

                      Figure 319-2. Test Run Sheet

    Other report formats which contain the same information are 
acceptable.
    11.1.1.2 Record the date, time, test operator, Test , paint 
arrestor brand/model and its assigned ID number. For tests with no 
arrestor, record none.
    11.1.1.3 Ensure that the arrestor is undamaged and is in ``new'' 
condition.
    11.1.1.4 Mount the arrestor in the appropriate frame. Inspect for 
any airflow leak paths.
    11.1.1.5 Install frame-mounted arrestor in the test duct. Examine 
the installed arrestor to verify that it is sealed in the duct. For 
tests with no arrestor, install the empty frame.

[[Page 307]]

    11.1.1.6 Visually confirm the manometer zero and level. Adjust as 
needed.
    11.1.2 Clean Efficiency Test.
    11.1.2.1 Record the date and time upon beginning this section.
    11.1.2.2 Optical Particle Counter.
    11.1.2.2.1 General: Operate the OPC per the manufacturer's 
instructions allowing a minimum of 20 minutes warm up before making any 
measurements.
    11.1.2.2.2 Overload: The OPC will yield inaccurate data if the 
aerosol concentration it is attempting to measure exceeds its operating 
limit. To ensure reliable measurements, the maximum aerosol 
concentration will not exceed 10 percent of the manufacturer's claimed 
upper concentration limit corresponding to a 10 percent count error. If 
this value is exceeded, reduce the aerosol concentration until the 
acceptable conditions are met.
    11.1.2.2.3 Zero Count: Connect a HEPA capsule to the inlet of the 
OPC and obtain printouts for three samples (each a minimum of 1-minute 
each). Record maximum cumulative zero count. If the count rate exceeds 
50 counts per minute, the OPC requires servicing before continuing.
    11.1.2.2.4 PSL Check of OPC Calibration: Confirm the calibration of 
the OPC by sampling a known size PSL aerosol. Aerosolize the PSL using 
an appropriate nebulizer. Record whether the peak count is observed in 
the proper channel. If the peak is not seen in the appropriate channel, 
have the OPC recalibrated.
    11.1.2.3 Test Conditions:
    11.1.2.3.1 Airflow: The test airflow corresponds to a nominal face 
velocity of 120 FPM through the arrestor. For arrestors having nominal 
20 in.x20 in. face dimensions, this measurement corresponds to an 
airflow of 333 cfm. For arrestors having nominal face dimensions of 24 
in.x24 in., this measurement corresponds to an airflow of 480 cfm.
    11.1.2.3.2 Temperature and Relative Humidity: The temperature and 
relative humidity of the challenge air stream will be measured to within 
an accuracy of 2 [deg]F and 10 percent RH. To protect the probe from fouling, it may 
be removed during periods of aerosol generation.
    11.1.2.3.3 Barometric Pressure: Use a mercury barometer. Record the 
atmospheric pressure.
    11.1.2.4 Upstream and Downstream Background Counts.
    11.1.2.4.1 With the arrestor installed in the test duct and the 
airflow set at the proper value, turn on the data acquisition computer 
and bring up the data acquisition program.
    11.1.2.4.2 Set the OPC settings for the appropriate test sample 
duration with output for both printer and computer data collection.
    11.1.2.4.3 Obtain one set of upstream-downstream background 
measurements.
    11.1.2.4.4 After obtaining the upstream-downstream measurements, 
stop data acquisition.
    11.1.2.5 Efficiency Measurements:
    11.1.2.5.1 Record the arrestor pressure drop.
    11.1.2.5.2 Turn on the Aerosol Generator. Begin aerosol generation 
and record the operating parameters.
    11.1.2.5.3 Monitor the particle counts. Allow a minimum of 5 minutes 
for the generator to stabilize.
    11.1.2.5.4 Confirm that the total particle count does not exceed the 
predetermined upper limit. Adjust generator as needed.
    11.1.2.5.5 Confirm that a minimum of 50 particle counts are measured 
in the upstream sample in each of the OPC channels per sample. (A 
minimum of 50 counts per channel per sample will yield the required 
minimum 500 counts per channel total for the 10 upstream samples as 
specified in Table 319-1.) Adjust generator or sample time as needed.
    11.1.2.5.6 If you are unable to obtain a stable concentration within 
the concentration limit and with the 50 count minimum per channel, 
adjust the aerosol generator.
    11.1.2.5.7 When the counts are stable, perform repeated upstream-
downstream sampling until 10 upstream-downstream measurements are 
obtained.
    11.1.2.5.8 After collection of the 10 upstream-downstream samples, 
stop data acquisition and allow 2 more minutes for final purging of 
generator.
    11.1.2.5.9 Obtain one additional set of upstream-downstream 
background samples.
    11.1.2.5.10 After obtaining the upstream-downstream background 
samples, stop data acquisition.
    11.1.2.5.11 Record the arrestor pressure drop.
    11.1.2.5.12 Turn off blower.
    11.1.2.5.13 Remove the paint arrestor assembly from the test duct. 
Note any signs of physical deterioration.
    11.1.2.5.14 Remove the arrestor from the frame and place the 
arrestor in an appropriate storage bag.
    11.2 Control Test: 100 Percent Penetration Test. A 100 percent 
penetration test must be performed immediately before each individual 
paint arrestor test using the same challenge aerosol substance (i.e., 
oleic acid or KCl) as to be used in the arrestor test. These tests are 
performed with no arrestor installed in the test housing. This test is a 
relatively stringent test of the adequacy of the overall duct, sampling, 
measurement, and aerosol generation system. The test is performed as a 
normal penetration test except the paint arrestor is not used. A perfect 
system would yield a measured penetration of 1 at all particle sizes. 
Deviations from 1

[[Page 308]]

can occur due to particle losses in the duct, differences in the degree 
of aerosol uniformity (i.e., mixing) at the upstream and downstream 
probes, and differences in particle transport efficiency in the upstream 
and downstream sampling lines.
    11.3 Control Test: 0 Percent Penetration. One 0 percent penetration 
test must be performed at least monthly during testing. The test is 
performed by using a HEPA filter rather than a paint arrestor. This test 
assesses the adequacy of the instrument response time and sample line 
lag.

                  12.0 Data Analysis and Calculations.

    12.1 Analysis. The analytical procedures for the fractional 
penetration and flow velocity measurements are described in Section 11. 
Note that the primary measurements, those of the upstream and downstream 
aerosol concentrations, are performed with the OPC which acquires the 
sample and analyzes it in real time. Because all the test data are 
collected in real time, there are no analytical procedures performed 
subsequent to the actual test, only data analysis.
    12.2 Calculations.
    12.2.1 Penetration.

                              Nomenclature

U = Upstream particle count
D = Downstream particle count
Ub = Upstream background count
Db = Downstream background count
P100 = 100 percent penetration value determined immediately 
prior to the arrestor test computed for each channel as:
[GRAPHIC] [TIFF OMITTED] TR27MR98.011

P = Penetration of the arrestor corrected for P100
[rho]= sample standard deviation
CV = coefficient of variation = [rho]/mean
E = Efficiency.

    Overbar denotes arithmetic mean of quantity.
    Analysis of each test involves the following quantities:
     P100 value for each sizing channel 
from the 100 percent penetration control test,
     2 upstream background values,
     2 downstream background values,
     10 upstream values with aerosol generator on, and
     10 downstream values with aerosol generator on.
    Using the values associated with each sizing channel, the 
penetration associated with each particle-sizing channel is calculated 
as:
[GRAPHIC] [TIFF OMITTED] TR27MR98.012

[GRAPHIC] [TIFF OMITTED] TR27MR98.013

    Most often, the background levels are small compared to the values 
when the aerosol generator is on.
    12.3 The relationship between the physical diameter 
(DPhysical) as measured by the OPC to the aerodynamic 
diameter (DAero) is given by:
[GRAPHIC] [TIFF OMITTED] TR27MR98.014

Where:

pO = unit density of 1 g/cm3.
pParticle = the density of the particle, 0.89 g/
cm3 for oleic acid.
CCFPhysical = the Cunningham Correction Factor at 
DPhysical.
CCFAero = the Cunningham Correction Factor at 
DAero.

    12.4 Presentation of Results. For a given arrestor, results will be 
presented for:
     Triplicate arrestor tests with the liquid-phase 
challenge aerosol,
    sbull; Triplicate arrestor tests with the solid-phase challenge 
aerosol,
    sbull; Triplicate 100 percent penetration tests with the liquid-
phase challenge aerosol,
    sbull; Triplicate 100 percent penetration tests with the solid-phase 
challenge aerosol, and
    sbull; One 0 percent filter test (using either the liquid-phase or 
solid-phase aerosol and performed at least monthly).
    12.4.1 Results for the paint arrestor test must be presented in both 
graphical and tabular form. The X-axis of the graph will be a 
logarithmic scale of aerodynamic diameter from 0.1 to 100 [mu]m. The Y-
axis will be efficiency (%) on a linear scale from 0 to 100. Plots for 
each individual run and a plot of

[[Page 309]]

the average of triplicate solid-phase and of the average triplicate 
liquid-phase tests must be prepared. All plots are to be based on point-
to-point plotting (i.e., no curve fitting is to be used). The data are 
to be plotted based on the geometric mean diameter of each of the OPC's 
sizing channels.
    12.4.2 Tabulated data from each test must be provided. The data must 
include the upper and lower diameter bound and geometric mean diameter 
of each of the OPC sizing channels, the background particle counts for 
each channel for each sample, the upstream particle counts for each 
channel for each sample, the downstream particle counts for each channel 
for each sample, the 100 percent penetration values computed for each 
channel, and the 0 percent penetration values computed for each channel.

                       13.0 Pollution Prevention.

    13.1 The quantities of materials to be aerosolized should be 
prepared in accord with the amount needed for the current tests so as to 
prevent wasteful excess.

                         14.0 Waste Management.

    14.1 Paint arrestors may be returned to originator, if requested, or 
disposed of with regular laboratory waste.

                            15.0 References.

    1. Hanley, J.T., D.D. Smith and L. Cox. ``Fractional Penetration of 
Paint Overspray Arrestors, Draft Final Report,'' EPA Cooperative 
Agreement CR-817083-01-0, January 1994.
    2. Hanley, J.T., D.D. Smith, and D.S. Ensor. ``Define a Fractional 
Efficiency Test Method that is Compatible with Particulate Removal Air 
Cleaners Used in General Ventilation,'' Final Report, 671-RP, American 
Society of Heating, Refrigerating, and Air-Conditioning Engineers, Inc., 
December 1993.
    3. ``Project Work and Quality Assurance Plan: Fractional Penetration 
of Paint Overspray Arrestors, Category II,'' EPA Cooperative Agreement 
No. CR-817083, July 1994.

   Test Method 320--Measurement of Vapor Phase Organic and Inorganic 
 Emissions by Extractive Fourier Transform Infrared (FTIR) Spectroscopy

                            1.0 Introduction.

    Persons unfamiliar with basic elements of FTIR spectroscopy should 
not attempt to use this method. This method describes sampling and 
analytical procedures for extractive emission measurements using Fourier 
transform infrared (FTIR) spectroscopy. Detailed analytical procedures 
for interpreting infrared spectra are described in the ``Protocol for 
the Use of Extractive Fourier Transform Infrared (FTIR) Spectrometry in 
Analyses of Gaseous Emissions from Stationary Sources,'' hereafter 
referred to as the ``Protocol.'' Definitions not given in this method 
are given in appendix A of the Protocol. References to specific sections 
in the Protocol are made throughout this Method. For additional 
information refer to references 1 and 2, and other EPA reports, which 
describe the use of FTIR spectrometry in specific field measurement 
applications and validation tests. The sampling procedure described here 
is extractive. Flue gas is extracted through a heated gas transport and 
handling system. For some sources, sample conditioning systems may be 
applicable. Some examples are given in this method.

    Note: sample conditioning systems may be used providing the method 
validation requirements in Sections 9.2 and 13.0 of this method are met.

                      1.1 Scope and Applicability.

    1.1.1 Analytes. Analytes include hazardous air pollutants (HAPs) for 
which EPA reference spectra have been developed. Other compounds can 
also be measured with this method if reference spectra are prepared 
according to section 4.6 of the protocol.
    1.1.2 Applicability. This method applies to the analysis of vapor 
phase organic or inorganic compounds which absorb energy in the mid-
infrared spectral region, about 400 to 4000 cm-1 (25 to 2.5 
[mu]m). This method is used to determine compound-specific 
concentrations in a multi-component vapor phase sample, which is 
contained in a closed-path gas cell. Spectra of samples are collected 
using double beam infrared absorption spectroscopy. A computer program 
is used to analyze spectra and report compound concentrations.
    1.2 Method Range and Sensitivity. Analytical range and sensitivity 
depend on the frequency-dependent analyte absorptivity, instrument 
configuration, data collection parameters, and gas stream composition. 
Instrument factors include: (a) spectral resolution, (b) interferometer 
signal averaging time, (c) detector sensitivity and response, and (d) 
absorption path length.
    1.2.1 For any optical configuration the analytical range is between 
the absorbance values of about .01 (infrared transmittance relative to 
the background = 0.98) and 1.0
(T = 0.1). (For absorbance  1.0 the relation between 
absorbance and concentration may not be linear.)
    1.2.2 The concentrations associated with this absorbance range 
depend primarily on the cell path length and the sample temperature. An 
analyte absorbance greater than 1.0, can be lowered by decreasing the 
optical path length. Analyte absorbance increases with a longer path 
length. Analyte detection also depends on the presence of other species 
exhibiting absorbance in the same analytical

[[Page 310]]

region. Additionally, the estimated lower absorbance (A) limit
(A = 0.01) depends on the root mean square deviation (RMSD) noise in the 
analytical region.
    1.2.3 The concentration range of this method is determined by the 
choice of optical configuration.
    1.2.3.1 The absorbance for a given concentration can be decreased by 
decreasing the path length or by diluting the sample. There is no 
practical upper limit to the measurement range.
    1.2.3.2 The analyte absorbance for a given concentration may be 
increased by increasing the cell path length or (to some extent) using a 
higher resolution. Both modifications also cause a corresponding 
increased absorbance for all compounds in the sample, and a decrease in 
the signal throughput. For this reason the practical lower detection 
range (quantitation limit) usually depends on sample characteristics 
such as moisture content of the gas, the presence of other interferants, 
and losses in the sampling system.
    1.3 Sensitivity. The limit of sensitivity for an optical 
configuration and integration time is determined using appendix D of the 
Protocol: Minimum Analyte Uncertainty, (MAU). The MAU depends on the 
RMSD noise in an analytical region, and on the absorptivity of the 
analyte in the same region.
    1.4 Data Quality. Data quality shall be determined by executing 
Protocol pre-test procedures in appendices B to H of the protocol and 
post-test procedures in appendices I and J of the protocol.
    1.4.1 Measurement objectives shall be established by the choice of 
detection limit (DLi) and analytical uncertainty 
(AUi) for each analyte.
    1.4.2 An instrumental configuration shall be selected. An estimate 
of gas composition shall be made based on previous test data, data from 
a similar source or information gathered in a pre-test site survey. 
Spectral interferants shall be identified using the selected 
DLi and AUi and band areas from reference spectra 
and interferant spectra. The baseline noise of the system shall be 
measured in each analytical region to determine the MAU of the 
instrument configuration for each analyte and interferant 
(MIUi).
    1.4.3 Data quality for the application shall be determined, in part, 
by measuring the RMS (root mean square) noise level in each analytical 
spectral region (appendix C of the Protocol). The RMS noise is defined 
as the RMSD of the absorbance values in an analytical region from the 
mean absorbance value in the region.
    1.4.4 The MAU is the minimum analyte concentration for which the 
AUi can be maintained; if the measured analyte concentration 
is less than MAUi then data quality are unacceptable.

                          2.0 Summary of Method

    2.1 Principle. References 4 through 7 provide background material on 
infrared spectroscopy and quantitative analysis. A summary is given in 
this section.
    2.1.1 Infrared absorption spectroscopy is performed by directing an 
infrared beam through a sample to a detector. The frequency-dependent 
infrared absorbance of the sample is measured by comparing this detector 
signal (single beam spectrum) to a signal obtained without a sample in 
the beam path (background).
    2.1.2 Most molecules absorb infrared radiation and the absorbance 
occurs in a characteristic and reproducible pattern. The infrared 
spectrum measures fundamental molecular properties and a compound can be 
identified from its infrared spectrum alone.
    2.1.3 Within constraints, there is a linear relationship between 
infrared absorption and compound concentration. If this frequency 
dependent relationship (absorptivity) is known (measured), it can be 
used to determine compound concentration in a sample mixture.
    2.1.4 Absorptivity is measured by preparing, in the laboratory, 
standard samples of compounds at known concentrations and measuring the 
FTIR ``reference spectra'' of these standard samples. These ``reference 
spectra'' are then used in sample analysis: (1) Compounds are detected 
by matching sample absorbance bands with bands in reference spectra, and 
(2) concentrations are measured by comparing sample band intensities 
with reference band intensities.
    2.1.5 This method is self-validating provided that the results meet 
the performance requirement of the QA spike in sections 8.6.2 and 9.0 of 
this method, and results from a previous method validation study support 
the use of this method in the application.
    2.2 Sampling and Analysis. In extractive sampling a probe assembly 
and pump are used to extract gas from the exhaust of the affected source 
and transport the sample to the FTIR gas cell. Typically, the sampling 
apparatus is similar to that used for single-component continuous 
emission monitor (CEM) measurements.
    2.2.1 The digitized infrared spectrum of the sample in the FTIR gas 
cell is measured and stored on a computer. Absorbance band intensities 
in the spectrum are related to sample concentrations by what is commonly 
referred to as Beer's Law.
[GRAPHIC] [TIFF OMITTED] TR14JN99.003

Where:

Ai = absorbance at a given frequency of the ith sample 
component.
ai = absorption coefficient (absorptivity) of the ith sample 
component.
b = path length of the cell.

[[Page 311]]

ci = concentration of the ith sample component.

    2.2.2 Analyte spiking is used for quality assurance (QA). In this 
procedure (section 8.6.2 of this method) an analyte is spiked into the 
gas stream at the back end of the sample probe. Analyte concentrations 
in the spiked samples are compared to analyte concentrations in unspiked 
samples. Since the concentration of the spike is known, this procedure 
can be used to determine if the sampling system is removing the spiked 
analyte(s) from the sample stream.
    2.3 Reference Spectra Availability. Reference spectra of over 100 
HAPs are available in the EPA FTIR spectral library on the EMTIC 
(Emission Measurement Technical Information Center) computer bulletin 
board service and at internet address http://info.arnold.af.mil/epa/
welcome.htm. Reference spectra for HAPs, or other analytes, may also be 
prepared according to section 4.6 of the Protocol.
    2.4 Operator Requirements. The FTIR analyst shall be trained in 
setting up the instrumentation, verifying the instrument is functioning 
properly, and performing routine maintenance. The analyst must evaluate 
the initial sample spectra to determine if the sample matrix is 
consistent with pre-test assumptions and if the instrument configuration 
is suitable. The analyst must be able to modify the instrument 
configuration, if necessary.
    2.4.1 The spectral analysis shall be supervised by someone familiar 
with EPA FTIR Protocol procedures.
    2.4.2 A technician trained in instrumental test methods is qualified 
to install and operate the sampling system. This includes installing the 
probe and heated line assembly, operating the analyte spike system, and 
performing moisture and flow measurements.

                             3.0 Definitions

    See appendix A of the Protocol for definitions relating to infrared 
spectroscopy. Additional definitions are given in sections 3.1 through 
3.29.
    3.1 Analyte. A compound that this method is used to measure. The 
term ``target analyte'' is also used. This method is multi-component and 
a number of analytes can be targeted for a test.
    3.2 Reference Spectrum. Infrared spectrum of an analyte prepared 
under controlled, documented, and reproducible laboratory conditions 
according to procedures in section 4.6 of the Protocol. A library of 
reference spectra is used to measure analytes in gas samples.
    3.3 Standard Spectrum. A spectrum that has been prepared from a 
reference spectrum through a (documented) mathematical operation. A 
common example is de-resolving of reference spectra to lower-resolution 
standard spectra (Protocol, appendix K to the addendum of this method). 
Standard spectra, prepared by approved, and documented, procedures can 
be used as reference spectra for analysis.
    3.4 Concentration. In this method concentration is expressed as a 
molar concentration, in ppm-meters, or in (ppm-meters)/K, where K is the 
absolute temperature (Kelvin). The latter units allow the direct 
comparison of concentrations from systems using different optical 
configurations or sampling temperatures.
    3.5 Interferant. A compound in the sample matrix whose infrared 
spectrum overlaps with part of an analyte spectrum. The most accurate 
analyte measurements are achieved when reference spectra of interferants 
are used in the quantitative analysis with the analyte reference 
spectra. The presence of an interferant can increase the analytical 
uncertainty in the measured analyte concentration.
    3.6 Gas Cell. A gas containment cell that can be evacuated. It is 
equipped with the optical components to pass the infrared beam through 
the sample to the detector. Important cell features include: path length 
(or range if variable), temperature range, materials of construction, 
and total gas volume.
    3.7 Sampling System. Equipment used to extract the sample from the 
test location and transport the sample gas to the FTIR analyzer. This 
includes sample conditioning systems.
    3.8 Sample Analysis. The process of interpreting the infrared 
spectra to obtain sample analyte concentrations. This process is usually 
automated using a software routine employing a classical least squares 
(cls), partial least squares (pls), or K- or P-matrix method.
    3.9 One hundred percent line. A double beam transmittance spectrum 
obtained by combining two background single beam spectra. Ideally, this 
line is equal to 100 percent transmittance (or zero absorbance) at every 
frequency in the spectrum. Practically, a zero absorbance line is used 
to measure the baseline noise in the spectrum.
    3.10 Background Deviation. A deviation from 100 percent 
transmittance in any region of the 100 percent line. Deviations greater 
than 5 percent in an analytical region are 
unacceptable (absorbance of 0.021 to -0.022). Such deviations indicate a 
change in the instrument throughput relative to the background single 
beam.
    3.11 Batch Sampling. A procedure where spectra of discreet, static 
samples are collected. The gas cell is filled with sample and the cell 
is isolated. The spectrum is collected. Finally, the cell is evacuated 
to prepare for the next sample.
    3.12 Continuous Sampling. A procedure where spectra are collected 
while sample gas

[[Page 312]]

is flowing through the cell at a measured rate.
    3.13 Sampling resolution. The spectral resolution used to collect 
sample spectra.
    3.14 Truncation. Limiting the number of interferogram data points by 
deleting points farthest from the center burst (zero path difference, 
ZPD).
    3.15 Zero filling. The addition of points to the interferogram. The 
position of each added point is interpolated from neighboring real data 
points. Zero filling adds no information to the interferogram, but 
affects line shapes in the absorbance spectrum (and possibly analytical 
results).
    3.16 Reference CTS. Calibration Transfer Standard spectra that were 
collected with reference spectra.
    3.17 CTS Standard. CTS spectrum produced by applying a de-resolution 
procedure to a reference CTS.
    3.18 Test CTS. CTS spectra collected at the sampling resolution 
using the same optical configuration as for sample spectra. Test spectra 
help verify the resolution, temperature and path length of the FTIR 
system.
    3.19 RMSD. Root Mean Square Difference, defined in EPA FTIR 
Protocol, appendix A.
    3.20 Sensitivity. The noise-limited compound-dependent detection 
limit for the FTIR system configuration. This is estimated by the MAU. 
It depends on the RMSD in an analytical region of a zero absorbance 
line.
    3.21 Quantitation Limit. The lower limit of detection for the FTIR 
system configuration in the sample spectra. This is estimated by 
mathematically subtracting scaled reference spectra of analytes and 
interferences from sample spectra, then measuring the RMSD in an 
analytical region of the subtracted spectrum. Since the noise in 
subtracted sample spectra may be much greater than in a zero absorbance 
spectrum, the quantitation limit is generally much higher than the 
sensitivity. Removing spectral interferences from the sample or 
improving the spectral subtraction can lower the quantitation limit 
toward (but not below) the sensitivity.
    3.22 Independent Sample. A unique volume of sample gas; there is no 
mixing of gas between two consecutive independent samples. In continuous 
sampling two independent samples are separated by at least 5 cell 
volumes. The interval between independent measurements depends on the 
cell volume and the sample flow rate (through the cell).
    3.23 Measurement. A single spectrum of flue gas contained in the 
FTIR cell.
    3.24 Run. A run consists of a series of measurements. At a minimum a 
run includes 8 independent measurements spaced over 1 hour.
    3.25 Validation. Validation of FTIR measurements is described in 
sections 13.0 through 13.4 of this method. Validation is used to verify 
the test procedures for measuring specific analytes at a source. 
Validation provides proof that the method works under certain test 
conditions.
    3.26 Validation Run. A validation run consists of at least 24 
measurements of independent samples. Half of the samples are spiked and 
half are not spiked. The length of the run is determined by the interval 
between independent samples.
    3.27 Screening. Screening is used when there is little or no 
available information about a source. The purpose of screening is to 
determine what analytes are emitted and to obtain information about 
important sample characteristics such as moisture, temperature, and 
interferences. Screening results are semi-quantitative (estimated 
concentrations) or qualitative (identification only). Various optical 
and sampling configurations may be used. Sample conditioning systems may 
be evaluated for their effectiveness in removing interferences. It is 
unnecessary to perform a complete run under any set of sampling 
conditions. Spiking is not necessary, but spiking can be a useful 
screening tool for evaluating the sampling system, especially if a 
reactive or soluble analyte is used for the spike.
    3.28 Emissions Test. An FTIR emissions test is performed according 
specific sampling and analytical procedures. These procedures, for the 
target analytes and the source, are based on previous screening and 
validation results. Emission results are quantitative. A QA spike 
(sections 8.6.2 and 9.2 of this method) is performed under each set of 
sampling conditions using a representative analyte. Flow, gas 
temperature and diluent data are recorded concurrently with the FTIR 
measurements to provide mass emission rates for detected compounds.
    3.29 Surrogate. A surrogate is a compound that is used in a QA spike 
procedure (section 8.6.2 of this method) to represent other compounds. 
The chemical and physical properties of a surrogate shall be similar to 
the compounds it is chosen to represent. Under given sampling 
conditions, usually a single sampling factor is of primary concern for 
measuring the target analytes: for example, the surrogate spike results 
can be representative for analytes that are more reactive, more soluble, 
have a lower absorptivity, or have a lower vapor pressure than the 
surrogate itself.

                            4.0 Interferences

    Interferences are divided into two classifications: analytical and 
sampling.
    4.1 Analytical Interferences. An analytical interference is a 
spectral feature that complicates (in extreme cases may prevent) the 
analysis of an analyte. Analytical interferences are classified as 
background or spectral interference.
    4.1.1 Background Interference. This results from a change in 
throughput relative to the

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single beam background. It is corrected by collecting a new background 
and proceeding with the test. In severe instances the cause must be 
identified and corrected. Potential causes include: (1) Deposits on 
reflective surfaces or transmitting windows, (2) changes in detector 
sensitivity, (3) a change in the infrared source output, or (4) failure 
in the instrument electronics. In routine sampling throughput may 
degrade over several hours. Periodically a new background must be 
collected, but no other corrective action will be required.
    4.1.2 Spectral Interference. This results from the presence of 
interfering compound(s) (interferant) in the sample. Interferant 
spectral features overlap analyte spectral features. Any compound with 
an infrared spectrum, including analytes, can potentially be an 
interferant. The Protocol measures absorbance band overlap in each 
analytical region to determine if potential interferants shall be 
classified as known interferants (FTIR Protocol, section 4.9 and 
appendix B). Water vapor and CO2 are common spectral 
interferants. Both of these compounds have strong infrared spectra and 
are present in many sample matrices at high concentrations relative to 
analytes. The extent of interference depends on the (1) interferant 
concentration, (2) analyte concentration, and (3) the degree of band 
overlap. Choosing an alternate analytical region can minimize or avoid 
the spectral interference. For example, CO2 interferes with 
the analysis of the 670 cm-1 benzene band. However, benzene 
can also be measured near 3000 cm-1 (with less sensitivity).
    4.2 Sampling System Interferences. These prevent analytes from 
reaching the instrument. The analyte spike procedure is designed to 
measure sampling system interference, if any.
    4.2.1 Temperature. A temperature that is too low causes condensation 
of analytes or water vapor. The materials of the sampling system and the 
FTIR gas cell usually set the upper limit of temperature.
    4.2.2 Reactive Species. Anything that reacts with analytes. Some 
analytes, like formaldehyde, polymerize at lower temperatures.
    4.2.3 Materials. Poor choice of material for probe, or sampling line 
may remove some analytes. For example, HF reacts with glass components.
    4.2.4 Moisture. In addition to being a spectral interferant, 
condensed moisture removes soluble compounds.

                               5.0 Safety

    The hazards of performing this method are those associated with any 
stack sampling method and the same precautions shall be followed. Many 
HAPs are suspected carcinogens or present other serious health risks. 
Exposure to these compounds should be avoided in all circumstances. For 
instructions on the safe handling of any particular compound, refer to 
its material safety data sheet. When using analyte standards, always 
ensure that gases are properly vented and that the gas handling system 
is leak free. (Always perform a leak check with the system under maximum 
vacuum and, again, with the system at greater than ambient pressure.) 
Refer to section 8.2 of this method for leak check procedures. This 
method does not address all of the potential safety risks associated 
with its use. Anyone performing this method must follow safety and 
health practices consistent with applicable legal requirements and with 
prudent practice for each application.

                       6.0 Equipment and Supplies

    Note: Mention of trade names or specific products does not 
constitute endorsement by the Environmental Protection Agency.

    The equipment and supplies are based on the schematic of a sampling 
system shown in Figure 1. Either the batch or continuous sampling 
procedures may be used with this sampling system. Alternative sampling 
configurations may also be used, provided that the data quality 
objectives are met as determined in the post-analysis evaluation. Other 
equipment or supplies may be necessary, depending on the design of the 
sampling system or the specific target analytes.
    6.1 Sampling Probe. Glass, stainless steel, or other appropriate 
material of sufficient length and physical integrity to sustain heating, 
prevent adsorption of analytes, and to transport analytes to the 
infrared gas cell. Special materials or configurations may be required 
in some applications. For instance, high stack sample temperatures may 
require special steel or cooling the probe. For very high moisture 
sources it may be desirable to use a dilution probe.
    6.2 Particulate Filters. A glass wool plug (optional) inserted at 
the probe tip (for large particulate removal) and a filter (required) 
rated for 99 percent removal efficiency at 1-micron (e.g., Balston'') 
connected at the outlet of the heated probe.
    6.3 Sampling Line/Heating System. Heated (sufficient to prevent 
condensation) stainless steel, polytetrafluoroethane, or other material 
inert to the analytes.
    6.4 Gas Distribution Manifold. A heated manifold allowing the 
operator to control flows of gas standards and samples directly to the 
FTIR system or through sample conditioning systems. Usually includes 
heated flow meter, heated valve for selecting and sending sample to the 
analyzer, and a by-pass vent. This is typically constructed of stainless 
steel tubing and fittings, and high-temperature valves.
    6.5 Stainless Steel Tubing. Type 316, appropriate diameter (e.g., 3/
8 in.) and length for

[[Page 314]]

heated connections. Higher grade stainless may be desirable in some 
applications.
    6.6 Calibration/Analyte Spike Assembly. A three way valve assembly 
(or equivalent) to introduce analyte or surrogate spikes into the 
sampling system at the outlet of the probe upstream of the out-of-stack 
particulate filter and the FTIR analytical system.
    6.7 Mass Flow Meter (MFM). These are used for measuring analyte 
spike flow. The MFM shall be calibrated in the range of 0 to 5 L/min and 
be accurate to  2 percent (or better) of the flow 
meter span.
    6.8 Gas Regulators. Appropriate for individual gas standards.
    6.9 Polytetrafluoroethane Tubing. Diameter (e.g., \3/8\ in.) and 
length suitable to connect cylinder regulators to gas standard manifold.
    6.10 Sample Pump. A leak-free pump (e.g., KNFTM), with 
by-pass valve, capable of producing a sample flow rate of at least 10 L/
min through 100 ft of sample line. If the pump is positioned upstream of 
the distribution manifold and FTIR system, use a heated pump that is 
constructed from materials non-reactive to the analytes. If the pump is 
located downstream of the FTIR system, the gas cell sample pressure will 
be lower than ambient pressure and it must be recorded at regular 
intervals.
    6.11 Gas Sample Manifold. Secondary manifold to control sample flow 
at the inlet to the FTIR manifold. This is optional, but includes a by-
pass vent and heated rotameter.
    6.12 Rotameter. A 0 to 20 L/min rotameter. This meter need not be 
calibrated.
    6.13 FTIR Analytical System. Spectrometer and detector, capable of 
measuring the analytes to the chosen detection limit. The system shall 
include a personal computer with compatible software allowing automated 
collection of spectra.
    6.14 FTIR Cell Pump. Required for the batch sampling technique, 
capable of evacuating the FTIR cell volume within 2 minutes. The pumping 
speed shall allow the operator to obtain 8 sample spectra in 1 hour.
    6.15 Absolute Pressure Gauge. Capable of measuring pressure from 0 
to 1000 mmHg to within 2.5 mmHg (e.g., 
BaratronTM).
    6.16 Temperature Gauge. Capable of measuring the cell temperature to 
within  2 [deg]C.
    6.17 Sample Conditioning. One option is a condenser system, which is 
used for moisture removal. This can be helpful in the measurement of 
some analytes. Other sample conditioning procedures may be devised for 
the removal of moisture or other interfering species.
    6.17.1 The analyte spike procedure of section 9.2 of this method, 
the QA spike procedure of section 8.6.2 of this method, and the 
validation procedure of section 13 of this method demonstrate whether 
the sample conditioning affects analyte concentrations. Alternatively, 
measurements can be made with two parallel FTIR systems; one measuring 
conditioned sample, the other measuring unconditioned sample.
    6.17.2 Another option is sample dilution. The dilution factor 
measurement must be documented and accounted for in the reported 
concentrations. An alternative to dilution is to lower the sensitivity 
of the FTIR system by decreasing the cell path length, or to use a 
short-path cell in conjunction with a long path cell to measure more 
than one concentration range.

                       7.0 Reagents and Standards

    7.1 Analyte(s) and Tracer Gas. Obtain a certified gas cylinder 
mixture containing all of the analyte(s) at concentrations within 2 percent of the emission source levels (expressed in 
ppm-meter/K). If practical, the analyte standard cylinder shall also 
contain the tracer gas at a concentration which gives a measurable 
absorbance at a dilution factor of at least 10:1. Two ppm SF6 
is sufficient for a path length of 22 meters at 250 [deg]F.
    7.2 Calibration Transfer Standard(s). Select the calibration 
transfer standards (CTS) according to section 4.5 of the FTIR Protocol. 
Obtain a National Institute of Standards and Technology (NIST) traceable 
gravimetric standard of the CTS ( 2 percent).
    7.3 Reference Spectra. Obtain reference spectra for each analyte, 
interferant, surrogate, CTS, and tracer. If EPA reference spectra are 
not available, use reference spectra prepared according to procedures in 
section 4.6 of the EPA FTIR Protocol.

                   8.0 Sampling and Analysis Procedure

    Three types of testing can be performed: (1) Screening, (2) 
emissions test, and (3) validation. Each is defined in section 3 of this 
method. Determine the purpose(s) of the FTIR test. Test requirements 
include: (a) AUi, DLi, overall fractional 
uncertainty, OFUi, maximum expected concentration 
(CMAXi), and tAN for each, (b) potential 
interferants, (c) sampling system factors, e.g., minimum absolute cell 
pressure, (Pmin), FTIR cell volume (VSS), 
estimated sample absorption pathlength, LS', estimated sample 
pressure, PS', TS', signal integration time 
(tSS), minimum instrumental linewidth, MIL, fractional error, 
and (d) analytical regions, e.g., m = 1 to M, lower wavenumber position, 
FLm, center wavenumber position, FCm, and upper wavenumber 
position, FUm, plus interferants, upper wavenumber position 
of the CTS absorption band, FFUm, lower wavenumber position 
of the CTS absorption band, FFLm, wavenumber range FNU to 
FNL. If necessary, sample and acquire an initial spectrum. From analysis 
of this preliminary spectrum determine a suitable operational path 
length. Set up the sampling train as shown in Figure 1 or use an 
appropriate alternative configuration. Sections 8.1 through 8.11 of this 
method provide guidance on pre-

[[Page 315]]

test calculations in the EPA protocol, sampling and analytical 
procedures, and post-test protocol calculations.
    8.1 Pretest Preparations and Evaluations. Using the procedure in 
section 4.0 of the FTIR Protocol, determine the optimum sampling system 
configuration for measuring the target analytes. Use available 
information to make reasonable assumptions about moisture content and 
other interferences.
    8.1.1 Analytes. Select the required detection limit (DLi) 
and the maximum permissible analytical uncertainty (AUi) for 
each analyte (labeled from 1 to i). Estimate, if possible, the maximum 
expected concentration for each analyte, CMAXi. The expected 
measurement range is fixed by DLi and CMAXi for 
each analyte (i).
    8.1.2 Potential Interferants. List the potential interferants. This 
usually includes water vapor and CO2, but may also include 
some analytes and other compounds.
    8.1.3. Optical Configuration. Choose an optical configuration that 
can measure all of the analytes within the absorbance range of .01 to 
1.0 (this may require more than one path length). Use Protocol sections 
4.3 to 4.8 for guidance in choosing a configuration and measuring CTS.
    8.1.4 Fractional Reproducibility Uncertainty (FRUi). The 
FRU is determined for each analyte by comparing CTS spectra taken before 
and after the reference spectra were measured. The EPA para-xylene 
reference spectra were collected on 10/31/91 and 11/01/91 with 
corresponding CTS spectra ``cts1031a,'' and ``cts1101b.'' The CTS 
spectra are used to estimate the reproducibility (FRU) in the system 
that was used to collect the references. The FRU must be < AU. Appendix 
E of the protocol is used to calculate the FRU from CTS spectra. Figure 
2 plots results for 0.25 cm-1 CTS spectra in EPA reference 
library: S3 (cts1101b-cts1031a), and S4 
[(cts1101b+cts1031a)/2]. The RMSD (SRMS) is calculated in the subtracted 
baseline, S3, in the corresponding CTS region from 850 to 
1065 cm-1. The area (BAV) is calculated in the same region of 
the averaged CTS spectrum, S4.
    8.1.5 Known Interferants. Use appendix B of the EPA FTIR Protocol.
    8.1.6 Calculate the Minimum Analyte Uncertainty, MAU (section 1.3 of 
this method discusses MAU and protocol appendix D gives the MAU 
procedure). The MAU for each analyte, i, and each analytical region, m, 
depends on the RMS noise.
    8.1.7 Analytical Program. See FTIR Protocol, section 4.10. Prepare 
computer program based on the chosen analytical technique. Use as input 
reference spectra of all target analytes and expected interferants. 
Reference spectra of additional compounds shall also be included in the 
program if their presence (even if transient) in the samples is 
considered possible. The program output shall be in ppm (or ppb) and 
shall be corrected for differences between the reference path length, 
LR, temperature, TR, and pressure, PR, 
and the conditions used for collecting the sample spectra. If sampling 
is performed at ambient pressure, then any pressure correction is 
usually small relative to corrections for path length and temperature, 
and may be neglected.

                             8.2 Leak-Check

    8.2.1 Sampling System. A typical FTIR extractive sampling train is 
shown in Figure 1. Leak check from the probe tip to pump outlet as 
follows: Connect a 0-to 250-mL/min rate meter (rotameter or bubble 
meter) to the outlet of the pump. Close off the inlet to the probe, and 
record the leak rate. The leak rate shall be <=200 mL/min.
    8.2.2 Analytical System Leak check. Leak check the FTIR cell under 
vacuum and under pressure (greater than ambient). Leak check connecting 
tubing and inlet manifold under pressure.
    8.2.2.1 For the evacuated sample technique, close the valve to the 
FTIR cell, and evacuate the absorption cell to the minimum absolute 
pressure Pmin. Close the valve to the pump, and determine the 
change in pressure [Delta]Pv after 2 minutes.
    8.2.2.2 For both the evacuated sample and purging techniques, 
pressurize the system to about 100 mmHg above atmospheric pressure. 
Isolate the pump and determine the change in pressure 
[Delta]Pp after 2 minutes.
    8.2.2.3 Measure the barometric pressure, Pb in mmHg.
    8.2.2.4 Determine the percent leak volume %VL for the 
signal integration time tSS and for [Delta]Pmax, 
i.e., the larger of [Delta]Pv or [Delta]Pp, as 
follows:
[GRAPHIC] [TIFF OMITTED] TR14JN99.004

where 50 = 100% divided by the leak-check time of 2 minutes. 8.2.2.5 
Leak volumes in excess of 4 percent of the FTIR system volume 
VSS are unacceptable.
    8.3 Detector Linearity. Once an optical configuration is chosen, use 
one of the procedures of sections 8.3.1 through 8.3.3 to verify that the 
detector response is linear. If the detector response is not linear, 
decrease the aperture, or attenuate the infrared beam. After a change in 
the instrument configuration perform a linearity check until it is 
demonstrated that the detector response is linear.
    8.3.1 Vary the power incident on the detector by modifying the 
aperture setting. Measure the background and CTS at three instrument 
aperture settings: (1) at the aperture setting to be used in the 
testing, (2) at one half this aperture and (3) at twice the proposed 
testing aperture. Compare the

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three CTS spectra. CTS band areas shall agree to within the uncertainty 
of the cylinder standard and the RMSD noise in the system. If test 
aperture is the maximum aperture, collect CTS spectrum at maximum 
aperture, then close the aperture to reduce the IR throughput by half. 
Collect a second background and CTS at the smaller aperture setting and 
compare the spectra again.
    8.3.2 Use neutral density filters to attenuate the infrared beam. 
Set up the FTIR system as it will be used in the test measurements. 
Collect a CTS spectrum. Use a neutral density filter to attenuate the 
infrared beam (either immediately after the source or the 
interferometer) to approximately \1/2\ its original intensity. Collect a 
second CTS spectrum. Use another filter to attenuate the infrared beam 
to approximately \1/4\ its original intensity. Collect a third 
background and CTS spectrum. Compare the CTS spectra. CTS band areas 
shall agree to within the uncertainty of the cylinder standard and the 
RMSD noise in the system.
    8.3.3 Observe the single beam instrument response in a frequency 
region where the detector response is known to be zero. Verify that the 
detector response is ``flat'' and equal to zero in these regions.
    8.4 Data Storage Requirements. All field test spectra shall be 
stored on a computer disk and a second backup copy must stored on a 
separate disk. The stored information includes sample interferograms, 
processed absorbance spectra, background interferograms, CTS sample 
interferograms and CTS absorbance spectra. Additionally, documentation 
of all sample conditions, instrument settings, and test records must be 
recorded on hard copy or on computer medium. Table 1 gives a sample 
presentation of documentation.
    8.5 Background Spectrum. Evacuate the gas cell to <=5 mmHg, and fill 
with dry nitrogen gas to ambient pressure (or purge the cell with 10 
volumes of dry nitrogen). Verify that no significant amounts of 
absorbing species (for example water vapor and CO2) are 
present. Collect a background spectrum, using a signal averaging period 
equal to or greater than the averaging period for the sample spectra. 
Assign a unique file name to the background spectrum. Store two copies 
of the background interferogram and processed single-beam spectrum on 
separate computer disks (one copy is the back-up).
    8.5.1 Interference Spectra. If possible, collect spectra of known 
and suspected major interferences using the same optical system that 
will be used in the field measurements. This can be done on-site or 
earlier. A number of gases, e.g. CO2, SO2, CO, 
NH3, are readily available from cylinder gas suppliers.
    8.5.2 Water vapor spectra can be prepared by the following 
procedure. Fill a sample tube with distilled water. Evacuate above the 
sample and remove dissolved gasses by alternately freezing and thawing 
the water while evacuating. Allow water vapor into the FTIR cell, then 
dilute to atmospheric pressure with nitrogen or dry air. If quantitative 
water spectra are required, follow the reference spectrum procedure for 
neat samples (protocol, section 4.6). Often, interference spectra need 
not be quantitative, but for best results the absorbance must be 
comparable to the interference absorbance in the sample spectra.

                        8.6 Pre-Test Calibrations

    8.6.1 Calibration Transfer Standard. Evacuate the gas cell to <= 5 
mmHg absolute pressure, and fill the FTIR cell to atmospheric pressure 
with the CTS gas. Alternatively, purge the cell with 10 cell volumes of 
CTS gas. (If purge is used, verify that the CTS concentration in the 
cell is stable by collecting two spectra 2 minutes apart as the CTS gas 
continues to flow. If the absorbance in the second spectrum is no 
greater than in the first, within the uncertainty of the gas standard, 
then this can be used as the CTS spectrum.) Record the spectrum.
    8.6.2 QA Spike. This procedure assumes that the method has been 
validated for at least some of the target analytes at the source. For 
emissions testing perform a QA spike. Use a certified standard, if 
possible, of an analyte, which has been validated at the source. One 
analyte standard can serve as a QA surrogate for other analytes which 
are less reactive or less soluble than the standard. Perform the spike 
procedure of section 9.2 of this method. Record spectra of at least 
three independent (section 3.22 of this method) spiked samples. 
Calculate the spiked component of the analyte concentration. If the 
average spiked concentration is within 0.7 to 1.3 times the expected 
concentration, then proceed with the testing. If applicable, apply the 
correction factor from the Method 301 of this appendix validation test 
(not the result from the QA spike).
    8.7 Sampling. If analyte concentrations vary rapidly with time, 
continuous sampling is preferable using the smallest cell volume, 
fastest sampling rate and fastest spectra collection rate possible. 
Continuous sampling requires the least operator intervention even 
without an automated sampling system. For continuous monitoring at one 
location over long periods, Continuous sampling is preferred. Batch 
sampling and continuous static sampling are used for screening and 
performing test runs of finite duration. Either technique is preferred 
for sampling several locations in a matter of days. Batch sampling gives 
reasonably good time resolution and ensures that each spectrum measures 
a discreet (and unique) sample volume. Continuous static (and 
continuous) sampling provide a very stable background over long periods. 
Like batch sampling, continuous static

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sampling also ensures that each spectrum measures a unique sample 
volume. It is essential that the leak check procedure under vacuum 
(section 8.2 of this method) is passed if the batch sampling procedure 
is used. It is essential that the leak check procedure under positive 
pressure is passed if the continuous static or continuous sampling 
procedures are used. The sampling techniques are described in sections 
8.7.1 through 8.7.2 of this method.
    8.7.1 Batch Sampling. Evacuate the absorbance cell to <=5 mmHg 
absolute pressure. Fill the cell with exhaust gas to ambient pressure, 
isolate the cell, and record the spectrum. Before taking the next 
sample, evacuate the cell until no spectral evidence of sample 
absorption remains. Repeat this procedure to collect eight spectra of 
separate samples in 1 hour.
    8.7.2 Continuous Static Sampling. Purge the FTIR cell with 10 cell 
volumes of sample gas. Isolate the cell, collect the spectrum of the 
static sample and record the pressure. Before measuring the next sample, 
purge the cell with 10 more cell volumes of sample gas.

                      8.8 Sampling QA and Reporting

    8.8.1 Sample integration times shall be sufficient to achieve the 
required signal-to-noise ratio. Obtain an absorbance spectrum by filling 
the cell with N2. Measure the RMSD in each analytical region in this 
absorbance spectrum. Verify that the number of scans used is sufficient 
to achieve the target MAU.
    8.8.2 Assign a unique file name to each spectrum.
    8.8.3 Store two copies of sample interferograms and processed 
spectra on separate computer disks.
    8.8.4 For each sample spectrum, document the sampling conditions, 
the sampling time (while the cell was being filled), the time the 
spectrum was recorded, the instrumental conditions (path length, 
temperature, pressure, resolution, signal integration time), and the 
spectral file name. Keep a hard copy of these data sheets.
    8.9 Signal Transmittance. While sampling, monitor the signal 
transmittance. If signal transmittance (relative to the background) 
changes by 5 percent or more (absorbance = -.02 to .02) in any 
analytical spectral region, obtain a new background spectrum.
    8.10 Post-test CTS. After the sampling run, record another CTS 
spectrum.
    8.11 Post-test QA
    8.11.1 Inspect the sample spectra immediately after the run to 
verify that the gas matrix composition was close to the expected 
(assumed) gas matrix.
    8.11.2 Verify that the sampling and instrumental parameters were 
appropriate for the conditions encountered. For example, if the moisture 
is much greater than anticipated, it may be necessary to use a shorter 
path length or dilute the sample.
    8.11.3 Compare the pre- and post-test CTS spectra. The peak 
absorbance in pre- and post-test CTS must be 5 
percent of the mean value. See appendix E of the FTIR Protocol.

                           9.0 Quality Control

    Use analyte spiking (sections 8.6.2, 9.2 and 13.0 of this method) to 
verify that the sampling system can transport the analytes from the 
probe to the FTIR system.
    9.1 Spike Materials. Use a certified standard (accurate to 2 percent) of the target analyte, if one can be 
obtained. If a certified standard cannot be obtained, follow the 
procedures in section 4.6.2.2 of the FTIR Protocol.
    9.2 Spiking Procedure. QA spiking (section 8.6.2 of this method) is 
a calibration procedure used before testing. QA spiking involves 
following the spike procedure of sections 9.2.1 through 9.2.3 of this 
method to obtain at least three spiked samples. The analyte 
concentrations in the spiked samples shall be compared to the expected 
spike concentration to verify that the sampling/analytical system is 
working properly. Usually, when QA spiking is used, the method has 
already been validated at a similar source for the analyte in question. 
The QA spike demonstrates that the validated sampling/analytical 
conditions are being duplicated. If the QA spike fails then the 
sampling/analytical system shall be repaired before testing proceeds. 
The method validation procedure (section 13.0 of this method) involves a 
more extensive use of the analyte spike procedure of sections 9.2.1 
through 9.2.3 of this method. Spectra of at least 12 independent spiked 
and 12 independent unspiked samples are recorded. The concentration 
results are analyzed statistically to determine if there is a systematic 
bias in the method for measuring a particular analyte. If there is a 
systematic bias, within the limits allowed by Method 301 of this 
appendix, then a correction factor shall be applied to the analytical 
results. If the systematic bias is greater than the allowed limits, this 
method is not valid and cannot be used.
    9.2.1 Introduce the spike/tracer gas at a constant flow rate of <=10 
percent of the total sample flow, when possible.
    Note: Use the rotameter at the end of the sampling train to estimate 
the required spike/tracer gas flow rate.

    Use a flow device, e.g., mass flow meter ( 2 percent), to 
monitor the spike flow rate. Record the spike flow rate every 10 
minutes.
    9.2.2 Determine the response time (RT) of the system by continuously 
collecting spectra of the spiked effluent until the spectrum of the 
spiked component is constant for 5 minutes. The RT is the interval from 
the

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first measurement until the spike becomes constant. Wait for twice the 
duration of the RT, then collect spectra of two independent spiked gas 
samples. Duplicate analyses of the spiked concentration shall be within 
5 percent of the mean of the two measurements.
    9.2.3 Calculate the dilution ratio using the tracer gas as follows: 
where:
[GRAPHIC] [TIFF OMITTED] TR14JN99.005

Where:

[GRAPHIC] [TIFF OMITTED] TR14JN99.006

DF=Dilution factor of the spike gas; this value shall be =10.
SF6(dir)=SF6 (or tracer gas) concentration 
measured directly in undiluted spike gas.
SF6(spk)=Diluted SF6 (or tracer gas) concentration 
measured in a spiked sample.
Spikedir=Concentration of the analyte in the spike standard 
measured by filling the FTIR cell directly.
CS=Expected concentration of the spiked samples.
Unspike=Native concentration of analytes in unspiked samples.

                  10.0 Calibration and Standardization

    10.1 Signal-to-Noise Ratio (S/N). The RMSD in the noise must be less 
than one tenth of the minimum analyte peak absorbance in each analytical 
region. For example if the minimum peak absorbance is 0.01 at the 
required DL, then RMSD measured over the entire analytical region must 
be <=0.001.
    10.2 Absorbance Path length. Verify the absorbance path length by 
comparing reference CTS spectra to test CTS spectra. See appendix E of 
the FTIR Protocol.
    10.3 Instrument Resolution. Measure the line width of appropriate 
test CTS band(s) to verify instrument resolution. Alternatively, compare 
CTS spectra to a reference CTS spectrum, if available, measured at the 
nominal resolution.
    10.4 Apodization Function.In transforming the sample interferograms 
to absorbance spectra use the same apodization function that was used in 
transforming the reference spectra.
    10.5 FTIR Cell Volume. Evacuate the cell to <=5 mmHg. Measure the 
initial absolute temperature (Ti) and absolute pressure 
(Pi). Connect a wet test meter (or a calibrated dry gas 
meter), and slowly draw room air into the cell. Measure the meter volume 
(Vm), meter absolute temperature (Tm), and meter 
absolute pressure (Pm); and the cell final absolute 
temperature (Tf) and absolute pressure (Pf). 
Calculate the FTIR cell volume VSS, including that of the connecting 
tubing, as follows:
[GRAPHIC] [TIFF OMITTED] TR14JN99.007

                   11.0 Data Analysis and Calculations

    Analyte concentrations shall be measured using reference spectra 
from the EPA FTIR spectral library. When EPA library spectra are not 
available, the procedures in section 4.6 of the Protocol shall be 
followed to prepare reference spectra of all the target analytes.
    11.1 Spectral De-resolution. Reference spectra can be converted to 
lower resolution standard spectra (section 3.3 of this method) by 
truncating the original reference sample and background interferograms. 
Appendix K of the FTIR Protocol gives specific deresolution procedures. 
Deresolved spectra shall be transformed using the same apodization 
function and level of zero filling as the sample spectra. Additionally, 
pre-test FTIR protocol calculations (e.g., FRU, MAU, FCU) shall be 
performed using the de-resolved standard spectra.
    11.2 Data Analysis. Various analytical programs are available for 
relating sample absorbance to a concentration standard. Calculated 
concentrations shall be verified by analyzing residual baselines after 
mathematically subtracting scaled reference spectra from the sample 
spectra. A full description of the data analysis and calculations is 
contained in the FTIR Protocol (sections 4.0, 5.0, 6.0 and appendices). 
Correct the calculated concentrations in the sample spectra for 
differences in absorption path length and temperature between the 
reference and sample spectra using equation 6,
[GRAPHIC] [TIFF OMITTED] TR14JN99.008

Where:

Ccorr=Concentration, corrected for path length.

[[Page 319]]

Ccalc=Concentration, initial calculation (output of the 
analytical program designed for the compound).
Lr=Reference spectra path length.
Ls=Sample spectra path length.
Ts=Absolute temperature of the sample gas, K.
Tr=Absolute gas temperature of reference spectra, K.
Ps=Sample cell pressure.
Pr=Reference spectrum sample pressure.

                         12.0 Method Performance

    12.1 Spectral Quality. Refer to the FTIR Protocol appendices for 
analytical requirements, evaluation of data quality, and analysis of 
uncertainty.
    12.2 Sampling QA/QC. The analyte spike procedure of section 9 of 
this method, the QA spike of section 8.6.2 of this method, and the 
validation procedure of section 13 of this method are used to evaluate 
the performance of the sampling system and to quantify sampling system 
effects, if any, on the measured concentrations. This method is self-
validating provided that the results meet the performance requirement of 
the QA spike in sections 9.0 and 8.6.2 of this method and results from a 
previous method validation study support the use of this method in the 
application. Several factors can contribute to uncertainty in the 
measurement of spiked samples. Factors which can be controlled to 
provide better accuracy in the spiking procedure are listed in sections 
12.2.1 through 12.2.4 of this method.
    12.2.1 Flow meter. An accurate mass flow meter is accurate to 1 percent of its span. If a flow of 1 L/min is monitored 
with such a MFM, which is calibrated in the range of 0-5 L/min, the flow 
measurement has an uncertainty of 5 percent. This may be improved by re-
calibrating the meter at the specific flow rate to be used.
    12.2.2 Calibration gas. Usually the calibration standard is 
certified to within  2 percent. With reactive 
analytes, such as HCl, the certified accuracy in a commercially 
available standard may be no better than  5 
percent.
    12.2.3 Temperature. Temperature measurements of the cell shall be 
quite accurate. If practical, it is preferable to measure sample 
temperature directly, by inserting a thermocouple into the cell chamber 
instead of monitoring the cell outer wall temperature.
    12.2.4 Pressure. Accuracy depends on the accuracy of the barometer, 
but fluctuations in pressure throughout a day may be as much as 2.5 
percent due to weather variations.

                    13.0 Method Validation Procedure

    This validation procedure, which is based on EPA Method 301 (40 CFR 
part 63, appendix (A), may be used to validate this method for the 
analytes in a gas matrix. Validation at one source may also apply to 
another type of source, if it can be shown that the exhaust gas 
characteristics are similar at both sources.
    13.1 Section 5.3 of Method 301 (40 CFR part 63, appendix A), the 
Analyte Spike procedure, is used with these modifications. The 
statistical analysis of the results follows section 6.3 of EPA Method 
301. Section 3 of this method defines terms that are not defined in 
Method 301.
    13.1.1 The analyte spike is performed dynamically. This means the 
spike flow is continuous and constant as spiked samples are measured.
    13.1.2 The spike gas is introduced at the back of the sample probe.
    13.1.3 Spiked effluent is carried through all sampling components 
downstream of the probe.
    13.1.4 A single FTIR system (or more) may be used to collect and 
analyze spectra (not quadruplicate integrated sampling trains).
    13.1.5 All of the validation measurements are performed sequentially 
in a single ``run'' (section 3.26 of this method).
    13.1.6 The measurements analyzed statistically are each independent 
(section 3.22 of this method).
    13.1.7 A validation data set can consist of more than 12 spiked and 
12 unspiked measurements.
    13.2 Batch Sampling. The procedure in sections 13.2.1 through 13.2.2 
may be used for stable processes. If process emissions are highly 
variable, the procedure in section 13.2.3 shall be used.
    13.2.1 With a single FTIR instrument and sampling system, begin by 
collecting spectra of two unspiked samples. Introduce the spike flow 
into the sampling system and allow 10 cell volumes to purge the sampling 
system and FTIR cell. Collect spectra of two spiked samples. Turn off 
the spike and allow 10 cell volumes of unspiked sample to purge the FTIR 
cell. Repeat this procedure until the 24 (or more) samples are 
collected.
    13.2.2 In batch sampling, collect spectra of 24 distinct samples. 
(Each distinct sample consists of filling the cell to ambient pressure 
after the cell has been evacuated.)
    13.2.3 Alternatively, a separate probe assembly, line, and sample 
pump can be used for spiked sample. Verify and document that sampling 
conditions are the same in both the spiked and the unspiked sampling 
systems. This can be done by wrapping both sample lines in the same 
heated bundle. Keep the same flow rate in both sample lines. Measure 
samples in sequence in pairs. After two spiked samples are measured, 
evacuate the FTIR cell, and turn the manifold valve so that spiked 
sample flows to the FTIR cell. Allow the connecting line from the 
manifold to the FTIR cell to purge thoroughly (the

[[Page 320]]

time depends on the line length and flow rate). Collect a pair of spiked 
samples. Repeat the procedure until at least 24 measurements are 
completed.
    13.3 Simultaneous Measurements With Two FTIR Systems. If unspiked 
effluent concentrations of the target analyte(s) vary significantly with 
time, it may be desirable to perform synchronized measurements of spiked 
and unspiked sample. Use two FTIR systems, each with its own cell and 
sampling system to perform simultaneous spiked and unspiked 
measurements. The optical configurations shall be similar, if possible. 
The sampling configurations shall be the same. One sampling system and 
FTIR analyzer shall be used to measure spiked effluent. The other 
sampling system and FTIR analyzer shall be used to measure unspiked flue 
gas. Both systems shall use the same sampling procedure (i.e., batch or 
continuous).
    13.3.1 If batch sampling is used, synchronize the cell evacuation, 
cell filling, and collection of spectra. Fill both cells at the same 
rate (in cell volumes per unit time).
    13.3.2 If continuous sampling is used, adjust the sample flow 
through each gas cell so that the same number of cell volumes pass 
through each cell in a given time (i.e. TC1 = 
TC2).
    13.4 Statistical Treatment. The statistical procedure of EPA Method 
301 of this appendix, section 6.3 is used to evaluate the bias and 
precision. For FTIR testing a validation ``run'' is defined as spectra 
of 24 independent samples, 12 of which are spiked with the analyte(s) 
and 12 of which are not spiked.
    13.4.1 Bias. Determine the bias (defined by EPA Method 301 of this 
appendix, section 6.3.2) using equation 7:
[GRAPHIC] [TIFF OMITTED] TR14JN99.009

Where:

B = Bias at spike level.
Sm = Mean concentration of the analyte spiked samples.
CS = Expected concentration of the spiked samples.

    13.4.2 Correction Factor. Use section 6.3.2.2 of Method 301 of this 
appendix to evaluate the statistical significance of the bias. If it is 
determined that the bias is significant, then use section 6.3.3 of 
Method 301 to calculate a correction factor (CF). Analytical results of 
the test method are multiplied by the correction factor, if 0.7 <= CF <= 
1.3. If is determined that the bias is significant and CF  
 30 percent, then the test method is considered to 
``not valid.''
    13.4.3 If measurements do not pass validation, evaluate the sampling 
system, instrument configuration, and analytical system to determine if 
improper set-up or a malfunction was the cause. If so, repair the system 
and repeat the validation.

                       14.0 Pollution Prevention.

    The extracted sample gas is vented outside the enclosure containing 
the FTIR system and gas manifold after the analysis. In typical method 
applications the vented sample volume is a small fraction of the source 
volumetric flow and its composition is identical to that emitted from 
the source. When analyte spiking is used, spiked pollutants are vented 
with the extracted sample gas. Approximately 1.6 x 10-\4\ to 3.2 x 10-
\4\ lbs of a single HAP may be vented to the atmosphere in a typical 
validation run of 3 hours. (This assumes a molar mass of 50 to 100 g, 
spike rate of 1.0 L/min, and a standard concentration of 100 ppm). 
Minimize emissions by keeping the spike flow off when not in use.

                         15.0 Waste Management.

    Small volumes of laboratory gas standards can be vented through a 
laboratory hood. Neat samples must be packed and disposed according to 
applicable regulations. Surplus materials may be returned to supplier 
for disposal.
    16.0 References.
    1. ``Field Validation Test Using Fourier Transform Infrared (FTIR) 
Spectrometry To Measure Formaldehyde, Phenol and Methanol at a Wool 
Fiberglass Production Facility.'' Draft. U.S. Environmental Protection 
Agency Report, EPA Contract No. 68D20163, Work Assignment I-32, 
September 1994.
    2. ``FTIR Method Validation at a Coal-Fired Boiler''. Prepared for 
U.S. Environmental Protection Agency, Research Triangle Park, NC. 
Publication No.: EPA-454/R95-004, NTIS No.: PB95-193199. July, 1993.
    3. ``Method 301--Field Validation of Pollutant Measurement Methods 
from Various Waste Media,'' 40 CFR part 63, appendix A.
    4. ``Molecular Vibrations; The Theory of Infrared and Raman 
Vibrational Spectra,'' E. Bright Wilson, J. C. Decius, and P. C. Cross, 
Dover Publications, Inc., 1980. For a less intensive treatment of 
molecular rotational-vibrational spectra see, for example, ``Physical 
Chemistry,'' G. M. Barrow, chapters 12, 13, and 14, McGraw Hill, Inc., 
1979.
    5. ``Fourier Transform Infrared Spectrometry,'' Peter R. Griffiths 
and James de Haseth, Chemical Analysis, 83, 16-25,(1986), P. J. Elving, 
J. D. Winefordner and I. M. Kolthoff (ed.), John Wiley and Sons.
    6. ``Computer-Assisted Quantitative Infrared Spectroscopy,'' Gregory 
L. McClure (ed.), ASTM Special Publication 934 (ASTM), 1987.
    7. ``Multivariate Least-Squares Methods Applied to the Quantitative 
Spectral Analysis of Multicomponent Mixtures,'' Applied Spectroscopy, 
39(10), 73-84, 1985.

[[Page 321]]



                             Table 1--Example Presentation of Sampling Documentation
----------------------------------------------------------------------------------------------------------------
                                                        Background file         Sample
           Sample time            Spectrum file name         name            conditioning      Process condition
----------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
----------------------------------------------------------------------------------------------------------------


 
          Sample time               Spectrum file       Interferogram        Resolution        Scans        Apodization        Gain       CTS Spectrum
--------------------------------------------------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
--------------------------------------------------------------------------------------------------------------------------------------------------------

[GRAPHIC] [TIFF OMITTED] TR14JN99.010


[[Page 322]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.011

Addendum to Test Method 320--Protocol for the Use of Extractive Fourier 
   Transform Infrared (FTIR) Spectrometry for the Analyses of Gaseous 
                    Emissions from Stationary Sources

                            1.0 Introduction

    The purpose of this addendum is to set general guidelines for the 
use of modern FTIR spectroscopic methods for the analysis of gas samples 
extracted from the effluent of stationary emission sources. This 
addendum outlines techniques for developing and evaluating such methods 
and sets basic requirements for reporting and quality assurance 
procedures.

                            1.1 Nomenclature

    1.1.1 Appendix A to this addendum lists definitions of the symbols 
and terms used in this Protocol, many of which have been taken directly 
from American Society for Testing and Materials (ASTM) publication E 
131-90a, entitled ``Terminology Relating to Molecular Spectroscopy.''
    1.1.2 Except in the case of background spectra or where otherwise 
noted, the term ``spectrum'' refers to a double-beam spectrum in units 
of absorbance vs. wavenumber (cm-1).
    1.1.3 The term ``Study'' in this addendum refers to a publication 
that has been subjected to EPA- or peer-review.

               2.0 Applicability and Analytical Principle

    2.1 Applicability. This Protocol applies to the determination of 
compound-specific concentrations in single- and multiple-component gas 
phase samples using double-beam absorption spectroscopy in the mid-
infrared band. It does not specifically address other FTIR applications, 
such as single-beam spectroscopy, analysis of open-path (non-enclosed) 
samples, and continuous measurement techniques. If multiple 
spectrometers, absorption cells, or instrumental linewidths are used in 
such analyses, each distinct operational configuration of the system 
must be evaluated separately according to this Protocol.

                        2.2 Analytical Principle

    2.2.1 In the mid-infrared band, most molecules exhibit 
characteristic gas phase absorption spectra that may be recorded by FTIR 
systems. Such systems consist of a source of mid-infrared radiation, an 
interferometer, an enclosed sample cell of known absorption pathlength, 
an infrared detector, optical elements for the transfer of infrared 
radiation between components, and gas flow

[[Page 323]]

control and measurement components. Adjunct and integral computer 
systems are used for controlling the instrument, processing the signal, 
and for performing both Fourier transforms and quantitative analyses of 
spectral data.
    2.2.2 The absorption spectra of pure gases and of mixtures of gases 
are described by a linear absorbance theory referred to as Beer's Law. 
Using this law, modern FTIR systems use computerized analytical programs 
to quantify compounds by comparing the absorption spectra of known 
(reference) gas samples to the absorption spectrum of the sample gas. 
Some standard mathematical techniques used for comparisons are classical 
least squares, inverse least squares, cross-correlation, factor 
analysis, and partial least squares. Reference A describes several of 
these techniques, as well as additional techniques, such as 
differentiation methods, linear baseline corrections, and non-linear 
absorbance corrections.

             3.0 General Principles of Protocol Requirements

    The characteristics that distinguish FTIR systems from gas analyzers 
used in instrumental gas analysis methods (e.g., Methods 6C and 7E of 
appendix A to part 60 of this chapter) are: (1) Computers are necessary 
to obtain and analyze data; (2) chemical concentrations can be 
quantified using previously recorded infrared reference spectra; and (3) 
analytical assumptions and results, including possible effects of 
interfering compounds, can be evaluated after the quantitative analysis. 
The following general principles and requirements of this Protocol are 
based on these characteristics.
    3.1 Verifiability and Reproducibility of Results. Store all data and 
document data analysis techniques sufficient to allow an independent 
agent to reproduce the analytical results from the raw interferometric 
data.
    3.2 Transfer of Reference Spectra. To determine whether reference 
spectra recorded under one set of conditions (e.g., optical bench, 
instrumental linewidth, absorption pathlength, detector performance, 
pressure, and temperature) can be used to analyze sample spectra taken 
under a different set of conditions, quantitatively compare 
``calibration transfer standards'' (CTS) and reference spectra as 
described in this Protocol.
    Note: The CTS may, but need not, include analytes of interest). To 
effect this, record the absorption spectra of the CTS (a) immediately 
before and immediately after recording reference spectra and (b) 
immediately after recording sample spectra.
    3.3 Evaluation of FTIR Analyses. The applicability, accuracy, and 
precision of FTIR measurements are influenced by a number of 
interrelated factors, which may be divided into two classes:
    3.3.1 Sample-Independent Factors. Examples are system configuration 
and performance (e.g., detector sensitivity and infrared source output), 
quality and applicability of reference absorption spectra, and type of 
mathematical analyses of the spectra. These factors define the 
fundamental limitations of FTIR measurements for a given system 
configuration. These limitations may be estimated from evaluations of 
the system before samples are available. For example, the detection 
limit for the absorbing compound under a given set of conditions may be 
estimated from the system noise level and the strength of a particular 
absorption band. Similarly, the accuracy of measurements may be 
estimated from the analysis of the reference spectra.
    3.3.2 Sample-Dependent Factors. Examples are spectral interferants 
(e.g., water vapor and CO2) or the overlap of spectral 
features of different compounds and contamination deposits on reflective 
surfaces or transmitting windows. To maximize the effectiveness of the 
mathematical techniques used in spectral analysis, identification of 
interferants (a standard initial step) and analysis of samples (includes 
effect of other analytical errors) are necessary. Thus, the Protocol 
requires post-analysis calculation of measurement concentration 
uncertainties for the detection of these potential sources of 
measurement error.

                4.0 Pre-Test Preparations and Evaluations

    Before testing, demonstrate the suitability of FTIR spectrometry for 
the desired application according to the procedures of this section.
    4.1 Identify Test Requirements. Identify and record the test 
requirements described in sections 4.1.1 through 4.1.4 of this addendum. 
These values set the desired or required goals of the proposed analysis; 
the description of methods for determining whether these goals are 
actually met during the analysis comprises the majority of this 
Protocol.
    4.1.1 Analytes (specific chemical species) of interest. Label the 
analytes from i = 1 to I.
    4.1.2 Analytical uncertainty limit (AUi). The 
AUi is the maximum permissible fractional uncertainty of 
analysis for the ith analyte concentration, expressed as a 
fraction of the analyte concentration in the sample.
    4.1.3 Required detection limit for each analyte (DLi, 
ppm). The detection limit is the lowest concentration of an analyte for 
which its overall fractional uncertainty (OFUi) is required 
to be less than its analytical uncertainty limit (AUi).
    4.1.4 Maximum expected concentration of each analyte 
(CMAXi, ppm).
    4.2 Identify Potential Interferants. Considering the chemistry of 
the process or results of previous studies, identify potential

[[Page 324]]

interferants, i.e., the major effluent constituents and any relatively 
minor effluent constituents that possess either strong absorption 
characteristics or strong structural similarities to any analyte of 
interest. Label them 1 through Nj, where the subscript ``j'' 
pertains to potential interferants. Estimate the concentrations of these 
compounds in the effluent (CPOTj, ppm).
    4.3 Select and Evaluate the Sampling System. Considering the source, 
e.g., temperature and pressure profiles, moisture content, analyte 
characteristics, and particulate concentration), select the equipment 
for extracting gas samples. Recommended are a particulate filter, 
heating system to maintain sample temperature above the dew point for 
all sample constituents at all points within the sampling system 
(including the filter), and sample conditioning system (e.g., coolers, 
water-permeable membranes that remove water or other compounds from the 
sample, and dilution devices) to remove spectral interferants or to 
protect the sampling and analytical components. Determine the minimum 
absolute sample system pressure (Pmin, mmHg) and the infrared 
absorption cell volume (VSS, liter). Select the techniques 
and/or equipment for the measurement of sample pressures and 
temperatures.
    4.4 Select Spectroscopic System. Select a spectroscopic 
configuration for the application. Approximate the absorption pathlength 
(LS', meter), sample pressure (PS', kPa), absolute 
sample temperature TS', and signal integration period 
(tSS, seconds) for the analysis. Specify the nominal minimum 
instrumental linewidth (MIL) of the system. Verify that the fractional 
error at the approximate values PS' and TS' is 
less than one half the smallest value AUi (see section 4.1.2 
of this addendum).
    4.5 Select Calibration Transfer Standards (CTS's). Select CTS's that 
meet the criteria listed in sections 4.5.1, 4.5.2, and 4.5.3 of this 
addendum.
    Note: It may be necessary to choose preliminary analytical regions 
(see section 4.7 of this addendum), identify the minimum analyte 
linewidths, or estimate the system noise level (see section 4.12 of this 
addendum) before selecting the CTS. More than one compound may be needed 
to meet the criteria; if so, obtain separate cylinders for each 
compound.
    4.5.1 The central wavenumber position of each analytical region 
shall lie within 25 percent of the wavenumber position of at least one 
CTS absorption band.
    4.5.2 The absorption bands in section 4.5.1 of this addendum shall 
exhibit peak absorbances greater than ten times the value 
RMSEST (see section 4.12 of this addendum) but less than 1.5 
absorbance units.
    4.5.3 At least one absorption CTS band within the operating range of 
the FTIR instrument shall have an instrument-independent linewidth no 
greater than the narrowest analyte absorption band. Perform and document 
measurements or cite Studies to determine analyte and CTS compound 
linewidths.
    4.5.4 For each analytical region, specify the upper and lower 
wavenumber positions (FFUm and FFLm, respectively) 
that bracket the CTS absorption band or bands for the associated 
analytical region. Specify the wavenumber range, FNU to FNL, containing 
the absorption band that meets the criterion of section 4.5.3 of this 
addendum.
    4.5.5 Associate, whenever possible, a single set of CTS gas 
cylinders with a set of reference spectra. Replacement CTS gas cylinders 
shall contain the same compounds at concentrations within 5 percent of 
that of the original CTS cylinders; the entire absorption spectra (not 
individual spectral segments) of the replacement gas shall be scaled by 
a factor between 0.95 and 1.05 to match the original CTS spectra.

                      4.6 Prepare Reference Spectra

    Note: Reference spectra are available in a permanent soft copy from 
the EPA spectral library on the EMTIC (Emission Measurement Technical 
Information Center) computer bulletin board; they may be used if 
applicable.
    4.6.1 Select the reference absorption pathlength (LR) of 
the cell.
    4.6.2 Obtain or prepare a set of chemical standards for each 
analyte, potential and known spectral interferants, and CTS. Select the 
concentrations of the chemical standards to correspond to the top of the 
desired range.
    4.6.2.1 Commercially-Prepared Chemical Standards. Chemical standards 
for many compounds may be obtained from independent sources, such as a 
specialty gas manufacturer, chemical company, or commercial laboratory. 
These standards (accurate to within 2 percent) 
shall be prepared according to EPA Traceability Protocol (see Reference 
D) or shall be traceable to NIST standards. Obtain from the supplier an 
estimate of the stability of the analyte concentration. Obtain and 
follow all of the supplier's recommendations for recertifying the 
analyte concentration.
    4.6.2.2 Self-Prepared Chemical Standards. Chemical standards may be 
prepared by diluting certified commercially prepared chemical gases or 
pure analytes with ultra-pure carrier (UPC) grade nitrogen according to 
the barometric and volumetric techniques generally described in 
Reference A, section A4.6.
    4.6.3 Record a set of the absorption spectra of the CTS {R1{time} , 
then a set of the reference spectra at two or more concentrations in 
duplicate over the desired range (the top of the range must be less than 
10 times that of the bottom), followed by a second set

[[Page 325]]

of CTS spectra {R2{time} . (If self-prepared standards are used, see 
section 4.6.5 of this addendum before disposing of any of the 
standards.) The maximum accepted standard concentration-pathlength 
product (ASCPP) for each compound shall be higher than the maximum 
estimated concentration-pathlength products for both analytes and known 
interferants in the effluent gas. For each analyte, the minimum ASCPP 
shall be no greater than ten times the concentration-pathlength product 
of that analyte at its required detection limit.
    4.6.4 Permanently store the background and interferograms in 
digitized form. Document details of the mathematical process for 
generating the spectra from these interferograms. Record the sample 
pressure (PR), sample temperature (TR), reference 
absorption pathlength (LR), and interferogram signal 
integration period (tSR). Signal integration periods for the 
background interferograms shall be =tSR. Values of 
PR, LR, and tSR shall not deviate by 
more than 1 percent from the time of recording 
[R1] to that of recording [R2].
    4.6.5 If self-prepared chemical standards are employed and spectra 
of only two concentrations are recorded for one or more compounds, 
verify the accuracy of the dilution technique by analyzing the prepared 
standards for those compounds with a secondary (non-FTIR) technique in 
accordance with sections 4.6.5.1 through 4.6.5.4 of this addendum.
    4.6.5.1 Record the response of the secondary technique to each of 
the four standards prepared.
    4.6.5.2 Perform a linear regression of the response values 
(dependant variable) versus the accepted standard concentration (ASC) 
values (independent variable), with the regression constrained to pass 
through the zero-response, zero ASC point.
    4.6.5.3 Calculate the average fractional difference between the 
actual response values and the regression-predicted values (those 
calculated from the regression line using the four ASC values as the 
independent variable).
    4.6.5.4 If the average fractional difference value calculated in 
section 4.6.5.3 of this addendum is larger for any compound than the 
corresponding AUi, the dilution technique is not sufficiently 
accurate and the reference spectra prepared are not valid for the 
analysis.
    4.7 Select Analytical Regions. Using the general considerations in 
section 7 of Reference A and the spectral characteristics of the 
analytes and interferants, select the analytical regions for the 
application. Label them m = 1 to M. Specify the lower, center and upper 
wavenumber positions of each analytical region (FLm, 
FCm, and FUm, respectively). Specify the analytes 
and interferants which exhibit absorption in each region.
    4.8 Determine Fractional Reproducibility Uncertainties. Using 
appendix E of this addendum, calculate the fractional reproducibility 
uncertainty for each analyte (FRUi) from a comparison of [R1] 
and [R2]. If FRUi  AUi for any analyte, 
the reference spectra generated in accordance with section 4.6 of this 
addendum are not valid for the application.
    4.9 Identify Known Interferants. Using appendix B of this addendum, 
determine which potential interferants affect the analyte concentration 
determinations. Relabel these potential interferant as ``known'' 
interferants, and designate these compounds from k = 1 to K. Appendix B 
to this addendum also provides criteria for determining whether the 
selected analytical regions are suitable.

              4.10 Prepare Computerized Analytical Programs

    4.10.1 Choose or devise mathematical techniques (e.g, classical 
least squares, inverse least squares, cross-correlation, and factor 
analysis) based on equation 4 of Reference A that are appropriate for 
analyzing spectral data by comparison with reference spectra.
    4.10.2 Following the general recommendations of Reference A, prepare 
a computer program or set of programs that analyzes all of the analytes 
and known interferants, based on the selected analytical regions 
(section 4.7 of this addendum) and the prepared reference spectra 
(section 4.6 of this addendum). Specify the baseline correction 
technique (e.g., determining the slope and intercept of a linear 
baseline contribution in each analytical region) for each analytical 
region, including all relevant wavenumber positions.
    4.10.3 Use programs that provide as output [at the reference 
absorption pathlength (LR), reference gas temperature 
(TR), and reference gas pressure (PR)] the analyte 
concentrations, the known interferant concentrations, and the baseline 
slope and intercept values. If the sample absorption pathlength 
(LS), sample gas temperature (TS), or sample gas 
pressure (PS) during the actual sample analyses differ from 
LR, TR, and PR, use a program or set of 
programs that applies multiplicative corrections to the derived 
concentrations to account for these variations, and that provides as 
output both the corrected and uncorrected values. Include in the report 
of the analysis (see section 7.0 of this addendum) the details of any 
transformations applied to the original reference spectra (e.g., 
differentiation), in such a fashion that all analytical results may be 
verified by an independent agent from the reference spectra and data 
spectra alone.
    4.11 Determine the Fractional Calibration Uncertainty. Calculate the 
fractional calibration uncertainty for each analyte (FCUi) according to 
appendix F of this addendum, and compare these values to the fractional 
uncertainty limits (AUi; see section 4.1.2 of this

[[Page 326]]

addendum). If FCUi AUi, either the 
reference spectra or analytical programs for that analyte are 
unsuitable.
    4.12 Verify System Configuration Suitability. Using appendix C of 
this addendum, measure or obtain estimates of the noise level 
(RMSEST, absorbance) of the FTIR system. Alternatively, 
construct the complete spectrometer system and determine the values 
RMSSm using appendix G of this addendum. Estimate the minimum 
measurement uncertainty for each analyte (MAUi, ppm) and 
known interferant (MIUk, ppm) using appendix D of this 
addendum. Verify that (a) MAUi < 
(AUi)(DLi), FRUi < AUi, and FCUi < 
AUi for each analyte and that (b) the CTS chosen meets the 
requirements listed in sections 4.5.1 through 4.5.5 of this addendum.

                   5.0 Sampling and Analysis Procedure

    5.1 Analysis System Assembly and Leak-Test. Assemble the analysis 
system. Allow sufficient time for all system components to reach the 
desired temperature. Then, determine the leak-rate (LR) and 
leak volume (VL), where VL=LR 
tSS. Leak volumes shall be <=4 percent of VSS.
    5.2 Verify Instrumental Performance. Measure the noise level of the 
system in each analytical region using the procedure of appendix G of 
this addendum. If any noise level is higher than that estimated for the 
system in section 4.12 of this addendum, repeat the calculations of 
appendix D of this addendum and verify that the requirements of section 
4.12 of this addendum are met; if they are not, adjust or repair the 
instrument and repeat this section.

             5.3 Determine the Sample Absorption Pathlength

    Record a background spectrum. Then, fill the absorption cell with 
CTS at the pressure PR and record a set of CTS spectra [R3]. 
Store the background and unscaled CTS single beam interferograms and 
spectra. Using appendix H of this addendum, calculate the sample 
absorption pathlength (LS) for each analytical region. The 
values LS shall not differ from the approximated sample 
pathlength LS' (see section 4.4 of this addendum) by more 
than 5 percent.
    5.4 Record Sample Spectrum. Connect the sample line to the source. 
Either evacuate the absorption cell to an absolute pressure below 5 mmHg 
before extracting a sample from the effluent stream into the absorption 
cell, or pump at least ten cell volumes of sample through the cell 
before obtaining a sample. Record the sample pressure PS. 
Generate the absorbance spectrum of the sample. Store the background and 
sample single beam interferograms, and document the process by which the 
absorbance spectra are generated from these data. (If necessary, apply 
the spectral transformations developed in section 5.6.2 of this 
addendum). The resulting sample spectrum is referred to below as 
SS.

    Note: Multiple sample spectra may be recorded according to the 
procedures of section 5.4 of this addendum before performing sections 
5.5 and 5.6 of this addendum.

    5.5 Quantify Analyte Concentrations. Calculate the unscaled analyte 
concentrations RUAi and unscaled interferant concentrations 
RUIK using the programs developed in section 4 of this 
addendum. To correct for pathlength and pressure variations between the 
reference and sample spectra, calculate the scaling factor, 
RLPS using equation A.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.012

Calculate the final analyte and interferant concentrations 
RSAi and RSIk using equations A.2 and A.3,
[GRAPHIC] [TIFF OMITTED] TR14JN99.013

[GRAPHIC] [TIFF OMITTED] TR14JN99.014

    5.6 Determine Fractional Analysis Uncertainty. Fill the absorption 
cell with CTS at the pressure PS. Record a set of CTS spectra 
[R4]. Store the background and CTS single beam interferograms. Using 
appendix H of this addendum, calculate the fractional analysis 
uncertainty (FAU) for each analytical region. If the FAU indicated for 
any analytical region is greater than the required accuracy requirements 
determined in sections 4.1.1 through 4.1.4 of this addendum, then 
comparisons to previously recorded reference spectra are invalid in that 
analytical region, and the analyst shall perform one or both of the 
procedures of sections 5.6.1 through 5.6.2 of this addendum.
    5.6.1 Perform instrumental checks and adjust the instrument to 
restore its performance to acceptable levels. If adjustments are made, 
repeat sections 5.3, 5.4 (except for the recording of a sample 
spectrum), and 5.5 of this addendum to demonstrate that acceptable 
uncertainties are obtained in all analytical regions.
    5.6.2 Apply appropriate mathematical transformations (e.g., 
frequency shifting, zero-filling, apodization, smoothing) to the spectra 
(or to the interferograms upon which the spectra are based) generated 
during the performance of the procedures of section 5.3 of this 
addendum. Document these transformations and their reproducibility. Do 
not apply multiplicative scaling of the spectra, or any set of 
transformations that is mathematically equivalent to multiplicative 
scaling. Different transformations may be applied to different 
analytical regions. Frequency shifts shall be less than one-half the 
minimum instrumental linewidth, and must be applied to all spectral data 
points in an

[[Page 327]]

analytical region. The mathematical transformations may be retained for 
the analysis if they are also applied to the appropriate analytical 
regions of all sample spectra recorded, and if all original sample 
spectra are digitally stored. Repeat sections 5.3, 5.4 (except the 
recording of a sample spectrum), and 5.5 of this addendum to demonstrate 
that these transformations lead to acceptable calculated concentration 
uncertainties in all analytical regions.

                      6.0 Post-Analysis Evaluations

    Estimate the overall accuracy of the analyses performed in 
accordance with sections 5.1 through 5.6 of this addendum using the 
procedures of sections 6.1 through 6.3 of this addendum.
    6.1 Qualitatively Confirm the Assumed Matrix. Examine each 
analytical region of the sample spectrum for spectral evidence of 
unexpected or unidentified interferants. If found, identify the 
interfering compounds (see Reference C for guidance) and add them to the 
list of known interferants. Repeat the procedures of section 4 of this 
addendum to include the interferants in the uncertainty calculations and 
analysis procedures. Verify that the MAU and FCU values do not increase 
beyond acceptable levels for the application requirements. Re-calculate 
the analyte concentrations (section 5.5 of this addendum) in the 
affected analytical regions.
    6.2 Quantitatively Evaluate Fractional Model Uncertainty (FMU). 
Perform the procedures of either section 6.2.1 or 6.2.2 of this 
addendum:
    6.2.1 Using appendix I of this addendum, determine the fractional 
model error (FMU) for each analyte.
    6.2.2 Provide statistically determined uncertainties FMU for each 
analyte which are equivalent to two standard deviations at the 95 
percent confidence level. Such determinations, if employed, must be 
based on mathematical examinations of the pertinent sample spectra (not 
the reference spectra alone). Include in the report of the analysis (see 
section 7.0 of this addendum) a complete description of the 
determination of the concentration uncertainties.
    6.3 Estimate Overall Concentration Uncertainty (OCU). Using appendix 
J of this addendum, determine the overall concentration uncertainty 
(OCU) for each analyte. If the OCU is larger than the required accuracy 
for any analyte, repeat sections 4 and 6 of this addendum.

                       7.0 Reporting Requirements

[Documentation pertaining to virtually all the procedures of sections 4, 
5, and 6 will be required. Software copies of reference spectra and 
sample spectra will be retained for some minimum time following the 
actual testing.]

                             8.0 References

    (A) Standard Practices for General Techniques of Infrared 
Quantitative Analysis (American Society for Testing and Materials, 
Designation E 168-88).
    (B) The Coblentz Society Specifications for Evaluation of Research 
Quality Analytical Infrared Reference Spectra (Class II); Anal. 
Chemistry 47, 945A (1975); Appl. Spectroscopy 444, pp. 211-215, 1990.
    (C) Standard Practices for General Techniques for Qualitative 
Infrared Analysis, American Society for Testing and Materials, 
Designation E 1252-88.
    (D) ``EPA Traceability Protocol for Assay and Certification of 
Gaseous Calibration Standards,'' U.S. Environmental Protection Agency 
Publication No. EPA/600/R-93/224, December 1993.

 Appendix A to Addendum to Method 320--Definitions of Terms and Symbols

    A.1 Definitions of Terms. All terms used in this method that are not 
defined below have the meaning given to them in the CAA and in subpart A 
of this part.
    Absorption band means a contiguous wavenumber region of a spectrum 
(equivalently, a contiguous set of absorbance spectrum data points) in 
which the absorbance passes through a maximum or a series of maxima.
    Absorption pathlength means the distance in a spectrophotometer, 
measured in the direction of propagation of the beam of radiant energy, 
between the surface of the specimen on which the radiant energy is 
incident and the surface of the specimen from which it is emergent.
    Analytical region means a contiguous wavenumber region 
(equivalently, a contiguous set of absorbance spectrum data points) used 
in the quantitative analysis for one or more analytes.

    Note: The quantitative result for a single analyte may be based on 
data from more than one analytical region.

    Apodization means modification of the ILS function by multiplying 
the interferogram by a weighing function whose magnitude varies with 
retardation.
    Background spectrum means the single beam spectrum obtained with all 
system components without sample present.
    Baseline means any line drawn on an absorption spectrum to establish 
a reference point that represents a function of the radiant power 
incident on a sample at a given wavelength.
    Beers's law means the direct proportionality of the absorbance of a 
compound in a homogeneous sample to its concentration.

[[Page 328]]

    Calibration transfer standard (CTS) gas means a gas standard of a 
compound used to achieve and/or demonstrate suitable quantitative 
agreement between sample spectra and the reference spectra; see section 
4.5.1 of this addendum.
    Compound means a substance possessing a distinct, unique molecular 
structure.
    Concentration (c) means the quantity of a compound contained in a 
unit quantity of sample. The unit ``ppm'' (number, or mole, basis) is 
recommended.
    Concentration-pathlength product means the mathematical product of 
concentration of the species and absorption pathlength. For reference 
spectra, this is a known quantity; for sample spectra, it is the 
quantity directly determined from Beer's law. The units ``centimeters-
ppm'' or ``meters-ppm'' are recommended.
    Derivative absorption spectrum means a plot of rate of change of 
absorbance or of any function of absorbance with respect to wavelength 
or any function of wavelength.
    Double beam spectrum means a transmission or absorbance spectrum 
derived by dividing the sample single beam spectrum by the background 
spectrum.

    Note: The term ``double-beam'' is used elsewhere to denote a 
spectrum in which the sample and background interferograms are collected 
simultaneously along physically distinct absorption paths. Here, the 
term denotes a spectrum in which the sample and background 
interferograms are collected at different times along the same 
absorption path.

    Fast Fourier transform (FFT) means a method of speeding up the 
computation of a discrete FT by factoring the data into sparse matrices 
containing mostly zeros.
    Flyback means interferometer motion during which no data are 
recorded.
    Fourier transform (FT) means the mathematical process for converting 
an amplitude-time spectrum to an amplitude-frequency spectrum, or vice 
versa.
    Fourier transform infrared (FTIR) spectrometer means an analytical 
system that employs a source of mid-infrared radiation, an 
interferometer, an enclosed sample cell of known absorption pathlength, 
an infrared detector, optical elements that transfer infrared radiation 
between components, and a computer system. The time-domain detector 
response (interferogram) is processed by a Fourier transform to yield a 
representation of the detector response vs. infrared frequency.

    Note: When FTIR spectrometers are interfaced with other instruments, 
a slash should be used to denote the interface; e.g., GC/FTIR; HPCL/
FTIR, and the use of FTIR should be explicit; i.e., FTIR not IR.

    Frequency, v means the number of cycles per unit time.
    Infrared means the portion of the electromagnetic spectrum 
containing wavelengths from approximately 0.78 to 800 microns.
    Interferogram, I([sigma]) means record of the modulated component of 
the interference signal measured as a function of retardation by the 
detector.
    Interferometer means device that divides a beam of radiant energy 
into two or more paths, generates an optical path difference between the 
beams, and recombines them in order to produce repetitive interference 
maxima and minima as the optical retardation is varied.
    Linewidth means the full width at half maximum of an absorption band 
in units of wavenumbers (cm-1).
    Mid-infrared means the region of the electromagnetic spectrum from 
approximately 400 to 5000 cm-1.
    Reference spectra means absorption spectra of gases with known 
chemical compositions, recorded at a known absorption pathlength, which 
are used in the quantitative analysis of gas samples.
    Retardation, [sigma] means optical path difference between two beams 
in an interferometer; also known as ``optical path difference'' or 
``optical retardation.''
    Scan means digital representation of the detector output obtained 
during one complete motion of the interferometer's moving assembly or 
assemblies.
    Scaling means application of a multiplicative factor to the 
absorbance values in a spectrum.
    Single beam spectrum means Fourier-transformed interferogram, 
representing the detector response vs. wavenumber.

    Note: The term ``single-beam'' is used elsewhere to denote any 
spectrum in which the sample and background interferograms are recorded 
on the same physical absorption path; such usage differentiates such 
spectra from those generated using interferograms recorded along two 
physically distinct absorption paths (see ``double-beam spectrum'' 
above). Here, the term applies (for example) to the two spectra used 
directly in the calculation of transmission and absorbance spectra of a 
sample.

    Standard reference material means a reference material, the 
composition or properties of which are certified by a recognized 
standardizing agency or group.

    Note: The equivalent ISO term is ``certified reference material.''

    Transmittance, T means the ratio of radiant power transmitted by the 
sample to the radiant power incident on the sample. Estimated in FTIR 
spectroscopy by forming the ratio of the single-beam sample and 
background spectra.
    Wavenumber, v means the number of waves per unit length.


[[Page 329]]


    Note: The usual unit of wavenumber is the reciprocal centimeter, 
cm-1. The wavenumber is the reciprocal of the wavelength, 
[lambda], when [lambda] is expressed in centimeters.

    Zero-filling means the addition of zero-valued points to the end of 
a measured interferogram.

    Note: Performing the FT of a zero-filled interferogram results in 
correctly interpolated points in the computed spectrum.

    A.2 Definitions of Mathematical Symbols. The symbols used in 
equations in this protocol are defined as follows:
    (1) A, absorbance = the logarithm to the base 10 of the reciprocal 
of the transmittance (T).
[GRAPHIC] [TIFF OMITTED] TR14JN99.015

    (2) AAIim = band area of the ith analyte in 
the mth analytical region, at the concentration 
(CLi) corresponding to the product of its required detection 
limit (DLi) and analytical uncertainty limit (AUi) 
.
    (3) AAVim = average absorbance of the ith 
analyte in the mth analytical region, at the concentration 
(CLi) corresponding to the product of its required detection 
limit (DLi) and analytical uncertainty limit 
(AUi).
    (4) ASC, accepted standard concentration = the concentration value 
assigned to a chemical standard.
    (5) ASCPP, accepted standard concentration-pathlength product = for 
a chemical standard, the product of the ASC and the sample absorption 
pathlength. The units ``centimeters-ppm'' or ``meters-ppm'' are 
recommended.
    (6) AUi, analytical uncertainty limit = the maximum 
permissible fractional uncertainty of analysis for the ith 
analyte concentration, expressed as a fraction of the analyte 
concentration determined in the analysis.
    (7) AVTm = average estimated total absorbance in the 
mth analytical region.
    (8) CKWNk = estimated concentration of the kth 
known interferant.
    (9) CMAXi = estimated maximum concentration of the 
ith analyte.
    (10) CPOTj = estimated concentration of the 
jth potential interferant.
    (11) DLi, required detection limit = for the 
ith analyte, the lowest concentration of the analyte for 
which its overall fractional uncertainty (OFUi) is required 
to be less than the analytical uncertainty limit (AUi).
    (12) FCm = center wavenumber position of the 
mth analytical region.
    (13) FAUi, fractional analytical uncertainty = calculated 
uncertainty in the measured concentration of the ith analyte 
because of errors in the mathematical comparison of reference and sample 
spectra.
    (14) FCUi, fractional calibration uncertainty = 
calculated uncertainty in the measured concentration of the 
ith analyte because of errors in Beer's law modeling of the 
reference spectra concentrations.
    (15) FFLm = lower wavenumber position of the CTS 
absorption band associated with the mth analytical region.
    (16) FFUm = upper wavenumber position of the CTS 
absorption band associated with the mth analytical region.
    (17) FLm = lower wavenumber position of the 
mth analytical region.
    (18) FMUi, fractional model uncertainty = calculated 
uncertainty in the measured concentration of the ith analyte 
because of errors in the absorption model employed.
    (19) FNL = lower wavenumber position of the CTS spectrum 
containing an absorption band at least as narrow as the analyte 
absorption bands.
    (20) FNU = upper wavenumber position of the CTS spectrum 
containing an absorption band at least as narrow as the analyte 
absorption bands.
    (21) FRUi, fractional reproducibility uncertainty = 
calculated uncertainty in the measured concentration of the 
ith analyte because of errors in the reproducibility of 
spectra from the FTIR system.
    (22) FUm = upper wavenumber position of the 
mth analytical region.
    (23) IAIjm = band area of the jth potential 
interferant in the mth analytical region, at its expected 
concentration (CPOTj).
    (24) IAVim = average absorbance of the ith 
analyte in the mth analytical region, at its expected 
concentration (CPOTj).
    (25) ISCi or k, indicated standard concentration = the 
concentration from the computerized analytical program for a single-
compound reference spectrum for the ith analyte or 
kth known interferant.
    (26) kPa = kilo-Pascal (see Pascal).
    (27) LS' = estimated sample absorption pathlength.
    (28) LR = reference absorption pathlength.
    (29) LS = actual sample absorption pathlength.
    (30) MAUi = mean of the MAUim over the 
appropriate analytical regions.
    (31) MAUim, minimum analyte uncertainty = the calculated 
minimum concentration for which the analytical uncertainty limit 
(AUi) in the measurement of the ith analyte, based 
on spectral data in the mth analytical region, can be 
maintained.
    (32) MIUj = mean of the MIUjm over the 
appropriate analytical regions.
    (33) MIUjm, minimum interferant uncertainty = the 
calculated minimum concentration for which the analytical uncertainty 
limit CPOTj/20 in the measurement of the jth 
interferant, based on spectral data in the mth analytical 
region, can be maintained.
    (34) MIL, minimum instrumental linewidth = the minimum linewidth 
from the FTIR system, in wavenumbers.


[[Page 330]]


    Note: The MIL of a system may be determined by observing an 
absorption band known (through higher resolution examinations) to be 
narrower than indicated by the system. The MIL is fundamentally limited 
by the retardation of the interferometer, but is also affected by other 
operational parameters (e.g., the choice of apodization).

    (35) Ni = number of analytes.
    (36) Nj = number of potential interferants.
    (37) Nk = number of known interferants.
    (38) Nscan = the number of scans averaged to obtain an 
interferogram.
    (39) OFUi = the overall fractional uncertainty in an 
analyte concentration determined in the analysis (OFUi = 
MAX[FRUi, FCUi, FAUi, 
FMUi]).
    (40) Pascal (Pa) = metric unit of static pressure, equal to one 
Newton per square meter; one atmosphere is equal to 101,325 Pa; 1/760 
atmosphere (one Torr, or one millimeter Hg) is equal to 133.322 Pa.
    (41) Pmin = minimum pressure of the sampling system 
during the sampling procedure.
    (42) PS' = estimated sample pressure.
    (43) PR = reference pressure.
    (44) PS = actual sample pressure.
    (45) RMSSm = measured noise level of the FTIR system in 
the mth analytical region.
    (46) RMSD, root mean square difference = a measure of accuracy 
determined by the following equation:
[GRAPHIC] [TIFF OMITTED] TR14JN99.016

Where:

n = the number of observations for which the accuracy is determined.
ei = the difference between a measured value of a property 
and its mean value over the n observations.

    Note: The RMSD value ``between a set of n contiguous absorbance 
values (Ai) and the mean of the values'' (AM) is 
defined as
[GRAPHIC] [TIFF OMITTED] TR14JN99.017

    (47) RSAi = the (calculated) final concentration of the 
ith analyte.
    (48) RSIk = the (calculated) final concentration of the 
kth known interferant.
    (49) tscan, scan time = time used to acquire a single 
scan, not including flyback.
    (50) tS, signal integration period = the period of time 
over which an interferogram is averaged by addition and scaling of 
individual scans. In terms of the number of scans Nscan and 
scan time tscan, tS = 
Nscantscan.
    (51) tSR = signal integration period used in recording 
reference spectra.
    (52) tSS = signal integration period used in recording 
sample spectra.
    (53) TR = absolute temperature of gases used in recording 
reference spectra.
    (54) TS = absolute temperature of sample gas as sample 
spectra are recorded.
    (55) TP, Throughput = manufacturer's estimate of the fraction of the 
total infrared power transmitted by the absorption cell and transfer 
optics from the interferometer to the detector.
    (56) VSS = volume of the infrared absorption cell, 
including parts of attached tubing.
    (57) Wik = weight used to average over analytical regions 
k for quantities related to the analyte i; see appendix D of this 
addendum.

 Appendix B to Addendum to Method 320--Identifying Spectral Interferants

                               B.1 General

    B.1.1 Assume a fixed absorption pathlength equal to the value 
LS'.
    B.1.2 Use band area calculations to compare the relative absorption 
strengths of the analytes and potential interferants. In the 
mth analytical region (FLm to FUm), use 
either rectangular or trapezoidal approximations to determine the band 
areas described below (see Reference A, sections A.3.1 through A.3.3). 
Document any baseline corrections applied to the spectra.
    B.1.3 Use the average total absorbance of the analytes and potential 
interferants in each analytical region to determine whether the 
analytical region is suitable for analyte concentration determinations.

    Note: The average absorbance in an analytical region is the band 
area divided by the width of the analytical region in wavenumbers. The 
average total absorbance in an analytical region is the sum of the 
average absorbances of all analytes and potential interferants.

                            B.2 Calculations

    B.2.1 Prepare spectral representations of each analyte at the 
concentration CLi = (DLi)(AUi), where 
DLi is the required detection limit and AUi is the 
maximum permissible analytical uncertainty. For the mth 
analytical region, calculate the band area (AAIim) and 
average absorbance (AAVim) from these scaled analyte spectra.
    B.2.2 Prepare spectral representations of each potential interferant 
at its expected concentration (CPOTj). For the mth 
analytical region, calculate the band area (IAIjm) and 
average absorbance (IAVjm) from these scaled potential 
interferant spectra.
    B.2.3 Repeat the calculation for each analytical region, and record 
the band area results in matrix form as indicated in Figure B.1.
    B.2.4 If the band area of any potential interferant in an analytical 
region is greater than the one-half the band area of any analyte (i.e., 
IAIjm  0.5 AAIim for any pair ij

[[Page 331]]

and any m), classify the potential interferant as a known interferant. 
Label the known interferants k = 1 to K. Record the results in matrix 
form as indicated in Figure B.2.
    B.2.5 Calculate the average total absorbance (AVTm) for 
each analytical region and record the values in the last row of the 
matrix described in Figure B.2. Any analytical region where 
AVTm  2.0 is unsuitable.

[[Page 332]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.018


[[Page 333]]



      Appendix C to Addendum to Method 320--Estimating Noise Levels

                               C.1 General

    C.1.1 The root-mean-square (RMS) noise level is the standard measure 
of noise in this addendum. The RMS noise level of a contiguous segment 
of a spectrum is defined as the RMS difference (RMSD) between the 
absorbance values which form the segment and the mean value of that 
segment (see appendix A of this addendum).
    C.1.2 The RMS noise value in double-beam absorbance spectra is 
assumed to be inversely proportional to: (a) the square root of the 
signal integration period of the sample single beam spectra from which 
it is formed, and (b) the total infrared power transmitted through the 
interferometer and absorption cell.
    C.1.3 Practically, the assumption of C.1.2 allows the RMS noise 
level of a complete system to be estimated from the quantities described 
in sections C.1.3.1 through C.1.3.4:
    C.1.3.1 RMSMAN, the noise level of the system (in 
absorbance units), without the absorption cell and transfer optics, 
under those conditions necessary to yield the specified minimum 
instrumental linewidth, e.g., Jacquinot stop size.
    C.1.3.2 tMAN, the manufacturer's signal integration time 
used to determine RMSMAN.
    C.1.3.3 tSS, the signal integration time for the 
analyses.
    C.1.3.4 TP, the manufacturer's estimate of the fraction of the total 
infrared power transmitted by the absorption cell and transfer optics 
from the interferometer to the detector.

                            C.2 Calculations

    C.2.1 Obtain the values of RMSMAN, tMAN, and 
TP from the manufacturers of the equipment, or determine the noise level 
by direct measurements with the completely constructed system proposed 
in section 4 of this addendum.
    C.2.2 Calculate the noise value of the system (RMSEST) 
using equation C.1.
[GRAPHIC] [TIFF OMITTED] TR14JN99.019

 Appendix D to Addendum to Method 320--Estimating Minimum Concentration 
                 Measurement Uncertainties (MAU and MIU)

                               D.1 General

    Estimate the minimum concentration measurement uncertainties for the 
ith analyte (MAUi) and jth interferant 
(MIUj) based on the spectral data in the mth 
analytical region by comparing the analyte band area in the analytical 
region (AAIim) and estimating or measuring the noise level of 
the system (RMSEST or RMSSM).

    Note: For a single analytical region, the MAU or MIU value is the 
concentration of the analyte or interferant for which the band area is 
equal to the product of the analytical region width (in wavenumbers) and 
the noise level of the system (in absorbance units). If data from more 
than one analytical region are used in the determination of an analyte 
concentration, the MAU or MIU is the mean of the separate MAU or MIU 
values calculated for each analytical region.

                            D.2 Calculations

    D.2.1 For each analytical region, set RMS = RMSSM if 
measured (appendix G of this addendum), or set RMS = RMSEST 
if estimated (appendix C of this addendum).
    D.2.2 For each analyte associated with the analytical region, 
calculate MAUim using equation D.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.020

    D.2.3 If only the mth analytical region is used to 
calculate the concentration of the ith analyte, set 
MAUi = MAUim.
    D.2.4 If more than one analytical region is used to calculate the 
concentration of the ith analyte, set MAUi equal 
to the weighted mean of the appropriate MAUim values 
calculated above; the weight for each term in the mean is equal to the 
fraction of the total wavenumber range used for the calculation

[[Page 334]]

represented by each analytical region. Mathematically, if the set of 
analytical regions employed is [m'], then the MAU for each analytical 
region is given by equation D.2.
[GRAPHIC] [TIFF OMITTED] TR14JN99.021

where the weight Wik is defined for each term in the sum as
[GRAPHIC] [TIFF OMITTED] TR14JN99.022

    D.2.5 Repeat sections D.2.1 through D.2.4 of this appendix to 
calculate the analogous values MIUj for the interferants j = 
1 to J. Replace the value (AUi) (DLi) in equation 
D.1 with CPOTj/20; replace the value AAIim in 
equation D.1 with IAIjm.

      Appendix E to Addendum to Method 320--Determining Fractional 
                   Reproducibility Uncertainties (FRU)

                               E.1 General

    To estimate the reproducibility of the spectroscopic results of the 
system, compare the CTS spectra recorded before and after preparing the 
reference spectra. Compare the difference between the spectra to their 
average band area. Perform the calculation for each analytical region on 
the portions of the CTS spectra associated with that analytical region.

                            E.2 Calculations

    E.2.1 The CTS spectra {R1{time}  consist of N spectra, denoted by 
S1i, i=1, N. Similarly, the CTS spectra {R2{time}  consist of 
N spectra, denoted by S2i, i=1, N. Each Ski is the 
spectrum of a single compound, where i denotes the compound and k 
denotes the set {{time}  of which Ski is a member. Form the 
spectra S3 according to S3i = S2i-
S1i for each i. Form the spectra S4 according to 
S4i = [S2i+S1i]/2 for each i.
    E.2.2 Each analytical region m is associated with a portion of the 
CTS spectra S2i and S1i, for a particular i, with 
lower and upper wavenumber limits FFLm and FFUm, 
respectively.
    E.2.3 For each m and the associated i, calculate the band area of 
S4i in the wavenumber range FFUm to 
FFLm. Follow the guidelines of section B.1.2 of this addendum 
for this band area calculation. Denote the result by BAVm.
    E.2.4 For each m and the associated i, calculate the RMSD of 
S3i between the absorbance values and their mean in the 
wavenumber range FFUm to FFLm. Denote the result 
by SRMSm.
    E.2.5 For each analytical region m, calculate FMm using 
equation E.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.023

    E.2.6 If only the mth analytical region is used to 
calculate the concentration of the ith analyte, set 
FRUi = FMm.
    E.2.7 If a number pi of analytical regions are used to 
calculate the concentration of the ith analyte, set 
FRUi equal to the weighted mean of the appropriate 
FMm values calculated according to section E.2.5. 
Mathematically, if the set of analytical regions employed is {m'{time} , 
then FRUi is given by equation E.2,
[GRAPHIC] [TIFF OMITTED] TR14JN99.024

where the Wik are calculated as described in appendix D of 
this addendum.

Appendix F of Addendum to Method 320--Determining Fractional Calibration 
                           Uncertainties (FCU)

                               F.1 General

    F.1.1 The concentrations yielded by the computerized analytical 
program applied to each single-compound reference spectrum are defined 
as the indicated standard concentrations (ISC's). The ISC values for a 
single compound spectrum should ideally equal the accepted standard 
concentration (ASC) for one analyte or interferant, and should ideally 
be zero for all other compounds. Variations from these results are 
caused by errors in the ASC values, variations from the Beer's law (or 
modified Beer's law) model used to determine the concentrations, and

[[Page 335]]

noise in the spectra. When the first two effects dominate, the 
systematic nature of the errors is often apparent and the analyst shall 
take steps to correct them.
    F.1.2 When the calibration error appears non-systematic, apply the 
procedures of sections F.2.1 through F.2.3 of this appendix to estimate 
the fractional calibration uncertainty (FCU) for each compound. The FCU 
is defined as the mean fractional error between the ASC and the ISC for 
all reference spectra with non-zero ASC for that compound. The FCU for 
each compound shall be less than the required fractional uncertainty 
specified in section 4.1 of this addendum.
    F.1.3 The computerized analytical programs shall also be required to 
yield acceptably low concentrations for compounds with ISC = 0 when 
applied to the reference spectra. The ISC of each reference spectrum for 
each analyte or interferant shall not exceed that compound's minimum 
measurement uncertainty (MAU or MIU).

                            F.2 Calculations

    F.2.1 Apply each analytical program to each reference spectrum. 
Prepare a similar table to that in Figure F.1 to present the ISC and ASC 
values for each analyte and interferant in each reference spectrum. 
Maintain the order of reference file names and compounds employed in 
preparing Figure F.1.
    F.2.2 For all reference spectra in Figure F.1, verify that the 
absolute values of the ISC's are less than the compound's MAU (for 
analytes) or MIU (for interferants).
    F.2.3 For each analyte reference spectrum, calculate the quantity 
(ASC-ISC)/ASC. For each analyte, calculate the mean of these values (the 
FCUi for the ith analyte) over all reference 
spectra. Prepare a similar table to that in Figure F.2 to present the 
FCUi and analytical uncertainty limit (AUi) for 
each analyte.

                                       Figure F.1--Presentation of Accepted Standard Concentrations (ASC's) and Indicated Standard Concentrations (ISC's)
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
 
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
          Compound name           Reference spectrum       ASC (ppm)                                                             ISC (ppm)
                                       file name
                                                                                                                           Analytes Interferants
                                                                                                                                   i=1 I
                                                                                                                                   j=1 J
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------


  Figure F.2--Presentation of Fractional Calibration Uncertainties (FCU's) and Analytical Uncertainties (AU's)
----------------------------------------------------------------------------------------------------------------
                  Analyte name                                FCU (%)                         AU (%)
----------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
----------------------------------------------------------------------------------------------------------------

      Appendix G to Addendum to Method 320--Measuring Noise Levels

                               G.1 General

    The root-mean-square (RMS) noise level is the standard measure of 
noise. The RMS noise level of a contiguous segment of a spectrum is the 
RMSD between the absorbance values that form the segment and the mean 
value of the segment (see appendix A of this addendum).

                            G.2 Calculations

    G.2.1 Evacuate the absorption cell or fill it with UPC grade 
nitrogen at approximately one atmosphere total pressure.
    G.2.2 Record two single beam spectra of signal integration period 
tSS.
    G.2.3 Form the double beam absorption spectrum from these two single 
beam spectra, and calculate the noise level RMSSm in the M 
analytical regions.

[[Page 336]]

  Appendix H of Addendum to Method 320--Determining Sample Absorption 
 Pathlength (LS) and Fractional Analytical Uncertainty (FAU)

                               H.1 General

    Reference spectra recorded at absorption pathlength (LR), 
gas pressure (PR), and gas absolute temperature 
(TR) may be used to determine analyte concentrations in 
samples whose spectra are recorded at conditions different from that of 
the reference spectra, i.e., at absorption pathlength (LS), 
absolute temperature (TS), and pressure (PS). This 
appendix describes the calculations for estimating the fractional 
uncertainty (FAU) of this practice. It also describes the calculations 
for determining the sample absorption pathlength from comparison of CTS 
spectra, and for preparing spectra for further instrumental and 
procedural checks.
    H.1.1 Before sampling, determine the sample absorption pathlength 
using least squares analysis. Determine the ratio LS/
LR by comparing the spectral sets {R1{time}  and {R3{time} , 
which are recorded using the same CTS at LS and 
LR, and TS and TR, but both at 
PR.
    H.1.2 Determine the fractional analysis uncertainty (FAU) for each 
analyte by comparing a scaled CTS spectral set, recorded at 
LS, TS, and PS, to the CTS reference 
spectra of the same gas, recorded at LR, TR, and 
PR. Perform the quantitative comparison after recording the 
sample spectra, based on band areas of the spectra in the CTS absorbance 
band associated with each analyte.

                            H.2 Calculations

    H.2.1 Absorption Pathlength Determination. Perform and document 
separate linear baseline corrections to each analytical region in the 
spectral sets {R1{time}  and {R3{time} . Form a one-dimensional array 
AR containing the absorbance values from all segments of 
{R1{time}  that are associated with the analytical regions; the members 
of the array are ARi, i = 1, n. Form a similar one-
dimensional array AS from the absorbance values in the 
spectral set {R3{time} ; the members of the array are ASi, i 
= 1, n. Based on the model AS = rAR + E, determine 
the least-squares estimate of r, the value of r which minimizes the 
square error E2. Calculate the sample absorption pathlength, 
LS, using equation H.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.025

    H.2.2 Fractional Analysis Uncertainty. Perform and document separate 
linear baseline corrections to each analytical region in the spectral 
sets {R1{time}  and {R4{time} . Form the arrays AS and 
AR as described in section H.2.1 of this appendix, using 
values from {R1{time}  to form AR, and values from {R4{time}  
to form AS. Calculate NRMSE and IAAV 
using equations H.2 and H.3,
[GRAPHIC] [TIFF OMITTED] TR14JN99.026

[GRAPHIC] [TIFF OMITTED] TR14JN99.027

    The fractional analytical uncertainty, FAU, is given by equation 
H.4,
[GRAPHIC] [TIFF OMITTED] TR14JN99.028

   Appendix I to Addendum to Method 320--Determining Fractional Model 
                           Uncertainties (FMU)

                               I.1 General

    To prepare analytical programs for FTIR analyses, the sample 
constituents must first be assumed. The calculations in this appendix, 
based upon a simulation of the sample spectrum, shall be used to verify 
the appropriateness of these assumptions. The simulated spectra consist 
of the sum of single compound reference spectra scaled to represent 
their contributions to the sample absorbance spectrum; scaling factors 
are based on the indicated standard concentrations (ISC) and measured 
(sample) analyte and interferant concentrations, the sample and 
reference absorption pathlengths, and the sample and reference gas 
pressures. No band-shape correction for differences in the temperature 
of the sample and reference spectra gases is made; such errors are 
included in the FMU estimate. The actual and simulated sample spectra 
are quantitatively compared to determine the fractional model 
uncertainty; this comparison uses the reference

[[Page 337]]

spectra band areas and residuals in the difference spectrum formed from 
the actual and simulated sample spectra.

                            I.2 Calculations

    I.2.1 For each analyte (with scaled concentration RSAi), 
select a reference spectrum SAi with indicated standard 
concentration ISCi. Calculate the scaling factors, 
RAi, using equation I.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.029

Form the spectra SACi by scaling each SAi by the 
factor RAi.
    I.2.2 For each interferant, select a reference spectrum 
SIk with indicated standard concentration ISCk. 
Calculate the scaling factors, RIk, using equation I.2,
[GRAPHIC] [TIFF OMITTED] TR14JN99.030

Form the spectra SICk by scaling each SIk by the 
factor RIk.
    I.2.3 For each analytical region, determine by visual inspection 
which of the spectra SACi and SICk exhibit 
absorbance bands within the analytical region. Subtract each spectrum 
SACi and SICk exhibiting absorbance from the 
sample spectrum SS to form the spectrum SUBS. To 
save analysis time and to avoid the introduction of unwanted noise into 
the subtracted spectrum, it is recommended that the calculation be made 
(1) only for those spectral data points within the analytical regions, 
and (2) for each analytical region separately using the original 
spectrum SS.
    I.2.4 For each analytical region m, calculate the RMSD of 
SUBS between the absorbance values and their mean in the 
region FFUm to FFLm. Denote the result by 
RMSSm.
    I.2.5 For each analyte i, calculate FMm, using equation 
I.3,
[GRAPHIC] [TIFF OMITTED] TR14JN99.031

for each analytical region associated with the analyte.
    I.2.6 If only the mth analytical region is used to 
calculate the concentration of the ith analyte, set 
FMUi=FMm.
    I.2.7 If a number of analytical regions are used to calculate the 
concentration of the ith analyte, set FMi equal to 
the weighted mean of the appropriate FMm values calculated 
using equation I-3. Mathematically, if the set of analytical regions 
employed is {m'{time} , then the fractional model uncertainty, FMU, is 
given by equation I.4,
[GRAPHIC] [TIFF OMITTED] TR14JN99.032

where Wik is calculated as described in appendix D of this 
addendum.

Appendix J of Addendum to Method 320--Determining Overall Concentration 
                           Uncertainties (OCU)

    The calculations in this addendum estimate the measurement 
uncertainties for various FTIR measurements. The lowest possible overall 
concentration uncertainty (OCU) for an analyte is its MAU value, which 
is an estimate of the absolute concentration uncertainty when spectral 
noise dominates the measurement error. However, if the product of the 
largest fractional concentration uncertainty (FRU, FCU, FAU, or FMU) and 
the measured concentration of an analyte exceeds the MAU for the 
analyte, then the OCU is this product. In mathematical terms, set 
OFUi = MAX{FRUi, FCUi, FAUi, 
FMUi{time}  and OCUi = 
MAX{RSAi*OFUi, MAUi{time} .

 Test Method 321--Measurement of Gaseous Hydrogen Chloride Emissions At 
 Portland Cement Kilns by Fourier Transform Infrared (FTIR) Spectroscopy

                            1.0 Introduction

    This method should be performed by those persons familiar with the 
operation of Fourier Transform Infrared (FTIR) instrumentation in the 
application to source sampling. This document describes the sampling 
procedures for use in the application of FTIR spectrometry for the 
determination of vapor phase hydrogen chloride (HCl) concentrations both 
before and after particulate matter control devices installed at 
portland cement kilns. A procedure for analyte spiking is included for 
quality assurance. This method is considered to be self validating 
provided that the requirements listed in section 9 of this method are 
followed. The analytical procedures for interpreting infrared spectra 
from emission measurements are described in the ``Protocol For The Use 
of Extractive

[[Page 338]]

Fourier Transform Infrared (FTIR) Spectrometry in Analyses of Gaseous 
Emissions From Stationary Industrial Sources'', included as an addendum 
to proposed Method 320 of this appendix (hereafter referred to as the 
``FTIR Protocol)''. References 1 and 2 describe the use of FTIR 
spectrometry in field measurements. Sample transport presents the 
principal difficulty in directly measuring HCl emissions. This identical 
problem must be overcome by any extractive measurement method. HCl is 
reactive and water soluble. The sampling system must be adequately 
designed to prevent sample condensation in the system.

                        1.1 Scope and Application

    This method is specifically designed for the application of FTIR 
Spectrometry in extractive measurements of gaseous HCl concentrations in 
portland cement kiln emissions.

                            1.2 Applicability

    This method applies to the measurement of HCl [CAS No. 7647-01-0]. 
This method can be applied to the determination of HCl concentrations 
both before and after particulate matter control devices installed at 
portland cement manufacturing facilities. This method applies to either 
continuous flow through measurement (with isolated sample analysis) or 
grab sampling (batch analysis). HCl is measured using the mid-infrared 
spectral region for analysis (about 400 to 4000 cm-1 or 25 to 
2.5 [mu]m). Table 1 lists the suggested analytical region for 
quantification of HCl taking the interference from water vapor into 
consideration.

               Table 1--Example Analytical Region for HCl
------------------------------------------------------------------------
                                    Analytical           Potential
           Compound               region  (cm-1)        interferants
------------------------------------------------------------------------
Hydrogen chloride.............          2679-2840  Water.
------------------------------------------------------------------------

                    1.3 Method Range and Sensitivity

    1.3.1 The analytical range is determined by the instrumental design 
and the composition of the gas stream. For practical purposes there is 
no upper limit to the range because the pathlength may be reduced or the 
sample may be diluted. The lower detection range depends on (1) the 
absorption coefficient of the compound in the analytical frequency 
region, (2) the spectral resolution, (3) the interferometer sampling 
time, (4) the detector sensitivity and response, and (5) the absorption 
pathlength.
    1.3.2 The practical lower quantification range is usually higher 
than the instrument sensitivity allows and is dependent upon (1) the 
presence of interfering species in the exhaust gas including 
H2O, CO2, and SO2, (2) analyte losses 
in the sampling system, (3) the optical alignment of the gas cell and 
transfer optics, and (4) the quality of the reflective surfaces in the 
cell (cell throughput). Under typical test conditions (moisture content 
of up to 30% and CO2 concentrations from 1 to 15 percent), a 
22 meter path length cell with a suitable sampling system may achieve a 
lower quantification range of from 1 to 5 ppm for HCl.

                       1.4 Data Quality Objectives

    1.4.1 In designing or configuring the analytical system, data 
quality is determined by measuring of the root mean square deviation 
(RMSD) of the absorbance values within a chosen spectral (analytical) 
region. The RMSD provides an indication of the signal-to-noise ratio (S/
N) of the spectral baseline. Appendix D of the FTIR Protocol (the 
addendum to Method 320 of this appendix) presents a discussion of the 
relationship between the RMSD, lower detection limit, DLi, 
and analytical uncertainty, AUi. It is important to consider 
the target analyte quantification limit when performing testing with 
FTIR instrumentation, and to optimize the system to achieve the desired 
detection limit.
    1.4.2 Data quality is determined by measuring the root mean square 
(RMS) noise level in each analytical spectral region (appendix C of the 
FTIR Protocol). The RMS noise is defined as the root mean square 
deviation (RMSD) of the absorbance values in an analytical region from 
the mean absorbance value in the same region. Appendix D of the FTIR 
Protocol defines the minimum analyte uncertainty (MAU), and how the RMSD 
is used to calculate the MAU. The MAUim is the minimum 
concentration of the ith analyte in the mth analytical region for which 
the analytical uncertainty limit can be maintained. Table 2 presents 
example values of AU and MAU using the analytical region presented in 
Table 1.

  Table 2--Example Pre-Test Protocol Calculations for Hydrogen Chloride
------------------------------------------------------------------------
                                                                 HCl
------------------------------------------------------------------------
Reference concentration (ppm-meters)/K.....................         11.2
Reference Band area........................................        2.881
DL (ppm-meters)/K..........................................       0.1117
AU.........................................................          0.2
CL (DL x AU)...............................................      0.02234

[[Page 339]]

 
FL (cm-1)..................................................      2679.83
FU (cm-1)..................................................      2840.93
FC (cm-1)..................................................      2760.38
AAI (ppm-meters)/K.........................................      0.06435
RMSD.......................................................     2.28E-03
MAU (ppm-meters)/K.........................................     1.28E-01
MAU ppm at 22 meters and 250 [deg]F........................      .0.2284
------------------------------------------------------------------------

                          2.0 Summary of Method

                              2.1 Principle

    See Method 320 of this appendix. HCl can also undergo rotation 
transitions by absorbing energy in the far-infrared spectral region. The 
rotational transitions are superimposed on the vibrational fundamental 
to give a series of lines centered at the fundamental vibrational 
frequency, 2885 cm-\1\. The frequencies of absorbance and the pattern of 
rotational/vibrational lines are unique to HCl. When this distinct 
pattern is observed in an infrared spectrum of an unknown sample, it 
unequivocally identifies HCl as a component of the mixture. The infrared 
spectrum of HCl is very distinctive and cannot be confused with the 
spectrum of any other compound. See Reference 6.
    2.2 Sampling and Analysis. See Method 320 of this appendix.
    2.3 Operator Requirements. The analyst must have knowledge of 
spectral patterns to choose an appropriate absorption path length or 
determine if sample dilution is necessary. The analyst should also 
understand FTIR instrument operation well enough to choose instrument 
settings that are consistent with the objectives of the analysis.

                             3.0 Definitions

    See appendix A of the FTIR Protocol.

                            4.0 Interferences

    This method will not measure HCl under conditions: (1) where the 
sample gas stream can condense in the sampling system or the 
instrumentation, or (2) where a high moisture content sample relative to 
the analyte concentrations imparts spectral interference due to the 
water vapor absorbance bands. For measuring HCl the first (sampling) 
consideration is more critical. Spectral interference from water vapor 
is not a significant problem except at very high moisture levels and low 
HCl concentrations.
    4.1 Analytical Interferences. See Method 320 of this appendix.
    4.1.1 Background Interferences. See Method 320 of this appendix.
    4.1.2 Spectral interferences. Water vapor can present spectral 
interference for FTIR gas analysis of HCl. Therefore, the water vapor in 
the spectra of kiln gas samples must be accounted for. This means 
preparing at least one spectrum of a water vapor sample where the 
moisture concentration is close to that in the kiln gas.
    4.2 Sampling System Interferences. The principal sampling system 
interferant for measuring HCl is water vapor. Steps must be taken to 
ensure that no condensation forms anywhere in the probe assembly, sample 
lines, or analytical instrumentation. Cold spots anywhere in the 
sampling system must be avoided. The extent of sampling system bias in 
the FTIR analysis of HCl depends on concentrations of potential 
interferants, moisture content of the gas stream, temperature of the gas 
stream, temperature of sampling system components, sample flow rate, and 
reactivity of HCl with other species in the gas stream (e.g., ammonia). 
For measuring HCl in a wet gas stream the temperatures of the gas 
stream, sampling components, and the sample flow rate are of primary 
importance. Analyte spiking with HCl is performed to demonstrate the 
integrity of the sampling system for transporting HCl vapor in the flue 
gas to the FTIR instrument. See section 9 of this method for a complete 
description of analyte spiking.

                               5.0 Safety

    5.1 Hydrogen chloride vapor is corrosive and can cause irritation or 
severe damage to respiratory system, eyes and skin. Exposure to this 
compound should be avoided.
    5.2 This method may involve sampling at locations having high 
positive or negative pressures, or high concentrations of hazardous or 
toxic pollutants, and can not address all safety problems encountered 
under these diverse sampling conditions. It is the responsibility of the 
tester(s) to ensure proper safety and health practices, and to determine 
the applicability of regulatory limitations before performing this test 
method. Leak-check procedures are outlined in section 8.2 of Method 320 
of this appendix.

                       6.0 Equipment and Supplies

    Note: Mention of trade names or specific products does not 
constitute endorsement by the Environmental Protection Agency.

    6.1 FTIR Spectrometer and Detector. An FTIR Spectrometer system 
(interferometer, transfer optics, gas cell and detector) having the 
capability of measuring HCl to the predetermined minimum detectable 
level required (see section 4.1.3 of the FTIR Protocol). The system must 
also include an accurate means to control and/or measure the temperature 
of the FTIR gas analysis cell, and a personal computer with compatible 
software that provides real-time updates of the spectral profile during 
sample and spectral collection.

[[Page 340]]

    6.2 Pump. Capable of evacuating the FTIR cell volume to 1 Torr 
(133.3 Pascals) within two minutes (for batch sample analysis).
    6.3 Mass Flow Meters/Controllers. To accurately measure analyte 
spike flow rate, having the appropriate calibrated range and a stated 
accuracy of 2 percent of the absolute measurement 
value. This device must be calibrated with the major component of the 
calibration/spike gas (e.g., nitrogen) using an NIST traceable bubble 
meter or equivalent. Single point calibration checks should be performed 
daily in the field. When spiking HCl, the mass flow meter/controller 
should be thoroughly purged before and after introduction of the gas to 
prevent corrosion of the interior parts.
    6.4 Polytetrafluoroethane tubing. Diameter and length suitable to 
connect cylinder regulators.
    6.5 Stainless Steel tubing. Type 316 of appropriate length and 
diameter for heated connections.
    6.6 Gas Regulators. Purgeable HCl regulator.
    6.7 Pressure Gauge. Capable of measuring pressure from 0 to 1000 
Torr (133.3 Pa=1 Torr) within 5 percent.
    6.8 Sampling Probe. Glass, stainless steel or other appropriate 
material of sufficient length and physical integrity to sustain heating, 
prevent adsorption of analytes and capable of reaching gas sampling 
point.
    6.9 Sampling Line. Heated 180 [deg]C (360 [deg]F) and fabricated of 
either stainless steel, polytetrafluoroethane or other material that 
prevents adsorption of HCl and transports effluent to analytical 
instrumentation. The extractive sample line must have the capability to 
transport sample gas to the analytical components as well as direct 
heated calibration spike gas to the calibration assembly located at the 
sample probe. It is important to minimize the length of heated sample 
line.
    6.10 Particulate Filters. A sintered stainless steel filter rated at 
20 microns or greater may be placed at the inlet of the probe (for 
removal of large particulate matter). A heated filter (Balston or 
equivalent) rated at 1 micron is necessary for primary particulate 
matter removal, and shall be placed immediately after the heated probe. 
The filter/filter holder temperature should be maintained at 180 [deg]C 
(360 [deg]F).
    6.11 Calibration/Analyte Spike Assembly. A heated three-way valve 
assembly (or equivalent) to introduce surrogate spikes into the sampling 
system at the outlet of the probe before the primary particulate filter.
    6.12 Sample Extraction Pump. A leak-free heated head pump (KNF 
Neuberger or equivalent) capable of extracting sample effluent through 
entire sampling system at a rate which prevents analyte losses and 
minimizes analyzer response time. The pump should have a heated by-pass 
and may be placed either before the FTIR instrument or after. If the 
sample pump is located upstream of the FTIR instrument, it must be 
fabricated from materials non-reactive to HCl. The sampling system and 
FTIR measurement system shall allow the operator to obtain at least six 
sample spectra during a one-hour period.
    6.13 Barometer. For measurement of barometric pressure.
    6.14 Gas Sample Manifold. A distribution manifold having the 
capabilities listed in sections 6.14.1 through 6.14.4;
    6.14.1 Delivery of calibration gas directly to the analytical 
instrumentation;
    6.14.2 Delivery of calibration gas to the sample probe (system 
calibration or analyte spike) via a heated traced sample line;
    6.14.3 Delivery of sample gas (kiln gas, spiked kiln gas, or system 
calibrations) to the analytical instrumentation;
    6.14.4 Delivery (optional) of a humidified nitrogen sample stream.
    6.15 Flow Measurement Device. Type S Pitot tube (or equivalent) and 
Magnahelic set for measurement of volumetric flow rate.

                       7.0 Reagents and Standards

    HCl can be purchased in a standard compressed gas cylinder. The most 
stable HCl cylinder mixture available has a concentration certified at 
5 percent. Such a cylinder is suitable for 
performing analyte spiking because it will provide reproducible samples. 
The stability of the cylinder can be monitored over time by periodically 
performing direct FTIR analysis of cylinder samples. It is recommended 
that a 10-50 ppm cylinder of HCl be prepared having from 2-5 ppm SF6 as 
a tracer compound. (See sections 7.1 through 7.3 of Method 320 of this 
appendix for a complete description of the use of existing HCl reference 
spectra. See section 9.1 of Method 320 of this appendix for a complete 
discussion of standard concentration selection.)

             8.0 Sample Collection, Preservation and Storage

    See also Method 320 of this appendix.
    8.1 Pretest. A screening test is ideal for obtaining proper data 
that can be used for preparing analytical program files. Information 
from literature surveys and source personnel is also acceptable. 
Information about the sampling location and gas stream composition is 
required to determine the optimum sampling system configuration for 
measuring HCl. Determine the percent moisture of the kiln gas by Method 
4 of appendix A to part 60 of this chapter or by performing a wet bulb/
dry bulb measurement. Perform a preliminary traverse of the sample duct 
or stack and select the sampling point(s). Acquire an initial spectrum 
and determine the optimum operational pathlength of the instrument.

[[Page 341]]

    8.2 Leak-Check. See Method 320 of this appendix, section 8.2 for 
direction on performing leak-checks.
    8.3 Background Spectrum. See Method 320 of this appendix, section 
8.5 for direction in background spectral acquisition.
    8.4 Pre-Test Calibration Transfer Standard (Direct Instrument 
Calibration). See Method 320 of this appendix, section 8.3 for direction 
in CTS spectral acquisition.
    8.5 Pre-Test System Calibration. See Method 320 of this appendix, 
sections 8.6.1 through 8.6.2 for direction in performing system 
calibration.

                              8.6 Sampling

    8.6.1 Extractive System. An extractive system maintained at 180 
[deg]C (360 [deg]F) or higher which is capable of directing a total flow 
of at least 12 L/min to the sample cell is required (References 1 and 
2). Insert the probe into the duct or stack at a point representing the 
average volumetric flow rate and 25 percent of the cross sectional area. 
Co-locate an appropriate flow monitoring device with the sample probe so 
that the flow rate is recorded at specified time intervals during 
emission testing (e.g., differential pressure measurements taken every 
10 minutes during each run).
    8.6.2 Batch Samples. Evacuate the absorbance cell to 5 Torr (or 
less) absolute pressure before taking first sample. Fill the cell with 
kiln gas to ambient pressure and record the infrared spectrum, then 
evacuate the cell until there is no further evidence of infrared 
absorption. Repeat this procedure, collecting a total of six separate 
sample spectra within a 1-hour period.
    8.6.3 Continuous Flow Through Sampling. Purge the FTIR cell with 
kiln gas for a time period sufficient to equilibrate the entire sampling 
system and FTIR gas cell. The time required is a function of the 
mechanical response time of the system (determined by performing the 
system calibration with the CTS gas or equivalent), and by the chemical 
reactivity of the target analytes. If the effluent target analyte 
concentration is not variable, observation of the spectral up-date of 
the flowing gas sample should be performed until equilibration of the 
sample is achieved. Isolate the gas cell from the sample flow by 
directing the purge flow to vent. Record the spectrum and pressure of 
the sample gas. After spectral acquisition, allow the sample gas to 
purge the cell with at least three volumes of kiln gas. The time 
required to adequately purge the cell with the required volume of gas is 
a function of (1) cell volume, (2) flow rate through the cell, and (3) 
cell design. It is important that the gas introduction and vent for the 
FTIR cell provides a complete purge through the cell.
    8.6.4 Continuous Sampling. In some cases it is possible to collect 
spectra continuously while the FTIR cell is purged with sample gas. The 
sample integration time, tss, the sample flow rate through 
the gas cell, and the sample integration time must be chosen so that the 
collected data consist of at least 10 spectra with each spectrum being 
of a separate cell volume of flue gas. Sampling in this manner may only 
be performed if the native source analyte concentrations do not affect 
the test results.

                         8.7 Sample Conditioning

    8.7.1 High Moisture Sampling. Kiln gas emitted from wet process 
cement kilns may contain 3- to 40 percent moisture. Zinc selenide 
windows or the equivalent should be used when attempting to analyze hot/
wet kiln gas under these conditions to prevent dissolution of water 
soluble window materials (e.g., KBr).
    8.7.2 Sample Dilution. The sample may be diluted using an in-stack 
dilution probe, or an external dilution device provided that the sample 
is not diluted below the instrument's quantification range. As an 
alternative to using a dilution probe, nitrogen may be dynamically 
spiked into the effluent stream in the same manner as analyte spiking. A 
constant dilution rate shall be maintained throughout the measurement 
process. It is critical to measure and verify the exact dilution ratio 
when using a dilution probe or the nitrogen spiking approach. 
Calibrating the system with a calibration gas containing an appropriate 
tracer compound will allow determination of the dilution ratio for most 
measurement systems. The tester shall specify the procedures used to 
determine the dilution ratio, and include these calibration results in 
the report.
    8.8 Sampling QA, Data Storage and Reporting. See the FTIR Protocol. 
Sample integration times shall be sufficient to achieve the required 
signal-to-noise ratio, and all sample spectra should have unique file 
names. Two copies of sample interferograms and processed spectra will be 
stored on separate computer media. For each sample spectrum the analyst 
must document the sampling conditions, the sampling time (while the cell 
was being filled), the time the spectrum was recorded, the instrumental 
conditions (path length, temperature, pressure, resolution, integration 
time), and the spectral file name. A hard copy of these data must be 
maintained until the test results are accepted.
    8.9 Signal Transmittance. Monitor the signal transmittance through 
the instrumental system. If signal transmittance (relative to the 
background) drops below 95 percent in any spectral region where the 
sample does not absorb infrared energy, then a new background spectrum 
must be obtained.

[[Page 342]]

    8.10 Post-test CTS. After the sampling run completion, record the 
CTS spectrum. Analysis of the spectral band area used for quantification 
from pre- and post-test CTS spectra should agree to within 5 percent or corrective action must be taken.
    8.11 Post-test QA. The sample spectra shall be inspected immediately 
after the run to verify that the gas matrix composition was close to the 
assumed gas matrix, (this is necessary to account for the concentrations 
of the interferants for use in the analytical analysis programs), and to 
confirm that the sampling and instrumental parameters were appropriate 
for the conditions encountered.

                           9.0 Quality Control

    Use analyte spiking to verify the effectiveness of the sampling 
system for the target compounds in the actual kiln gas matrix. QA 
spiking shall be performed before and after each sample run. QA spiking 
shall be performed after the pre- and post-test CTS direct and system 
calibrations. The system biases calculated from the pre- and post-test 
dynamic analyte spiking shall be within 30 percent 
for the spiked surrogate analytes for the measurements to be considered 
valid. See sections 9.3.1 through 9.3.2 for the requisite calculations. 
Measurement of the undiluted spike (direct-to-cell measurement) involves 
sending dry, spike gas to the FTIR cell, filling the cell to 1 
atmosphere and obtaining the spectrum of this sample. The direct-to-cell 
measurement should be performed before each analyte spike so that the 
recovery of the dynamically spiked analytes may be calculated. Analyte 
spiking is only effective for assessing the integrity of the sampling 
system when the concentration of HCl in the source does not vary 
substantially. Any attempt to quantify an analyte recovery in a variable 
concentration matrix will result in errors in the expected concentration 
of the spiked sample. If the kiln gas target analyte concentrations vary 
by more than 5 percent (or 5 ppm, whichever is 
greater) in the time required to acquire a sample spectrum, it may be 
necessary to: (1) Use a dual sample probe approach, (2) use two 
independent FTIR measurement systems, (3) use alternate QA/QC 
procedures, or (4) postpone testing until stable emission concentrations 
are achieved. (See section 9.2.3 of this method). It is recommended that 
a laboratory evaluation be performed before attempting to employ this 
method under actual field conditions. The laboratory evaluation shall 
include (1) performance of all applicable calculations in section 4 of 
the FTIR Protocol; (2) simulated analyte spiking experiments in dry 
(ambient) and humidified sample matrices using HCl; and (3) performance 
of bias (recovery) calculations from analyte spiking experiments. It is 
not necessary to perform a laboratory evaluation before every field 
test. The purpose of the laboratory study is to demonstrate that the 
actual instrument and sampling system configuration used in field 
testing meets the requirements set forth in this method.
    9.1 Spike Materials. Perform analyte spiking with an HCl standard to 
demonstrate the integrity of the sampling system.
    9.1.1 An HCl standard of approximately 50 ppm in a balance of ultra 
pure nitrogen is recommended. The SF6 (tracer) concentration 
shall be 2 to 5 ppm depending upon the measurement pathlength. The spike 
ratio (spike flow/total flow) shall be no greater than 1:10, and an 
ideal spike concentration should approximate the native effluent 
concentration.
    9.1.2 The ideal spike concentration may not be achieved because the 
target concentration cannot be accurately predicted prior to the field 
test, and limited calibration standards will be available during 
testing. Therefore, practical constraints must be applied that allow the 
tester to spike at an anticipated concentration. For these tests, the 
analyte concentration contributed by the HCl standard spike should be 1 
to 5 ppm or should more closely approximate the native concentration if 
it is greater.

                           9.2 Spike Procedure

    9.2.1 A spiking/sampling apparatus is shown in Figure 2. Introduce 
the spike/tracer gas mixture at a constant flow (2 
percent) rate at approximately 10 percent of the total sample flow. (For 
example, introduce the surrogate spike at 1 L/min 20 cc/min, into a 
total sample flow rate of 10 L/min). The spike must be pre-heated before 
introduction into the sample matrix to prevent a localized condensation 
of the gas stream at the spike introduction point. A heated sample 
transport line(s) containing multiple transport tubes within the heated 
bundle may be used to spike gas up through the sampling system to the 
spike introduction point. Use a calibrated flow device (e.g., mass flow 
meter/controller), to monitor the spike flow as indicated by a 
calibrated flow meter or controller, or alternately, the SF6 
tracer ratio may be calculated from the direct measurement and the 
diluted measurement. It is often desirable to use the tracer approach in 
calculating the spike/total flow ratio because of the difficulty in 
accurately measuring hot/wet total flow. The tracer technique has been 
successfully used in past validation efforts (Reference 1).
    9.2.2 Perform a direct-to-cell measurement of the dry, undiluted 
spike gas. Introduce the spike directly to the FTIR cell, bypassing the 
sampling system. Fill cell to 1 atmosphere and collect the spectrum of 
this sample. Ensure that the spike gas has equilibrated to the 
temperature of the measurement cell before acquisition of the spectra. 
Inspect the spectrum and verify that the gas

[[Page 343]]

is dry and contains negligible CO2. Repeat the process to 
obtain a second direct-to-cell measurement. Analysis of spectral band 
areas for HCl from these duplicate measurements should agree to within 
5 percent of the mean.
    9.2.3 Analyte Spiking. Determine whether the kiln gas contains 
native concentrations of HCl by examination of preliminary spectra. 
Determine whether the concentration varies significantly with time by 
observing a continuously up-dated spectrum of sample gas in the flow-
through sampling mode. If the concentration varies by more than 5 percent during the period of time required to acquire 
a spectra, then an alternate approach should be used. One alternate 
approach uses two sampling lines to convey sample to the gas 
distribution manifold. One of the sample lines is used to continuously 
extract unspiked kiln gas from the source. The other sample line serves 
as the analyte spike line. One FTIR system can be used in this 
arrangement. Spiked or unspiked sample gas may be directed to the FTIR 
system from the gas distribution manifold, with the need to purge only 
the components between the manifold and the FTIR system. This approach 
minimizes the time required to acquire an equilibrated sample of spiked 
or unspiked kiln gas. If the source varies by more than 5 percent (or 5 ppm, whichever is greater) in the time 
it takes to switch from the unspiked sample line to the spiked sample 
line, then analyte spiking may not be a feasible means to determine the 
effectiveness of the sampling system for the HCl in the sample matrix. A 
second alternative is to use two completely independent FTIR measurement 
systems. One system would measure unspiked samples while the other 
system would measure the spiked samples. As a last option, (where no 
other alternatives can be used) a humidified nitrogen stream may be 
generated in the field which approximates the moisture content of the 
kiln gas. Analyte spiking into this humidified stream can be employed to 
assure that the sampling system is adequate for transporting the HCl to 
the FTIR instrumentation.
    9.2.3.1 Adjust the spike flow rate to approximately 10 percent of 
the total flow by metering spike gas through a calibrated mass flowmeter 
or controller. Allow spike flow to equilibrate within the sampling 
system before analyzing the first spiked kiln gas samples. A minimum of 
two consecutive spikes are required. Analysis of the spectral band area 
used for quantification should agree to within 5 
percent or corrective action must be taken.
    9.2.3.2 After QA spiking is completed, the sampling system 
components shall be purged with nitrogen or dry air to eliminate traces 
of the HCl compound from the sampling system components. Acquire a 
sample spectra of the nitrogen purge to verify the absence of the 
calibration mixture.
    9.2.3.3 Analyte spiking procedures must be carefully executed to 
ensure that meaningful measurements are achieved. The requirements of 
sections 9.2.3.3.1 through 9.2.3.3.4 shall be met.
    9.2.3.3.1 The spike must be in the vapor phase, dry, and heated to 
(or above) the kiln gas temperature before it is introduced to the kiln 
gas stream.
    9.2.3.3.2 The spike flow rate must be constant and accurately 
measured.
    9.2.3.3.3 The total flow must also be measured continuously and 
reliably or the dilution ratio must otherwise be verified before and 
after a run by introducing a spike of a non-reactive, stable compound 
(i.e., tracer).
    9.2.3.3.4 The tracer must be inert to the sampling system 
components, not contained in the effluent gas, and readily detected by 
the analytical instrumentation. Sulfur hexafluoride (SF6) has 
been used successfully (References 1 and 2) for this purpose.

                            9.3 Calculations

    9.3.1 Recovery. Calculate the percent recovery of the spiked 
analytes using equations 1 and 2.
[GRAPHIC] [TIFF OMITTED] TR14JN99.033

Sm = Mean concentration of the analyte spiked effluent 
samples (observed).
[GRAPHIC] [TIFF OMITTED] TR14JN99.034

Ce = Expected concentration of the spiked samples 
(theoretical).
Df = dilution Factor (Total flow/Spike flow). total flow = 
spike flow plus effluent flow.
Cs = cylinder concentration of spike gas.
Su = native concentration of analytes in unspiked samples.

The spike dilution factor may be confirmed by measuring the total flow 
and the spike flow directly. Alternately, the spike dilution can be 
verified by comparing the concentration of the tracer compound in the 
spiked samples (diluted) to the tracer concentration in the direct 
(undiluted) measurement of the spike gas.
If SF6 is the tracer gas, then
[GRAPHIC] [TIFF OMITTED] TR14JN99.035

[SF6]spike = the diluted SF6 
concentration measured in a spiked sample.
[SF6]direct = the SF6 concentration 
measured directly.

    9.3.2 Bias. The bias may be determined by the difference between the 
observed spike value and the expected response (i.e., the equivalent 
concentration of the spiked material plus the analyte concentration 
adjusted

[[Page 344]]

for spike dilution). Bias is defined by section 6.3.1 of EPA Method 301 
of this appendix (Reference 8) as,
[GRAPHIC] [TIFF OMITTED] TR14JN99.036

Where:
B = Bias at spike level.
Sm = Mean concentration of the analyte spiked samples.
Ce = Expected concentration of the analyte in spiked samples.

Acceptable recoveries for analyte spiking are 30 
percent. Application of correction factors to the data based upon bias 
and recovery calculations is subject to the approval of the 
Administrator.

                  10.0 Calibration and Standardization

    10.1 Calibration transfer standards (CTS). The EPA Traceability 
Protocol gases or NIST traceable standards, with a minimum accuracy of 
2 percent shall be used. For other requirements of 
the CTS, see the FTIR Protocol section 4.5.
    10.2 Signal-to-Noise Ratio (S/N). The S/N shall be less than the 
minimum acceptable measurement uncertainty in the analytical regions to 
be used for measuring HCl.
    10.3 Absorbance Pathlength. Verify the absorbance path length by 
comparing CTS spectra to reference spectra of the calibration gas(es).
    10.4 Instrument Resolution. Measure the line width of appropriate 
CTS band(s) to verify instrumental resolution.
    10.5 Apodization Function. Choose the appropriate apodization 
function. Determine any appropriate mathematical transformations that 
are required to correct instrumental errors by measuring the CTS. Any 
mathematical transformations must be documented and reproducible. 
Reference 9 provides additional information about FTIR instrumentation.

                        11.0 Analytical Procedure

    A full description of the analytical procedures is given in sections 
4.6-4.11, sections 5, 6, and 7, and the appendices of the FTIR Protocol. 
Additional description of quantitative spectral analysis is provided in 
References 10 and 11.

                   12.0 Data Analysis and Calculations

    Data analysis is performed using appropriate reference spectra whose 
concentrations can be verified using CTS spectra. Various analytical 
programs (References 10 and 11) are available to relate sample 
absorbance to a concentration standard. Calculated concentrations should 
be verified by analyzing spectral baselines after mathematically 
subtracting scaled reference spectra from the sample spectra. A full 
description of the data analysis and calculations may be found in the 
FTIR Protocol (sections 4.0, 5.0, 6.0 and appendices).
    12.1 Calculated concentrations in sample spectra are corrected for 
differences in absorption pathlength between the reference and sample 
spectra by
[GRAPHIC] [TIFF OMITTED] TR14JN99.037

Where:

Ccorr = The pathlength corrected concentration.
Ccalc = The initial calculated concentration (output of the 
multicomponent analysis program designed for the compound).
Lr = The pathlength associated with the reference spectra.
Ls = The pathlength associated with the sample spectra.
Ts = The absolute temperature (K) of the sample gas.
Tr = The absolute temperature (K) at which reference spectra 
were recorded.

    12.2 The temperature correction in equation 5 is a volumetric 
correction. It does not account for temperature dependence of 
rotational-vibrational relative line intensities. Whenever possible, the 
reference spectra used in the analysis should be collected at a 
temperature near the temperature of the FTIR cell used in the test to 
minimize the calculated error in the measurement (FTIR Protocol, 
appendix D). Additionally, the analytical region chosen for the analysis 
should be sufficiently broad to minimize errors caused by small 
differences in relative line intensities between reference spectra and 
the sample spectra.

                         13.0 Method Performance

    A description of the method performance may be found in the FTIR 
Protocol. This method is self validating provided the results meet the 
performance specification of the QA spike in sections 9.0 through 9.3 of 
this method.

                        14.0 Pollution Prevention

    This is a gas phase measurement. Gas is extracted from the source, 
analyzed by the instrumentation, and discharged through the instrument 
vent.

[[Page 345]]

                          15.0 Waste Management

    Gas standards of HCl are handled according to the instructions 
enclosed with the material safety data sheet.

                             16.0 References

    1. ``Laboratory and Field Evaluation of a Methodology for 
Determination of Hydrogen Chloride Emissions From Municipal and 
Hazardous Waste Incinerators,'' S.C. Steinsberger and J.H. Margeson. 
Prepared for U.S. Environmental Protection Agency, Research Triangle 
Park, NC. NTIS Report No. PB89-220586. (1989).
    2. ``Evaluation of HCl Measurement Techniques at Municipal and 
Hazardous Waste Incinerators,'' S.A. Shanklin, S.C. Steinsberger, and L. 
Cone, Entropy, Inc. Prepared for U.S. Environmental Protection Agency, 
Research Triangle Park, NC. NTIS Report No. PB90-221896. (1989).
    3. ``Fourier Transform Infrared (FTIR) Method Validation at a Coal 
Fired-Boiler,'' Entropy, Inc. Prepared for U.S. Environmental Protection 
Agency, Research Triangle Park, NC. EPA Publication No. EPA-454/R95-004. 
NTIS Report No. PB95-193199. (1993).
    4. ``Field Validation Test Using Fourier Transform Infrared (FTIR) 
Spectrometry To Measure Formaldehyde, Phenol and Methanol at a Wool 
Fiberglass Production Facility.'' Draft. U.S. Environmental Protection 
Agency Report, Entropy, Inc., EPA Contract No. 68D20163, Work Assignment 
I-32.
    5. Kinner, L.L., Geyer, T.G., Plummer, G.W., Dunder, T.A., Entropy, 
Inc. ``Application of FTIR as a Continuous Emission Monitoring System.'' 
Presentation at 1994 International Incineration Conference, Houston, TX. 
May 10, 1994.
    6. ``Molecular Vibrations; The Theory of Infrared and Raman 
Vibrational Spectra,'' E. Bright Wilson, J.C. Decius, and P.C. Cross, 
Dover Publications, Inc., 1980. For a less intensive treatment of 
molecular rotational-vibrational spectra see, for example, ``Physical 
Chemistry,'' G.M. Barrow, chapters 12, 13, and 14, McGraw Hill, Inc., 
1979.
    7. ``Laboratory and Field Evaluations of Ammonium Chloride 
Interference in Method 26,'' U.S. Environmental Protection Agency 
Report, Entropy, Inc., EPA Contract No. 68D20163, Work Assignment No. I-
45.
    8. 40 CFR 63, appendix A. Method 301--Field Validation of Pollutant 
Measurement Methods from Various Waste Media.
    9. ``Fourier Transform Infrared Spectrometry,'' Peter R. Griffiths 
and James de Haseth, Chemical Analysis, 83, 16-25, (1986), P.J. Elving, 
J.D. Winefordner and I.M. Kolthoff (ed.), John Wiley and Sons.
    10. ``Computer-Assisted Quantitative Infrared Spectroscopy,'' 
Gregory L. McClure (ed.), ASTM Special Publication 934 (ASTM), 1987.
    11. ``Multivariate Least-Squares Methods Applied to the Quantitative 
Spectral Analysis of Multicomponent Mixtures,'' Applied Spectroscopy, 
39(10), 73-84, 1985.

[[Page 346]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.038


[[Page 347]]


[GRAPHIC] [TIFF OMITTED] TR14JN99.039


[57 FR 61992, Dec. 29, 1992]

    Editorial Note: For Federal Register citations affecting appendix A 
to part 63, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and on GPO Access.

[[Page 348]]

  Appendix B to Part 63--Sources Defined for Early Reduction Provisions

------------------------------------------------------------------------
                  Source                       Location of definition
------------------------------------------------------------------------
1. Organic Process Equipment in Volatile    56 FR 9315, March 6, 1991,
 Hazardous Air Pollutant Service at          Announcement of Negotiated
 Chemical Plants and Other Designated        Rulemaking
 Facilities.
 
    a. All valves in gas or light liquid
     service within a process unit
    b. All pumps in light liquid service
     within a process unit
    c. All connectors in gas or light
     liquid service within a process unit
    d. Each compressor
    e. Each product accumulator vessel
    f. Each agitator
    g. Each pressure relief device
    h. Each open-ended valve or line
    i. Each sampling connection system
    j. Each instrumentation system
    k. Each pump, valve, or connector in
     heavy liquid service
    l. Each closed vent system and control
     device
------------------------------------------------------------------------


[57 FR 62002, Dec. 29, 1992]

    Appendix C to Part 63--Determination of the Fraction Biodegraded 
            (Fbio) in a Biological Treatment Unit

                               I. Purpose

    The purpose of this appendix is to define the procedures for an 
owner or operator to use to calculate the site specific fraction of 
organic compounds biodegraded (Fbio) in a biological 
treatment unit. If an acceptable level of organic compounds is destroyed 
rather than emitted to the air or remaining in the effluent, the 
biological treatment unit may be used to comply with the applicable 
treatment requirements without the unit being covered and vented through 
a closed vent system to an air pollution control device.
    The determination of Fbio shall be made on a system as it 
would exist under the rule. The owner or operator should anticipate 
changes that would occur to the wastewater flow and concentration of 
organics, to be treated by the biological treatment unit, as a result of 
enclosing the collection and treatment system as required by the rule.
    Unless otherwise specified, the procedures presented in this 
appendix are designed to be applied to thoroughly mixed treatment units. 
A thoroughly mixed treatment unit is a unit that is designed and 
operated to approach or achieve uniform biomass distribution and organic 
compound concentration throughout the aeration unit by quickly 
dispersing the recycled biomass and the wastewater entering the unit. 
Detailed discussion on how to determine if a biological treatment unit 
is thoroughly mixed can be found in reference 7. Systems that are not 
thoroughly mixed treatment units should be subdivided into a series of 
zones that have uniform characteristics within each zone. The number of 
zones required to characterize a biological treatment system will depend 
on the design and operation of the treatment system. Detailed discussion 
on how to determine the number of zones in a biological treatment unit 
and examples of determination of f bio can be found in 
reference 8. Each zone should then be modeled as a separate unit. The 
amount of air emissions and biodegradation from the modeling of these 
separate zones can then be added to reflect the entire system.

                             II. Definitions

    Biological treatment unit = wastewater treatment unit designed and 
operated to promote the growth of bacteria to destroy organic materials 
in wastewater.

fbio = The fraction of individual applicable organic 
compounds in the wastewater biodegraded in a biological treatment unit.
Fbio = The fraction of total applicable organic compounds in 
the wastewater biodegraded in a biological treatment unit.
Fe = The fraction of applicable organic compounds emitted from the 
wastewater to the atmosphere.
K1 = First order biodegradation rate constant, L/g MLVSS-hr
KL = liquid-phase mass transfer coefficient, m/s
M = compound specific mass flow weighted average of organic compounds in 
the wastewater, Mg/Yr

          III. Procedures for Determination of fbio

    The first step in the analysis to determine if a biological 
treatment unit may be used without being covered and vented through a 
closed-vent system to an air pollution control device is to determine 
the compound-specific fbio. The following procedures may be 
used to determine fbio:
    (1) The EPA Test Method 304A or 304B (appendix A, part 63)--Method 
for the Determination of Biodegradation Rates of Organic Compounds,
    (2) Performance data with and without biodegradation,
    (3) Inlet and outlet concentration measurements,
    (4) Batch tests,
    (5) Multiple zone concentration measurements.
    All procedures must be executed so that the resulting 
fbio is based on the collection system and waste management 
units being in compliance with the rule. If the collection system and 
waste management units meet

[[Page 349]]

the suppression requirements at the time of the test, any of the 
procedures may be chosen. If the collection system and waste management 
units are not in compliance at the time of the performance test, then 
only Method 304A, B, or the batch test shall be chosen. If Method 304A, 
B, or the batch test is used, any anticipated changes to the influent of 
the full-scale biological treatment unit that will occur after the 
facility has enclosed the collection system must be represented in the 
influent feed to the benchtop bioreactor unit, or test unit.
    Select one or more appropriate procedures from the five listed above 
based on the availability of site specific data and the type of mixing 
that occurs in the unit (thoroughly mixed or multiple mixing zone). If 
the facility does not have site-specific data on the removal efficiency 
of its biological treatment unit, then Procedure 1 or Procedure 4 may be 
used. Procedure 1 allows the use of a benchtop bioreactor to determine 
the first-order biodegradation rate constant. An owner or operator may 
elect to assume the first order biodegradation rate constant is zero for 
any regulated compound(s) present in the wastewater. Procedure 4 
explains two types of batch tests which may be used to estimate the 
first order biodegradation rate constant. An owner or operator may elect 
to assume the first order biodegradation rate constant is zero for any 
regulated compound(s) present in the wastewater. Procedure 3 would be 
used if the facility has, or measures to determine, data on the inlet 
and outlet individual organic compound concentration for the biological 
treatment unit. Procedure 3 may only be used on a thoroughly mixed 
treatment unit. Procedure 5 is the concentration measurement test that 
can be used for units with multiple mixing zones. Procedure 2 is used if 
a facility has or obtains performance data on a biotreatment unit prior 
to and after addition of the microbial mass. An example where Procedure 
2 could be used is an activated sludge unit where measurements have been 
taken on inlet and exit concentration of organic compounds in the 
wastewater prior to seeding with the microbial mass and startup of the 
unit. The flow chart in figure 1 outlines the steps to use for each of 
the procedures.

                  A. Method 304A or 304B (Procedure 1)

    If the first procedure is selected, follow the instructions in 
appendix A of part 63 Method 304A ``Method for the Determination of 
Biodegradation Rates of Organic Compounds (Vented Option)'' or Method 
304B ``Method for the Determination of Biodegradation Rates of Organic 
Compounds (Scrubber Option).'' Method 304A or 304B provides instruction 
on setting up and operating a self-contained benchtop bioreactor system 
which is operated under conditions representative of the target full-
scale system. Method 304A uses a benchtop bioreactor system with a vent, 
and uses modeling to estimate any air emissions. Method 304B uses a 
benchtop bioreactor system which is equipped with a scrubber and is not 
vented.
    There are some restrictions on which method a source may use. If the 
facility is measuring the rate of biodegradation of compounds that may 
tend to react or hydrolyze in the scrubber of Method 304B, this method 
shall not be used and Method 304A is the required method. If a Henry's 
law value is not available to use with Form V, then Method 304A shall 
not be used and Method 304B is the required method. When using either 
method, the feed flow to the benchtop bioreactor shall be representative 
of the flow and concentration of the wastewater that will be treated by 
the full-scale biological treatment unit after the collection and 
treatment system has been enclosed as required under the applicable 
subpart.
    The conditions under which the full-scale biological treatment unit 
is run establish the operating parameters of Method 304A or 304B. If the 
biological treatment unit is operated under abnormal operating 
conditions (conditions outside the range of critical parameters examined 
and confirmed in the laboratory), the EPA believes this will adversely 
affect the biodegradation rate and is an unacceptable treatment option. 
The facility would be making multiple runs of the test method to 
simulate the operating range for its biological treatment unit. For wide 
ranges of variation in operating parameters, the facility shall 
demonstrate the biological treatment unit is achieving an acceptable 
level of control, as required by the regulation, across the ranges and 
not only at the endpoints.
    If Method 304A is used, complete Form V initially. Form V is used to 
calculate K1 from the Method 304A results. Form V uses the Henry's law 
constant to estimate the fraction lost from the benchtop reactor vent. 
The owner or operator shall use the Henry's law values in Table I. Form 
V also gives direction for calculating an equivalent KL. Note on Form V 
if the calculated number for line 11 is greater than the calculated 
value for line 13, this procedure shall not be used to demonstrate the 
compound is biodegradable. If line 11 is greater than line 13, this is 
an indication the fraction emitted from the vent is greater than the 
fraction biodegraded. The equivalent KL determined on Form V is used in 
Form II (line 6). Estimation of the Fe and fbio must be done 
following the steps in Form III. Form III uses the previously calculated 
values of K1 and KL (equivalent KL), and site-specific parameters of the 
full-scale bioreactor as input to the calculations. Forms II, III, and V 
must be completed for each organic compound in the wastewater to 
determine Fe and fbio.

[[Page 350]]

    If Method 304B is used, perform the method and use the measurements 
to determine K1, which is the first-order biodegradation rate constant. 
Form I lists the sequence of steps in the procedure for calculating K1 
from the Method 304B results. Once K1 is determined, KL must be 
calculated by use of mass transfer equations. Form II outlines the 
procedure to follow for use of mass transfer equations to determine KL. 
A computer program which incorporates these mass transfer equations may 
be used. Water7 is a program that incorporates these mass transfer 
equations and may be used to determine KL. Refer to Form II-A to 
determine KL, if Water7 or the most recent update to this model is used. 
In addition, the Bay Area Sewage Toxics Emission (BASTE) model version 
3.0 or equivalent upgrade and the TOXCHEM (Environment Canada's 
Wastewater Technology Centre and Environmega, Ltd.) model version 1.10 
or equivalent upgrade may also be used to determine KL for the 
biological treatment unit with several stipulations. The programs must 
be altered to output a KL value which is based on the site-specific 
parameters of the unit modeled, and the Henry's law values listed in 
Table I must be substituted for the existing Henry's law values in the 
programs. Input values used in the model and corresponding output values 
shall become documentation of the fbio determination. The 
owner or operator should be aware these programs do not allow modeling 
of certain units. To model these units, the owner or operator shall use 
one of the other appropriate procedures as outlined in this appendix. 
The owner or operator shall not use a default value for KL. The KL value 
determined by use of these models shall be based on the site-specific 
parameters of the specific unit. This KL value shall be inserted in Form 
II (line 6). Estimation of the Fe and fbio must be done 
following the steps in Form III. Form III uses the previously calculated 
values of K1 and KL, and site-specific parameters of the full-scale 
bioreactor as input to the calculations. Forms I, II, and III must be 
completed for each organic compound in the wastewater to determine Fe 
and fbio.

    B. Performance Data With and Without Biodegradation (Procedure 2)

    Procedure 2 uses site-specific performance data that represents or 
characterizes operation of the unit both with and without 
biodegradation. As previously mentioned, proper determination of 
fbio must be made on a system as it would exist under the 
rule. Using Form IV, calculate KL and K1. After KL and K1 are 
determined, Form III is used to calculate Fe and fbio for 
each organic compound present in the wastewater.

      C. Inlet and Outlet Concentration Measurements (Procedure 3)

    Procedure 3 uses measured inlet and outlet organic compound 
concentrations for the unit. This procedure may only be used on a 
thoroughly mixed treatment unit. Again, proper determination of 
fbio must be made on a system as it would exist under the 
rule. The first step in using this procedure is to calculate KL using 
Form II. A computer model may be used. If the Water7 model or the most 
recent update to this model is used, then use Form II-A to calculate KL. 
After KL is determined using field data, complete Form VI to calculate 
K1. The TOXCHEM or BASTE model may also be used to calculate KL for the 
biological treatment unit, with the stipulations listed in procedure 
304B. After KL and K1 are determined, Form III is used to calculate Fe 
and fbio for each organic compound.

                      D. Batch Tests (Procedure 4)

    Two types of batch tests which may be used to determine kinetic 
parameters are: (1) The aerated reactor test and (2) the sealed reactor 
test. The aerated reactor test is also known as the BOX test (batch test 
with oxygen addition). The sealed reactor test is also known as the 
serum bottle test. These batch tests should be conducted only by persons 
familiar with procedures for determining biodegradation kinetics. 
Detailed discussions of batch procedures for determining biodegradation 
kinetic parameters can be found in references 1-4.
    For both batch test approaches, a biomass sample from the activated 
sludge unit of interest is collected, aerated, and stored for no more 
than 4 hours prior to testing. To collect sufficient data when 
biodegradation is rapid, it may be necessary to dilute the biomass 
sample. If the sample is to be diluted, the biomass sample shall be 
diluted using treated effluent from the activated sludge unit of 
interest to a concentration such that the biodegradation test will last 
long enough to make at least six concentration measurements. It is 
recommended that the tests not be terminated until the compound 
concentration falls below the limit of quantitation (LOQ). Measurements 
that are below the LOQ should not be used in the data analysis. Biomass 
concentrations shall be determined using standard methods for 
measurement of mixed liquor volatile suspended solids (MLVSS) (reference 
5).
    The change in concentration of a test compound may be monitored by 
either measuring the concentration in the liquid or in the reactor 
headspace. The analytical technique chosen for the test should be as 
sensitive as possible. For the batch test procedures described in this 
section, equilibrium conditions must exist between the liquid and gas 
phases of the experiments because the

[[Page 351]]

data analysis procedures are based on this premise. To use the headspace 
sampling approach, the reactor headspace must be in equilibrium with the 
liquid so that the headspace concentrations can be correlated with the 
liquid concentrations. Before the biodegradation testing is conducted, 
the equilibrium assumption must be verified. A discussion of the 
equilibrium assumption verification is given below in sections D.1 and 
D.2 since different approaches are required for the two types of batch 
tests.
    To determine biodegradation kinetic parameters in a batch test, it 
is important to choose an appropriate initial substrate (compound(s) of 
interest) concentration for the test. The outcome of the batch 
experiment may be influenced by the initial substrate (SO) to 
biomass (XO) ratio (see references 3, 4, and 6). This ratio 
is typically measured in chemical oxygen demand (COD) units. When the 
SO/XO ratio is low, cell multiplication and growth 
in the batch test is negligible and the kinetics measured by the test 
are representative of the kinetics in the activated sludge unit of 
interest. The SO/XO ratio for a batch test is 
determined with the following equation:
[GRAPHIC] [TIFF OMITTED] TR17JA97.034

Where:

SO/XO=initial substrate to biomass ratio on a COD 
basis
Si=initial substrate concentration in COD units (g COD/L)
X=biomass concentration in the batch test (g MLVSS/L)
1.42 = Conversion factor to convert to COD units

    For the batch tests described in this section, the SO/
XO ratio (on a COD basis) must be initially less than 0.5.
    1. Aerated Reactor Test. An aerated draft tube reactor may be used 
for the biokinetics testing (as an example see Figure 2 of appendix C). 
Other aerated reactor configurations may also be used. Air is bubbled 
through a porous frit at a rate sufficient to aerate and keep the 
reactor uniformly mixed. Aeration rates typically vary from 50 to 200 
ml/min for a 1 liter system. A mass flow rate controller is used to 
carefully control the air flow rate because it is important to have an 
accurate measure of this rate. The dissolved oxygen (DO) concentration 
in the system must not fall below 2 mg/liter so that the biodegradation 
observed will not be DO-limited. Once the air flow rate is established, 
the test mixture (or compound) of interest is then injected into the 
reactor and the concentration of the compound(s) is monitored over time. 
Concentrations may be monitored in the liquid or in the headspace. A 
minimum of six samples shall be taken over the period of the test. 
However, it is necessary to collect samples until the compound 
concentration falls below the LOQ. If liquid samples are collected, they 
must be small enough such that the liquid volume in the batch reactor 
does not change by more than 10%.
    Before conducting experiments with biomass, it is necessary to 
verify the equilibrium assumption. The equilibrium assumption can be 
verified by conducting a stripping experiment using the effluent (no 
biomass) from the activated sludge unit of interest. Effluent is 
filtered with a 0.45 um or smaller filter and placed in the draft tube 
reactor. Air is sparged into the system and the compound concentration 
in the liquid or headspace is monitored over time. This test with no 
biomass may provide an estimate of the Henry's law constant. If the 
system is at equilibrium, the Henry's law constant may be estimated with 
the following equation:
[GRAPHIC] [TIFF OMITTED] TR17JA97.035

Where:

C=cencentration at time, t (min)
CO=concentration at t=0
G=volumetric gas flow rate (ml/min)
V=liquid volume in the batch reactor (ml)
Keq=Henry's law constant (mg/L-gas)/(mg/L-liquid)
t=time (min)

    A plot of--ln(C/Co) as a function of t will have a slope 
equal to GKeq/V. The equilibrium assumption can be verified 
by comparing the experimentally determined Keq for the system 
to literature values of the Henry's Law constant (including those listed 
in this appendix). If Keq does not match the Henry's law 
constant, Keq shall be determined from analysis of the 
headspace and liquid concentration in a batch system.
    The concentration of a compound decreases in the bioreactor due to 
both biodegradation and stripping. Biodegradation processes are 
typically described with a Monod model. This model and a stripping 
expression are combined to give a mass balance for the aerated draft 
tube reactor ):

[[Page 352]]

[GRAPHIC] [TIFF OMITTED] TR17JA97.036

Where:

s=test compound concentration, mg/liter
G=volumetric gas flow rate, liters/hr
Keq=Henry's Law constant measured in the system, (mg/liter 
gas)/(mg/liter liquid)
V=volume of liquid in the reactor, liters
X=biomass concentration (g MLVSS/liter)
Qm=maximum rate of substrate removal, mg/g MLVSS/hr
KS=Monod biorate constant at half the maximum rate, mg/liter

    Equation App. C-3 can be integrated to obtain the following 
equation:
[GRAPHIC] [TIFF OMITTED] TR22JA01.162

Where:
A=GKeqKs + QmVX
B=GKeq
So=test compound concentration at t=0
    This equation is used along with the substrate concentration versus 
time data to determine the best fit parameters (Qm and 
KS) to describe the biodegradation process in the aerated 
reactor. If the aerated reactor test is used, the following procedure is 
used to analyze the data. Evaluate Keq for the compound of 
interest with Form XI. The concentration in the vented headspace or 
liquid is measured as a function of time and the data is entered on Form 
XI. A plot is made from the data and attached to the Form XI. 
Keq is calculated on Form XI and the results are contrasted 
with the expected value of Henry's law obtained from Form IX. If the 
comparison is satisfactory, the stripping constant is calculated from 
Keq, completing Form XI. The values of Keq may 
differ because the theoretical value of Keq may not be 
applicable to the system of interest. If the comparison of the 
calculated Keq from the form and the expected value of 
Henry's law is unsatisfactory, Form X can alternatively be used to 
validate Keq. If the aerated reactor is demonstrated to not 
be at equilibrium, either modify the reactor design and/or operation, or 
use another type of batch test.
    The compound-specific biorate constants are then measured using Form 
XII. The stripping constant that was determined from Form XI and a 
headspace correction factor of 1 are entered on Form XII. The aerated 
reactor biotest may then be run, measuring concentrations of each 
compound of interest as a function of time. If headspace concentrations 
are measured instead of liquid concentrations, then the corresponding 
liquid concentrations are calculated from the headspace measurements 
using the Keq determined on Form XI and entered on Form XII.
    The concentration data on Form XII may contain scatter that can 
adversely influence the data interpretation. It is possible to curve fit 
the concentration data and enter the concentrations on the fitted curve 
instead of the actual data. If curve fitting is used, the curve-fitting 
procedure must be based upon the Equation App. C-4. When curve fitting 
is used, it is necessary to attach a plot of the actual data and the 
fitted curve to Form XII.
    If the stripping rate constant is relatively large when compared to 
the biorate at low concentrations, it may be difficult to obtain 
accurate evaluations of the first-order biorate constant. In these 
cases, either reducing the stripping rate constant by lowering the 
aeration rate, or increasing the biomass concentrations should be 
considered.
    The final result of the batch testing is the measurement of a 
biorate that can be used to estimate the fraction biodegraded, 
fbio. The number transferred to Form III is obtained from 
Form XII, line 9.
    2. Sealed Reactor Test. This test uses a closed system to prevent 
losses of the test compound by volatilization. This test may be 
conducted using a serum bottle or a sealed draft tube reactor (for an 
example see Figure 3 of appendix C). Since no air is supplied, it is 
necessary to ensure that sufficient oxygen is present in the system. The 
DO concentration in the system must not fall below 2 mg/liter so that 
the biodegradation observed will not be DO-limited. As an alternative, 
oxygen may be supplied by electrolysis as needed to maintain the DO 
concentration above 2 mg/liter. The reactor contents must be uniformly 
mixed, by stirring

[[Page 353]]

or agitation using a shaker or similar apparatus. The test mixture (or 
compound) of interest is injected into the reactor and the concentration 
is monitored over time. A minimum of six samples shall be taken over the 
period of the test. However, it is necessary to monitor the 
concentration until it falls below the LOQ.
    The equilibrium assumption must be verified for the batch reactor 
system. In this case, Keq may be determined by simultaneously 
measuring gas and liquid phase concentrations at different times within 
a given experiment. A constant ratio of gas/liquid concentrations 
indicates that equilibrium conditions are present and Keq is 
not a function of concentration. This ratio is then taken as the 
Keq for the specific compound in the test. It is not 
necessary to measure Keq for each experiment. If the ratio is 
not constant, the equilibrium assumption is not valid and it is 
necessary to (1) increase mixing energy for the system and retest for 
the equilibrium assumption, or (2) use a different type of test (for 
example, a collapsible volume reactor).
    The concentration of a compound decreases in the bioreactor due to 
biodegradation according to Equation App. C-5:
[GRAPHIC] [TIFF OMITTED] TR17JA97.038

Where:

s=test compound concentration (mg/liters)
Vl=the average liquid volume in the reactor (liters)
Vg=the average gas volume in the reactor (liters)
Qm=maximum rate of substrate removal (mg/g ML VSS/hr)
Keq=Henry's Law constant determined for the test, (mg/liter 
gas)/(mg/liter liquid)
Ks=Monod biorate constant at one-half the maximum rate (mg/
liter)
t=time (hours)
X=biomass concentration (g ML VSS/liter )
so=test compound concentration at time t=0

    Equation App. C-5 can be solved analytically to give:
    [GRAPHIC] [TIFF OMITTED] TR22JA01.163
    
    This equation is used along with the substrate concentration versus 
time data to determine the best fit parameters (Qm and 
Ks) to describe the biodegradation process in the sealed 
reactor.
    If the sealed reactor test is used, Form X is used to determine the 
headspace correction factor. The disappearance of a compound in the 
sealed reactor test is slowed because a fraction of the compound is not 
available for biodegradation because it is present in the headspace. If 
the compound is almost entirely in the liquid phase, the headspace 
correction factor is approximately one. If the headspace correction 
factor is substantially less than one, improved mass transfer or reduced 
headspace may improve the accuracy of the sealed reactor test. A 
preliminary sealed reactor test must be conducted to test the 
equilibrium assumption. As the compound of interest is degraded, 
simultaneous headspace and liquid samples should be collected and Form X 
should be used to evaluate Keq. The ratio of headspace to 
liquid concentrations must be constant in order to confirm that 
equilibrium conditions exist. If equilibrium conditions are not present, 
additional mixing or an alternate reactor configuration may be required.
    The compound-specific biorate constants are then calculated using 
Form XII. For the sealed reactor test, a stripping rate constant of zero 
and the headspace correction factor that was determined from Form X are 
entered on Form XII. The sealed reactor test may then be run, measuring 
the concentrations of each compound of interest as a function of time. 
If headspace concentrations are measured instead of liquid 
concentrations, then the corresponding liquid concentrations are 
calculated from the headspace measurements using Keq from 
Form X and entered on Form XII.
    The concentration data on Form XII may contain scatter that can 
adversely influence the data interpretation. It is possible to

[[Page 354]]

curve fit the concentration data and enter the concentrations on the 
fitted curve instead of the actual data. If curve fitting is used, the 
curve-fitting procedure must be based upon Equation App. C-6. When curve 
fitting is used, it is necessary to attach a plot of the actual data and 
the fitted curve to Form XII.
    If a sealed collapsible reactor is used that has no headspace, the 
headspace correction factor will equal 1, but the stripping rate 
constant may not equal 0 due to diffusion losses through the reactor 
wall. The ratio of the rate of loss of compound to the concentration of 
the compound in the reactor (units of per hour) must be evaluated. This 
loss ratio has the same units as the stripping rate constant and may be 
entered as the stripping rate constant on line 1 of Form XII.
    If the loss due to diffusion through the walls of the collapsible 
reactor is relatively large when compared to the biorate at low 
concentrations, it may be difficult to obtain accurate evaluations of 
the first-order biorate constant. In these cases, either replacing the 
materials used to construct the reactor with materials of low 
permeability or increasing the biomass concentration should be 
considered.
    The final result of the batch testing is the measurement of a 
biorate that can be used to estimate the fraction biodegraded, 
fbio. The number transferred to Form III is obtained from 
Form XII, line 9.
    The number on Form XII line 9 will equal the Monod first-order 
biorate constant if the full-scale system is operated in the first-order 
range. If the full-scale system is operated at concentrations above that 
of the Monod first-order range, the value of the number on line 9 will 
be somewhat lower than the Monod first-order biorate constant. With 
supporting biorate data, the Monod model used in Form XII may be used to 
estimate the effective biorate constant K1 for use in Form III.
    If a reactor with headspace is used, analysis of the data using 
equation App. C-6 is valid only if Vl and Vg do 
not change more than 10% (i.e., they can be approximated as constant for 
the duration of the test). Since biodegradation is occurring only in the 
liquid, as the liquid concentration decreases it is necessary for mass 
to transfer from the gas to the liquid phase. This may require vigorous 
mixing and/or reducing the volume in the headspace of the reactor.
    If there is no headspace (e.g., a collapsible reactor), equation 
App. C-6 is independent of V1 and there are no restrictions 
on the liquid volume. If a membrane or bag is used as the collapsible-
volume reactor, it may be important to monitor for diffusion losses in 
the system. To determine if there are losses, the bag should be used 
without biomass and spiked with the compound(s) of interest. The 
concentration of the compound(s) in the reactor should be monitored over 
time. The data are analyzed as described above for the sealed reactor 
test.
    3. Quality Control/Quality Assurance (QA/QC). A QA/QC plan outlining 
the procedures used to determine the biodegradation rate constants shall 
be prepared and a copy maintained at the source. The plan should 
include, but may not be limited to:
    1. A description of the apparatus used (e.g., size, volume, method 
of supplying air or oxygen, mixing, and sampling procedures) including a 
simplified schematic drawing.
    2. A description of how biomass was sampled from the activated 
sludge unit.
    3. A description of how biomass was held prior to testing (age, 
etc.).
    4. A description of what conditions (DO, gas-liquid equilibrium, 
temperature, etc.) are important, what the target values are, how the 
factors were controlled, and how well they were controlled.
    5. A description of how the experiment was conducted, including 
preparation of solutions, dilution procedures, sampling procedures, 
monitoring of conditions, etc.
    6. A description of the analytical instrumentation used, how the 
instruments were calibrated, and a summary of the precision for that 
equipment.
    7. A description of the analytical procedures used. If appropriate, 
reference to an ASTM, EPA or other procedure may be used. Otherwise, 
describe how the procedure is done, what is done to measure precision, 
accuracy, recovery, etc., as appropriate.
    8. A description of how data are captured, recorded, and stored.
    9. A description of the equations used and their solutions, 
including a reference to any software used for calculations and/or 
curve-fitting.

        E. Multiple Zone Concentration Measurements (Procedure 5)

    Procedure 5 is the concentration measurement method that can be used 
to determine the fbio for units that are not thoroughly mixed 
and thus have multiple zones of mixing. As with the other procedures, 
proper determination of fbio must be made on a system as it 
would exist under the rule. For purposes of this calculation, the 
biological unit must be divided \1\ into zones with uniform 
characteristics within each zone. The number of zones that is used 
depends on the complexity of the unit. Reference 8, ``Technical Support

[[Page 355]]

Document for the Evaluation of Aerobic Biological Treatment Units with 
Multiple Mixing Zones,'' is a source for further information concerning 
how to determine the number of zones that should be used for evaluating 
your unit. The following information on the biological unit must be 
available to use this procedure: basic unit variables such as inlet and 
recycle wastewater flow rates, type of agitation, and operating 
conditions; measured representative organic compound concentrations in 
each zone and the inlet and outlet; and estimated mass transfer 
coefficients for each zone.
---------------------------------------------------------------------------

    \1\ This is a mathematical division of the actual unit; not addition 
of physical barriers.
---------------------------------------------------------------------------

    Reference 8 ``Technical Support Document for the Evaluation of 
Aerobic Biological Treatment Units with Multiple Mixing Zones,'' is a 
source for further information concerning how to interpolate the 
biorates for multiple zones. In units with well-characterized 
concentration measurements obtained in an initial evaluation of the 
unit, it may be possible to demonstrate that there is a good correlation 
of the component concentrations with the locations in the multiple-zone 
unit. With this good correlation, it may be possible to accurately 
predict the concentrations in selected zones without actually testing 
each selected zone. This correlation method may be used for units that 
have many zones (greater than 5) or where one of the interior zones is 
not readily accessible for sampling. To use this correlation method of 
estimating zone concentrations, it is necessary to measure the 
concentrations in the inlet unit, the exit unit, and sufficient interior 
units to obtain a correlation of component concentrations with the 
locations. You cannot use this correlation method of estimating selected 
zone concentrations if monitoring of each zone is required, or if the 
accuracy and precision of the correlation is inferior to actual 
individual sampling error. The accuracy and precision of the correlation 
may be improved by increasing the number of locations tested. Because 
the correlation is based on many samples, it should provide an accurate 
representation of a stable operating system.
    The estimated mass transfer coefficient for each compound in each 
zone is obtained from Form II using the characteristics of each zone. A 
computer model may be used. If the Water7 model or the most recent 
update to this model is used, then use Form II-A to calculate KL. The 
TOXCHEM or BASTE model may also be used to calculate KL for the 
biological treatment unit, with the stipulations listed in Procedure 
304B. Compound concentration measurements for each zone are used in Form 
XIII to calculate the fbio. A copy of Form XIII is completed 
for each of the compounds of concern treated in the biological unit.

                         IV. Calculation of Fbio

    At this point, the individual fbios determined by the 
previously explained procedures must be summed to obtain the total 
Fbio. To determine the Fbio multiply each compound 
specific fbio by the compound-specific average mass flow rate 
of the organic compound in the wastewater stream (see regulation for 
instruction on calculation of average mass flow rate). Sum these 
products and divide by the total wastewater stream average mass flow 
rate of organic compounds.
[GRAPHIC] [TIFF OMITTED] TR17JA97.040

M=compound specific average mass flow rate of the organic compounds in 
the wastewater (Mg/Yr)
n=number of organic compounds in the wastewater

    The Fbio is then used in the applicable compliance 
equations in the regulation to determine if biodegradation may be used 
to comply with the treatment standard without covering and venting to an 
air pollution control device.

                               References

    1. Rajagopalan, S. et al. ``Comparison of Methods for Determining 
Biodegradation Kinetics of Volatile Organic Compounds.'' Proceedings of 
Water Environment Federation. 67th Annual Conference, October 15-19, 
1994.
    2. Ellis, T.G. et al. ``Determination of Toxic Organic Chemical 
Biodegradation Kinetics Using Novel Respirometric Technique''. 
Proceedings Water Environment Federation, 67th Annual Conference, 
October 15-19, 1994.
    3. Pitter, P. and J. Chudoba. Biodegradability of Organic Substances 
in

[[Page 356]]

the Aquatic Environment. CRC Press, Boca Raton, FL. 1990.
    4. Grady, C.P.L., B. Smets, and D. Barbeau. Variability in kinetic 
parameter estimates: A review of possible causes and a proposed 
terminology. Wat. Res. 30 (3), 742-748, 1996.
    5. Eaton, A.D., et al. eds., Standard Methods for the Examination of 
Water and Wastewater, 19th Edition, American Public Health Association, 
Washington, DC, 1995.
    6. Chudoba P., B. Capdeville, and J. Chudoba. Explanation of 
biological meaning of the So/Xo ratio in batch cultivation. Wat. Sci. 
Tech. 26 (3/4), 743-751, 1992.
    7. Technical Support Document for Evaluation of Thoroughly Mixed 
Biological Treatment Units. November 1998.
    8. Technical Support Document for the Evaluation of Aerobic 
Biological Treatment Units with Multiple Mixing Zones. July 1999.

                                 Table I
------------------------------------------------------------------------
                                  HL @ 25 [deg]C (atm/   HL @ 100 [deg]C
            Compound                   mole frac)        (atm/mole frac)
------------------------------------------------------------------------
1 Acetaldehyde.................  4.87e+00                5.64e+01
3 Acetonitrile.................  1.11e+00                1.78e+01
4 Acetophenone.................  5.09e-01                2.25e+01
5 Acrolein.....................  4.57e+00                6.61e+01
8 Acrylonitrile................  5.45e+00                6.67e+01
9 Allyl chloride...............  5.15e+02                2.26e+03
10 Aniline.....................  9.78e-02                1.42e+00
12 Benzene.....................  3.08e+02                1.93e+03
14 Benzyl chloride.............  1.77e+01                2.88e+02
15 Biphenyl....................  2.27e+01                1.27e+03
17 Bromoform...................  2.96e+01                3.98e+02
18 1,3-Butadiene...............  3.96e+03                1.56e+04
20 Carbon disulfide............  1.06e+03                3.60e+03
21 Carbon tetrachloride........  1.68e+03                1.69e+04
23 2-Chloroacetophenone........  4.84e-02                1.43e+01
24 Chlorobenzene...............  2.09e+02                3.12e+03
25 Chloroform..................  2.21e+02                1.34e+03
26 Chloroprene.................  5.16e+01                1.74e+02
29 o-Cresol....................  9.12e-02                2.44e+01
31 Cumene......................  7.28e+02                7.15e+03
32 1,4-Dichlorobenzene(p)......  1.76e+02                1.95e+03
33 Dichloroethyl ether.........  1.14e+00                3.57e+01
34 1,3-Dichloropropene.........  1.97e+02                1.44e+03
36 N,N-Dimethylaniline.........  7.70e-01                5.67e+02
37 Diethyl sulfate.............  3.41e-01                4.22e+01
38 3,3'-Dimethylbenzidine......  7.51e-05                5.09e-01
40 1,1-Dimethylhydrazine.......  9.11e-02                1.57e+01
42 Dimethyl sulfate............  2.23e-01                1.43e+01
43 2,4-Dinitrophenol...........  2.84e-01                1.50e+02
44 2,4-Dinitrotoluene..........  4.00e-01                9.62e+00
45 1,4-Dioxane.................  3.08e-01                9.53e+00
47 Epichlorohydrin.............  1.86e+00                4.34e+01
48 Ethyl acrylate..............  1.41e+01                3.01e+02
49 Ethylbenzene................  4.38e+02                4.27e+03
50 Ethyl chloride                6.72e+02                3.10e+03
 (chloroethane).
51 Ethylene dibromide..........  3.61e+01                5.15e+02
52 Ethylene dichloride (1,2-     6.54e+01                5.06e+02
 Dichloroethane).
54 Ethylene oxide..............  1.32e+01                9.09e+01
55 Ethylidene dichloride (1,1-   3.12e+02                2.92e+03
 Dichloroethane).
57 Ethylene glycol dimethyl      1.95e+00                4.12e+01
 ether.
60 Ethylene glycol monoethyl     9.86e-02                6.03e+00
 ether acetate.
62 Ethylene glycol monomethyl    1.22e-01                6.93e+00
 ether acetate.
64 Diethylene glycol dimethyl    8.38e-02                4.69e+00
 ether.
69 Diethylene glycol diethyl     1.19e-01                7.71e+00
 ether.
72 Ethylene glycol monobutyl     2.75e-01                2.50e+01
 ether acetate.
73 Hexachlorobenzene...........  9.45e+01                2.57e+04
74 Hexachlorobutadiene.........  5.72e+02                6.92e+03
75 Hexachloroethane............  4.64e+02                7.49e+04
76 Hexane......................  4.27e+04                9.44e+04
78 Isophorone..................  3.68e-01                1.68e+01
80 Methanol....................  2.89e-01                7.73e+00
81 Methyl bromide                3.81e+02                2.12e+03
 (Bromomethane).
82 Methyl chloride               4.90e+02                2.84e+03
 (Chloromethane).
83 Methyl chloroform (1,1,1-     9.67e+02                5.73e+03
 Trichloroethane).
84 Methyl ethyl ketone (2-       7.22e+00                5.92e+01
 Butanone).
86 Methyl isobutyl ketone        2.17e+01                3.72e+02
 (Hexone).
88 Methyl methacrylate.........  7.83e+00                9.15e+01
89 Methyl tert-butyl ether.....  3.08e+01                2.67e+02

[[Page 357]]

 
90 Methylene chloride            1.64e+02                9.15e+02
 (Dichloromethane).
93 Naphthalene.................  2.68e+01                7.10e+02
94 Nitrobenzene................  1.33e+00                2.80e+01
96 2-Nitropropane..............  6.61e+00                8.76e+01
99 Phosgene....................  7.80e+02                3.51e+03
102 Propionaldehyde............  3.32e+00                1.42e+02
103 Propylene dichloride.......  1.59e+02                1.27e+03
104 Propylene oxide............  1.98e+01                1.84e+02
106 Styrene....................  1.45e+02                1.72e+03
107 1,1,2,2-Tetrachloroethane..  1.39e+01                1.99e+02
108 Tetrachloroethylene          9.83e+02                1.84e+04
 (Perchloroethylene).
109 Toluene....................  3.57e+02                2.10e+03
112 o-Toluidine................  1.34e-01                1.15e+01
113 1,2,4-Trichlorobenzene.....  1.07e+02                1.04e+03
114 1,1,2-Trichloroethane......  4.58e+01                5.86e+02
115 Trichloroethylene..........  5.67e+02                7.66e+03
116 2,4,5-Trichlorophenol......  4.84e-01                6.27e+01
117 Triethylamine..............  6.94e+00                2.57e+02
118 2,2,4-Trimethylpentane.....  1.85e+05                9.74e+05
119 Vinyl acetate..............  2.82e+01                2.80e+02
120 Vinyl chloride.............  1.47e+03                6.45e+03
121 Vinylidene chloride (1,1-    1.44e+03                1.40e+04
 Dichloroethylene).
123 m-Xylene...................  4.13e+02                3.25e+03
124 o-Xylene...................  2.71e+02                2.55e+03
125 p-Xylene...................  4.13e+02                3.20e+03
------------------------------------------------------------------------


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[62 FR 2801, Jan. 17, 1997, as amended at 63 FR 67794, Dec. 9, 1998; 66 
FR 6935, Jan. 22, 2001]

 Appendix D to Part 63--Alternative Validation Procedure for EPA Waste 
                         and Wastewater Methods

                            1. Applicability

    This procedure is to be applied exclusively to Environmental 
Protection Agency methods developed by the Office of Water and the 
Office of Solid Waste. Alternative methods developed by any other group 
or agency shall be validated according to the procedures in Sections 5.1 
and 5.3 of Test Method 301, 40 CFR Part 63, Appendix A. For the purposes 
of this appendix, ``waste'' means waste and wastewater.

                              2. Procedure

    This procedure shall be applied once for each waste matrix. Waste 
matrix in the context of this procedure refers to the target compound 
mixture in the waste as well as the formulation of the medium in which 
the

[[Page 380]]

target compounds are suspended. The owner or operator shall prepare a 
sampling plan. Wastewater samples shall be collected using sampling 
procedures which minimize loss of organic compounds during sample 
collection and analysis and maintain sample integrity. The sample plan 
shall include procedures for determining recovery efficiency of the 
relevant compounds regulated in the applicable subpart. An example of an 
acceptable sampling plan would be one that incorporates similar sampling 
and sample handling requirements to those of Method 25D of 40 CFR part 
60, appendix A.

                       2.1. Sampling and Analysis

    2.1.1. For each waste matrix, collect twice the number of samples 
required by the applicable regulation. Designate and label half the 
sample vials the ``spiked'' sample set, and the other half the 
``unspiked'' sample set. Immediately before or immediately after 
sampling (immediately after in the context of this procedure means after 
placing the sample into the sample vial, but before the sample is 
capped, cooled, and shipped to the laboratory for analysis), inject, 
either individually or as a solution, all the target compounds into each 
spiked sample.
    2.1.2. The mass of each spiked compound shall be 40 to 60 percent of 
the mass expected to be present in the waste matrix. If the 
concentration of the target compounds in the waste are not known, the 
mass of each spiked compound shall be 40 to 60 percent of the limit 
allowed in the applicable regulation. Analyze both sets of samples 
(spiked and unspiked) with the chosen method.

                             3. Calculations

    For each pair of spiked and unspiked samples, determine the fraction 
of spiked compound recovered (R) using the following equations.

where:
mr = mass spiked compound measured ([mu] g).
ms = total mass of compound measured in spiked sample ([mu] 
g).
mu = total mass of compound measured in unspiked sample ([mu] 
g).
where:
S = theoretical mass of compound spiked into spiked sample ([mu] g).

                         3.1. Method Evaluation

    In order for the chosen method to be acceptable for a compound, 
0.70<=R<=1.30 (R in this case is an average value of all the spiked and 
unspiked sample set R values). If the average R value does not meet this 
criterion for a target compound, the chosen method is not acceptable for 
that compound, and therefore another method shall be evaluated for 
acceptance (by repeating the procedures outlined above with another 
method).

                        3.2. Records and Reports

    Report the average R value in the test report and correct all 
reported measurements made with the method with the calculated R value 
for that compound by using the following equation:
[GRAPHIC] [TIFF OMITTED] TR01JY96.048

                      3.3. Optional Correction Step

    If the applicable regulation allows for correction of the mass of 
the compound in the waste by a published fm value, multiply 
the reported result calculated above with the appropriate fm 
value for that compound.

[61 FR 34200, July 1, 1996]

Appendix E to Part 63--Monitoring Procedure for Nonthoroughly Mixed Open 
 Biological Treatment Systems at Kraft Pulp Mills Under Unsafe Sampling 
                               Conditions

                               I. Purpose

    This procedure is required to be performed in subpart S of this 
part, entitled National Emission Standards for Hazardous Air Pollutants 
from the Pulp and Paper Industry. Subpart S requires this procedure in 
Sec. 63.453(p)(3) to be followed during unsafe sampling conditions when 
it is not practicable to obtain representative samples of hazardous air 
pollutants (HAP) concentrations from an open biological treatment unit. 
It is assumed that inlet and outlet HAP concentrations from the open 
biological treatment unit may be obtained during the unsafe sampling 
conditions. The purpose of this procedure is to estimate the 
concentration of HAP within the open biological treatment unit based on 
information obtained at inlet and outlet sampling locations in units 
that are not thoroughly mixed and, therefore, have different 
concentrations of HAP at different locations within the unit.

[[Page 381]]

                             II. Definitions

    Biological treatment unit = wastewater treatment unit designed and 
operated to promote the growth of bacteria to destroy organic materials 
in wastewater.

fbio =The fraction of organic compounds in the wastewater 
biodegraded in a biological treatment unit.
Fe=The fraction of applicable organic compounds emitted from the 
wastewater to the atmosphere.
K1=First-order biodegradation rate constant, L/g mixed liquor volatile 
suspended solids (MLVSS)-hr
KL=Liquid-phase mass transfer coefficient, m/s
Ks=Monod biorate constant at half the maximum rate, g/m3

 III. Test Procedure for Determination of fbio for Nonthoroughly Mixed 
    Open Biological Treatment Units Under Unsafe Sampling Conditions

    This test procedure is used under unsafe sampling conditions that do 
not permit practicable sampling of open biological treatment units 
within the unit itself, but rather relies on sampling at the inlet and 
outlet locations of the unit. This procedure may be used only under 
unsafe sampling conditions to estimate fbio. Once the unsafe 
conditions have passed, then the formal compliance demonstration 
procedures of fbio based upon measurements within the open 
biological treatment unit must be completed.

                   A. Overview of Estimation Procedure

    The steps in the estimation procedure include data collection, the 
estimation of concentrations within the unit, and the use of Form 1 to 
estimate fbio. The data collection procedure consists of two 
separate components. The first data collection component demonstrates 
that the open biological treatment unit can be represented by Monod 
kinetics and characterizes the effectiveness of the open biological 
treatment unit as part of the initial performance test, and the second 
data collection component is used when there are unsafe sampling 
conditions. These two data collection components are used together in a 
data calculation procedure based on a Monod kinetic model to estimate 
the concentrations in each zone of the open biological treatment unit. 
After the first two components of data collection are completed, the 
calculation procedures are used to back estimate the zone 
concentrations, starting with the last zone in the series and ending 
with the first zone.

                     B. Data Collection Requirements

    This method is based upon modeling the nonthoroughly mixed open 
biological treatment unit as a series of well-mixed zones with internal 
recycling between the units and assuming that two Monod biological 
kinetic parameters can be used to characterize the biological removal 
rates in each unit. The data collection procedure consists of two 
separate components. The first data collection component is part of the 
initial performance test, and the second data collection component is 
used during unsafe sampling conditions.

                       1. Initial Performance Test

    The objective of the first data collection component is to 
demonstrate that the open biological treatment unit can be represented 
by Monod kinetics and to characterize the performance of the open 
biological treatment unit. An appropriate value of the biorate constant, 
Ks, is determined using actual sampling data from the open biological 
treatment unit. This is done during the initial performance test when 
the open biological treatment unit is operating under normal conditions. 
This specific Ks value obtained during the initial performance test is 
used in the calculation procedure to characterize the open biological 
treatment unit during unsafe sampling conditions. The following open 
biological treatment unit characterization information is obtained from 
the first component of the data collection procedure:
    (1) The value of the biorate constant, Ks;
    (2) The number and characteristics of each zone in the open 
biological treatment unit (depth, area, characterization parameters for 
surface aeration, submerged aeration rates, biomass concentration, 
concentrations of organic compounds, dissolved oxygen (DO), dissolved 
solids, temperature, and other relevant variables); and
    (3) The recycle ratio of internal recirculation between the zones. 
The number of zones and the above characterization of the zones are also 
used to determine the performance of the unit under the unsafe sampling 
conditions of concern.

           2. Data Collected Under Unsafe Sampling Conditions

    In the second data collection component obtained under unsafe 
sampling conditions, the measured inlet and outlet HAP concentrations 
and the biomass concentration are obtained for the open biological 
treatment unit. After the site specific data collection is completed on 
the day a parameter excursion occurs, the inlet and outlet 
concentrations are used with the prior open biological treatment unit 
characterization to estimate the concentrations of HAP in each zone. The 
following information on the open biological treatment unit must be 
available in the second data collection component:
    (1) Basic unit variables such as inlet and recycle wastewater flow 
rates, type of agitation, and operating conditions;

[[Page 382]]

    (2) The value of the inlet and outlet HAP concentrations; and
    (3) The biomass concentration in the open biological treatment unit.

 C. One Time Determination of a Single Value of Ks (Initial Performance 
                                  Test)

    A single value of Ks is calculated using Form 3 for each data set 
that is collected during the initial performance test. A single 
composite value of Ks, deemed to be representative of the biological 
unit, is subsequently selected so that the fbio values 
calculated by the procedures in this appendix (using this single value 
of Ks) for the data sets collected during the initial performance test 
are within 10 percent of the fbio value determined by using 
Form 1 with these same data sets. The value of Ks meeting these criteria 
is obtained by the following steps:
    (1) Determine the median of the Ks values calculated for each data 
set;
    (2) Estimate fbio for each data set using the selected Ks 
value (Form 1 and Form 2);
    (3) Calculate fbio for each data set using Form 1; and
    (4) Compare the fbio values obtained in steps (2) and 
(3); if the fbio value calculated using step (2) differs from 
that calculated using step (3) by more than 10 percent, adjust Ks 
(decrease Ks if the fbio value is lower than that calculated 
by Form 1 and vice versa) and repeat this procedure starting at step 
(2). If a negative value is obtained for the values of Ks, then this 
negative kinetic constant may not be used with the Monod model. If a 
negative value of Ks is obtained, this test procedure cannot be used for 
evaluating the performance of the open biological treatment unit.

      D. Confirmation of Monod Kinetics (Initial Performance Test)

    (1) Confirmation that the unit can be represented by Monod kinetics 
is made by identifying the following two items:
    (i) The zone methanol concentrations measured during the initial 
performance test; and
    (ii) The zone methanol concentrations estimated by the Multiple Zone 
Concentrations Calculations Procedure based on inlet and outlet 
concentrations (Column A of Form 2). For each zone, the concentration in 
item 1 is compared to the concentration in item 2.
    (2) For each zone, the estimated value of item 2 must be:
    (i) Within 25 percent of item 1 when item 1 exceeds 8 mg/L; or
    (ii) Within 2 mg/L of item 1 when item 1 is 8 mg/L or less.
    (3) Successful demonstration that the calculated zone concentrations 
meet these criteria must be achieved for 80 percent of the performance 
test data sets.
    (4) If negative values are obtained for the values of K1 and Ks, 
then these negative kinetic constants may not be used with the Monod 
model, even if the criteria are met. If negative values are obtained, 
this test procedure cannot be used for evaluating the performance of the 
open biological treatment unit.

    E. Determination of KL for Each Zone (Unsafe Sampling Conditions)

    (1) A site-specific liquid-phase mass transfer coefficient (KL) must 
be obtained for each zone during the unsafe sampling conditions. Do not 
use a default value for KL. The KL value for each zone must be based on 
the site-specific parameters of the specific unit. The first step in 
using this procedure is to calculate KL for each zone in the unit using 
Form 4. Form 4 outlines the procedure to follow for using mass transfer 
equations to determine KL. Form 4 identifies the appropriate form to use 
for providing the detailed calculations to support the estimate of the 
value of KL. Forms 5 and 6 are used to provide individual compound 
estimates of KL for quiescent and aerated impoundments, respectively. A 
computer model may be used to perform the calculations. If the WATER8 
model or the most recent update to this model is used, then report the 
computer model input parameters that you used as an attachment to Form 
4. In addition, the Bay Area Sewage Toxics Emission (BASTE) model, 
version 3.0, or equivalent upgrade and the TOXCHEM (Environment Canada's 
Wastewater Technology Centre and Environmega, Ltd.) model, version 1.10, 
or equivalent upgrade may also be used to determine KL for the open 
biological treatment unit with the following stipulations:
    (i) The programs must be altered to output a KL value that is based 
on the site-specific parameters of the unit modeled; and
    (ii) The Henry's law value listed in Form 4 must be substituted for 
the existing Henry's law values in the models.
    (2) The Henry's law value listed in Form 4 may be obtained from the 
following sources:
    (i) Values listed by EPA with temperature adjustment if needed;
    (ii) Measured values for the system of concern with temperature 
adjustment; or
    (iii) Literature values of Henry's law values for methanol, adjusted 
for temperature if needed.
    (3) Input values used in the model and corresponding output values 
shall become part of the documentation of the fbio 
determination. The owner or operator should be aware that these models 
may not provide equivalent KL values for some types of units. To obtain 
an equivalent KL value in this situation, the owner or operator shall 
either use the appropriate procedure on Form 4 or adjust the KL value 
from the model to the equivalent KL value as described on Form 4.

[[Page 383]]

    (4) Report the input parameters that you used in the computer model 
on Forms 5, 6, and 7 as an attachment to Form 4. If you have submerged 
air flow in your unit, you must add the value of KL estimated on Form 7 
to the value of KL obtained with Forms 5 and 6 before using the value of 
KL with Form 2.

    F. Estimation of Zone Concentrations (Unsafe Sampling Conditions)

    Form 2 is used to estimate the zone concentrations of HAP based on 
the inlet and outlet data. The value of Ks entered on the form is that 
single composite value of Ks discussed in section III.C of this 
appendix. This value of Ks is calculated during the Initial Performance 
Test (and subsequently updated, if necessary). A unique value of the 
biorate K1 is entered on line 5 of Form 2, and the inlet concentration 
is estimated in Column A of Form 2. The inlet concentration is located 
in the row of Form 2 corresponding to zone 0. If there are three zones 
in the system, n-3 equals 0 for the inlet concentration row. These 
estimated zone concentrations are then used in Form 1 to estimate f bio 
for the treatment unit.

              G. Quality Control/Quality Assurance (QA/QC)

    A QA/QC plan outlining the procedures used to determine the measured 
inlet and outlet concentrations during unsafe conditions and how the 
zone characterization data were obtained during the initial performance 
test shall be prepared and submitted with the initial performance test 
report. The plan should include, but may not be limited to:
    (1) A description of each of the sampling methods that were used 
(method, procedures, time, method to avoid losses during sampling and 
holding, and sampling procedures) including simplified schematic 
drawings;
    (2) A description of how that biomass was sampled from the 
biotreatment unit, including methods, locations, and times;
    (3) A description of what conditions (DO, temperature, etc.) are 
important, what the target values are in the zones, how the factors were 
controlled, and how they were monitored. These conditions are primarily 
used to establish that the conditions of the initial performance test 
correspond to the conditions of the day in question;
    (4) A description of how each analytical measurement was conducted, 
including preparation of solutions, dilution procedures, sampling 
procedures, monitoring of conditions, etc;
    (5) A description of the analytical instrumentation used, how the 
instruments were calibrated, and a summary of the accuracy and precision 
for each instrument;
    (6) A description of the test methods used to determine HAP 
concentrations and other measurements. Section 63.457(c)(3) specifies 
the test methods that must be used to determine HAP concentrations. 
During unsafe sampling conditions, you do not have to sample over an 
extended period of time or obtain more than one sample at each sample 
point.
    (7) A description of how data are captured, recorded, and stored; 
and
    (8) A description of the equations used and their solutions for 
sampling and analysis, including a reference to any software used for 
calculations and/or curve-fitting.

     IV. Calculation of Individual fbio (Unsafe Sampling Conditions)

    Use Form 1 with your zone concentration information to estimate the 
value of f bio under unsafe sampling conditions. Form 1 uses measured 
concentrations of HAP in the unit inlet and outlet, and Form 1 also uses 
the estimated concentrations in each zone of the unit obtained from Form 
2. This procedure may be used on an open biological treatment unit that 
has defined zones within the unit. Use Form 1 to determine 
fbio for each open biological treatment unit as it exists 
under subpart S of part 63. The first step in using Form 1 is to 
calculate KL for each zone in the unit using Form 4. Form 7 must also be 
used if submerged aeration is used. After KL is determined using field 
data, obtain the concentrations of the HAP in each zone. In this 
alternative procedure for unsafe sampling conditions, the actual 
measured concentrations of the HAP in each zone are replaced with the 
zone concentrations that are estimated with Form 2. After KL and the 
zone concentrations are determined, Form 1 is used to estimate the 
overall unit Fe and fbio for methanol.

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[GRAPHIC] [TIFF OMITTED] TR22DE00.049


[65 FR 80765, Dec. 22, 2000]

[[Page 393]]



                              FINDING AIDS




  --------------------------------------------------------------------

  A list of CFR titles, subtitles, chapters, subchapters and parts and 
an alphabetical list of agencies publishing in the CFR are included in 
the CFR Index and Finding Aids volume to the Code of Federal Regulations 
which is published separately and revised annually.

  Material Approved for Incorporation by Reference
  Table of CFR Titles and Chapters
  Alphabetical List of Agencies Appearing in the CFR
  List of CFR Sections Affected

[[Page 395]]

            Material Approved for Incorporation by Reference

                      (Revised as of July 1, 2004)

  The Director of the Federal Register has approved under 5 U.S.C. 
552(a) and 1 CFR Part 51 the incorporation by reference of the following 
publications. This list contains only those incorporations by reference 
effective as of the revision date of this volume. Incorporations by 
reference found within a regulation are effective upon the effective 
date of that regulation. For more information on incorporation by 
reference, see the preliminary pages of this volume.


40 CFR (63.8980 TO END)

ENVIRONMENTAL PROTECTION AGENCY
                                                                  40 CFR


American Conference of Governmental Industrial Hygienists, Customer 
Service Department

  1330 Kemper Meadow Drive, Cincinnati, Ohio 
  45240-1634


American Society of Mechanical Engineers

  3 Park Avenue, New York, NY 10016-5990; Order 
  inquiries: ASME International, Orders/Inquiries, 
  P.O. Box 2900, Fairfield, New Jersey 07007; 
  Phone: 1-800-843-2763 Also available from Global 
  Engineering Documents, Sales Department, 15 
  Inverness Way East, Englewood, CO 80112
ANSI/ASME PTC 19.10-1981, Flue and Exhaust Gas           63.9307(c)(2); 
  Analyses, Part 10: Instruments and Apparatus.            63.9323(a)(3)


American Society for Testing and Materials

  100 Barr Harbor Drive, West Conshohocken, PA 
  19428-2959; Telephone: (610) 832-9585, FAX: 
  (610) 832-9555
ASTM D 1193-77, Standard Specification for Reagent  Par. 4.1.1 and Par. 
  Water.                                            4.4.2 of Appendix A 
                                                     to Part 63; Method 
                                                     306, Section 7.1.1 
                                                   and 7.4.2 of Appendix 
                                                            A to Part 63
ASTM D 1331-89, Standard Test Methods for Surface  Par. 3.1 and Par. 4.2 
  and Interfacial Tension of Solutions of Surface  of Appendix A to Part 
  Active Agents.                                                      63
ASTM D 5291-02, Standard Test Methods for                Appendix A (to 
  Instrumental Determination of Carbon, Hydrogen,  subpart MMMM of Part 
  and Nitrogen in Petroleum Products and                             63)
  Lubricants.
ASTM D 6053-00, Standard Test Method for           Appendix A to Subpart 
  Determination of Volatile Organic Compounds           MMMM of Part 63)
  (VOC) Content of Electrical Insulating 
  Varnishes.
ASTM D 6522-00, Standard Test Method for               63.9307; Subpart 
  Determination of Nitrogen Oxides, Carbon                 ZZZZ, Table 4
  Monoxide, and Oxygen Concentrations in Emissions 
  from Natural Gas-Fired Reciprocating Engines, 
  Combustion Turbines, Boilers, and Process 
  Heaters Using Portable Analyzers, 2000.

[[Page 397]]



                    Table of CFR Titles and Chapters




                      (Revised as of July 1, 2004)

                      Title 1--General Provisions

         I  Administrative Committee of the Federal Register 
                (Parts 1--49)
        II  Office of the Federal Register (Parts 50--299)
        IV  Miscellaneous Agencies (Parts 400--500)

                    Title 2--Grants and Agreements

            Subtitle A--Office of Management and Budget Guidance 
                for Grants and Agreements
         I  [Reserved]
        II  Office of Management and Budget Circulars and Guidance 
                [Reserved]
            Subtitle B--Federal Agency Regulations for Grants and 
                Agreements [Reserved]


                        Title 3--The President

         I  Executive Office of the President (Parts 100--199)

                           Title 4--Accounts

         I  General Accounting Office (Parts 1--99)

                   Title 5--Administrative Personnel

         I  Office of Personnel Management (Parts 1--1199)
        II  Merit Systems Protection Board (Parts 1200--1299)
       III  Office of Management and Budget (Parts 1300--1399)
         V  The International Organizations Employees Loyalty 
                Board (Parts 1500--1599)
        VI  Federal Retirement Thrift Investment Board (Parts 
                1600--1699)
      VIII  Office of Special Counsel (Parts 1800--1899)
        IX  Appalachian Regional Commission (Parts 1900--1999)
        XI  Armed Forces Retirement Home (Part 2100)
       XIV  Federal Labor Relations Authority, General Counsel of 
                the Federal Labor Relations Authority and Federal 
                Service Impasses Panel (Parts 2400--2499)

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        XV  Office of Administration, Executive Office of the 
                President (Parts 2500--2599)
       XVI  Office of Government Ethics (Parts 2600--2699)
       XXI  Department of the Treasury (Parts 3100--3199)
      XXII  Federal Deposit Insurance Corporation (Part 3201)
     XXIII  Department of Energy (Part 3301)
      XXIV  Federal Energy Regulatory Commission (Part 3401)
       XXV  Department of the Interior (Part 3501)
      XXVI  Department of Defense (Part 3601)
    XXVIII  Department of Justice (Part 3801)
      XXIX  Federal Communications Commission (Parts 3900--3999)
       XXX  Farm Credit System Insurance Corporation (Parts 4000--
                4099)
      XXXI  Farm Credit Administration (Parts 4100--4199)
    XXXIII  Overseas Private Investment Corporation (Part 4301)
      XXXV  Office of Personnel Management (Part 4501)
        XL  Interstate Commerce Commission (Part 5001)
       XLI  Commodity Futures Trading Commission (Part 5101)
      XLII  Department of Labor (Part 5201)
     XLIII  National Science Foundation (Part 5301)
       XLV  Department of Health and Human Services (Part 5501)
      XLVI  Postal Rate Commission (Part 5601)
     XLVII  Federal Trade Commission (Part 5701)
    XLVIII  Nuclear Regulatory Commission (Part 5801)
         L  Department of Transportation (Part 6001)
       LII  Export-Import Bank of the United States (Part 6201)
      LIII  Department of Education (Parts 6300--6399)
       LIV  Environmental Protection Agency (Part 6401)
        LV  National Endowment for the Arts (Part 6501)
       LVI  National Endowment for the Humanities (Part 6601)
      LVII  General Services Administration (Part 6701)
     LVIII  Board of Governors of the Federal Reserve System (Part 
                6801)
       LIX  National Aeronautics and Space Administration (Part 
                6901)
        LX  United States Postal Service (Part 7001)
       LXI  National Labor Relations Board (Part 7101)
      LXII  Equal Employment Opportunity Commission (Part 7201)
     LXIII  Inter-American Foundation (Part 7301)
       LXV  Department of Housing and Urban Development (Part 
                7501)
      LXVI  National Archives and Records Administration (Part 
                7601)
     LXVII  Institute of Museum and Library Services (Part 7701)
      LXIX  Tennessee Valley Authority (Part 7901)
      LXXI  Consumer Product Safety Commission (Part 8101)
    LXXIII  Department of Agriculture (Part 8301)
     LXXIV  Federal Mine Safety and Health Review Commission (Part 
                8401)

[[Page 399]]

     LXXVI  Federal Retirement Thrift Investment Board (Part 8601)
    LXXVII  Office of Management and Budget (Part 8701)

                      Title 6--Homeland Security

         I  Department of Homeland Security, Office of the 
                Secretary (Parts 0--99)

                         Title 7--Agriculture

            Subtitle A--Office of the Secretary of Agriculture 
                (Parts 0--26)
            Subtitle B--Regulations of the Department of 
                Agriculture
         I  Agricultural Marketing Service (Standards, 
                Inspections, Marketing Practices), Department of 
                Agriculture (Parts 27--209)
        II  Food and Nutrition Service, Department of Agriculture 
                (Parts 210--299)
       III  Animal and Plant Health Inspection Service, Department 
                of Agriculture (Parts 300--399)
        IV  Federal Crop Insurance Corporation, Department of 
                Agriculture (Parts 400--499)
         V  Agricultural Research Service, Department of 
                Agriculture (Parts 500--599)
        VI  Natural Resources Conservation Service, Department of 
                Agriculture (Parts 600--699)
       VII  Farm Service Agency, Department of Agriculture (Parts 
                700--799)
      VIII  Grain Inspection, Packers and Stockyards 
                Administration (Federal Grain Inspection Service), 
                Department of Agriculture (Parts 800--899)
        IX  Agricultural Marketing Service (Marketing Agreements 
                and Orders; Fruits, Vegetables, Nuts), Department 
                of Agriculture (Parts 900--999)
         X  Agricultural Marketing Service (Marketing Agreements 
                and Orders; Milk), Department of Agriculture 
                (Parts 1000--1199)
        XI  Agricultural Marketing Service (Marketing Agreements 
                and Orders; Miscellaneous Commodities), Department 
                of Agriculture (Parts 1200--1299)
       XIV  Commodity Credit Corporation, Department of 
                Agriculture (Parts 1400--1499)
        XV  Foreign Agricultural Service, Department of 
                Agriculture (Parts 1500--1599)
       XVI  Rural Telephone Bank, Department of Agriculture (Parts 
                1600--1699)
      XVII  Rural Utilities Service, Department of Agriculture 
                (Parts 1700--1799)
     XVIII  Rural Housing Service, Rural Business-Cooperative 
                Service, Rural Utilities Service, and Farm Service 
                Agency, Department of Agriculture (Parts 1800--
                2099)
        XX  Local Television Loan Guarantee Board (Parts 2200--
                2299)

[[Page 400]]

      XXVI  Office of Inspector General, Department of Agriculture 
                (Parts 2600--2699)
     XXVII  Office of Information Resources Management, Department 
                of Agriculture (Parts 2700--2799)
    XXVIII  Office of Operations, Department of Agriculture (Parts 
                2800--2899)
      XXIX  Office of Energy, Department of Agriculture (Parts 
                2900--2999)
       XXX  Office of the Chief Financial Officer, Department of 
                Agriculture (Parts 3000--3099)
      XXXI  Office of Environmental Quality, Department of 
                Agriculture (Parts 3100--3199)
     XXXII  Office of Procurement and Property Management, 
                Department of Agriculture (Parts 3200--3299)
    XXXIII  Office of Transportation, Department of Agriculture 
                (Parts 3300--3399)
     XXXIV  Cooperative State Research, Education, and Extension 
                Service, Department of Agriculture (Parts 3400--
                3499)
      XXXV  Rural Housing Service, Department of Agriculture 
                (Parts 3500--3599)
     XXXVI  National Agricultural Statistics Service, Department 
                of Agriculture (Parts 3600--3699)
    XXXVII  Economic Research Service, Department of Agriculture 
                (Parts 3700--3799)
   XXXVIII  World Agricultural Outlook Board, Department of 
                Agriculture (Parts 3800--3899)
       XLI  [Reserved]
      XLII  Rural Business-Cooperative Service and Rural Utilities 
                Service, Department of Agriculture (Parts 4200--
                4299)

                    Title 8--Aliens and Nationality

         I  Department of Homeland Security (Immigration and 
                Naturalization) (Parts 1--499)
         V  Executive Office for Immigration Review, Department of 
                Justice (Parts 1000--1399)

                 Title 9--Animals and Animal Products

         I  Animal and Plant Health Inspection Service, Department 
                of Agriculture (Parts 1--199)
        II  Grain Inspection, Packers and Stockyards 
                Administration (Packers and Stockyards Programs), 
                Department of Agriculture (Parts 200--299)
       III  Food Safety and Inspection Service, Department of 
                Agriculture (Parts 300--599)

                           Title 10--Energy

         I  Nuclear Regulatory Commission (Parts 0--199)
        II  Department of Energy (Parts 200--699)

[[Page 401]]

       III  Department of Energy (Parts 700--999)
         X  Department of Energy (General Provisions) (Parts 
                1000--1099)
      XVII  Defense Nuclear Facilities Safety Board (Parts 1700--
                1799)
     XVIII  Northeast Interstate Low-Level Radioactive Waste 
                Commission (Part 1800)

                      Title 11--Federal Elections

         I  Federal Election Commission (Parts 1--9099)

                      Title 12--Banks and Banking

         I  Comptroller of the Currency, Department of the 
                Treasury (Parts 1--199)
        II  Federal Reserve System (Parts 200--299)
       III  Federal Deposit Insurance Corporation (Parts 300--399)
        IV  Export-Import Bank of the United States (Parts 400--
                499)
         V  Office of Thrift Supervision, Department of the 
                Treasury (Parts 500--599)
        VI  Farm Credit Administration (Parts 600--699)
       VII  National Credit Union Administration (Parts 700--799)
      VIII  Federal Financing Bank (Parts 800--899)
        IX  Federal Housing Finance Board (Parts 900--999)
        XI  Federal Financial Institutions Examination Council 
                (Parts 1100--1199)
       XIV  Farm Credit System Insurance Corporation (Parts 1400--
                1499)
        XV  Department of the Treasury (Parts 1500--1599)
      XVII  Office of Federal Housing Enterprise Oversight, 
                Department of Housing and Urban Development (Parts 
                1700--1799)
     XVIII  Community Development Financial Institutions Fund, 
                Department of the Treasury (Parts 1800--1899)

               Title 13--Business Credit and Assistance

         I  Small Business Administration (Parts 1--199)
       III  Economic Development Administration, Department of 
                Commerce (Parts 300--399)
        IV  Emergency Steel Guarantee Loan Board, Department of 
                Commerce (Parts 400--499)
         V  Emergency Oil and Gas Guaranteed Loan Board, 
                Department of Commerce (Parts 500--599)

                    Title 14--Aeronautics and Space

         I  Federal Aviation Administration, Department of 
                Transportation (Parts 1--199)
        II  Office of the Secretary, Department of Transportation 
                (Aviation Proceedings) (Parts 200--399)

[[Page 402]]

       III  Commercial Space Transportation, Federal Aviation 
                Administration, Department of Transportation 
                (Parts 400--499)
         V  National Aeronautics and Space Administration (Parts 
                1200--1299)
        VI  Air Transportation System Stabilization (Parts 1300--
                1399)

                 Title 15--Commerce and Foreign Trade

            Subtitle A--Office of the Secretary of Commerce (Parts 
                0--29)
            Subtitle B--Regulations Relating to Commerce and 
                Foreign Trade
         I  Bureau of the Census, Department of Commerce (Parts 
                30--199)
        II  National Institute of Standards and Technology, 
                Department of Commerce (Parts 200--299)
       III  International Trade Administration, Department of 
                Commerce (Parts 300--399)
        IV  Foreign-Trade Zones Board, Department of Commerce 
                (Parts 400--499)
       VII  Bureau of Industry and Security, Department of 
                Commerce (Parts 700--799)
      VIII  Bureau of Economic Analysis, Department of Commerce 
                (Parts 800--899)
        IX  National Oceanic and Atmospheric Administration, 
                Department of Commerce (Parts 900--999)
        XI  Technology Administration, Department of Commerce 
                (Parts 1100--1199)
      XIII  East-West Foreign Trade Board (Parts 1300--1399)
       XIV  Minority Business Development Agency (Parts 1400--
                1499)
            Subtitle C--Regulations Relating to Foreign Trade 
                Agreements
        XX  Office of the United States Trade Representative 
                (Parts 2000--2099)
            Subtitle D--Regulations Relating to Telecommunications 
                and Information
     XXIII  National Telecommunications and Information 
                Administration, Department of Commerce (Parts 
                2300--2399)

                    Title 16--Commercial Practices

         I  Federal Trade Commission (Parts 0--999)
        II  Consumer Product Safety Commission (Parts 1000--1799)

             Title 17--Commodity and Securities Exchanges

         I  Commodity Futures Trading Commission (Parts 1--199)
        II  Securities and Exchange Commission (Parts 200--399)
        IV  Department of the Treasury (Parts 400--499)

[[Page 403]]

          Title 18--Conservation of Power and Water Resources

         I  Federal Energy Regulatory Commission, Department of 
                Energy (Parts 1--399)
       III  Delaware River Basin Commission (Parts 400--499)
        VI  Water Resources Council (Parts 700--799)
      VIII  Susquehanna River Basin Commission (Parts 800--899)
      XIII  Tennessee Valley Authority (Parts 1300--1399)

                       Title 19--Customs Duties

         I  Bureau of Customs and Border Protection, Department of 
                Homeland Security; Department of the Treasury 
                (Parts 0--199)
        II  United States International Trade Commission (Parts 
                200--299)
       III  International Trade Administration, Department of 
                Commerce (Parts 300--399)
        IV  Bureau of Immigration and Customs Enforcement, 
                Department of Homeland Security (Parts 400--599)

                     Title 20--Employees' Benefits

         I  Office of Workers' Compensation Programs, Department 
                of Labor (Parts 1--199)
        II  Railroad Retirement Board (Parts 200--399)
       III  Social Security Administration (Parts 400--499)
        IV  Employees Compensation Appeals Board, Department of 
                Labor (Parts 500--599)
         V  Employment and Training Administration, Department of 
                Labor (Parts 600--699)
        VI  Employment Standards Administration, Department of 
                Labor (Parts 700--799)
       VII  Benefits Review Board, Department of Labor (Parts 
                800--899)
      VIII  Joint Board for the Enrollment of Actuaries (Parts 
                900--999)
        IX  Office of the Assistant Secretary for Veterans' 
                Employment and Training, Department of Labor 
                (Parts 1000--1099)

                       Title 21--Food and Drugs

         I  Food and Drug Administration, Department of Health and 
                Human Services (Parts 1--1299)
        II  Drug Enforcement Administration, Department of Justice 
                (Parts 1300--1399)
       III  Office of National Drug Control Policy (Parts 1400--
                1499)

                      Title 22--Foreign Relations

         I  Department of State (Parts 1--199)
        II  Agency for International Development (Parts 200--299)
       III  Peace Corps (Parts 300--399)

[[Page 404]]

        IV  International Joint Commission, United States and 
                Canada (Parts 400--499)
         V  Broadcasting Board of Governors (Parts 500--599)
       VII  Overseas Private Investment Corporation (Parts 700--
                799)
        IX  Foreign Service Grievance Board Regulations (Parts 
                900--999)
         X  Inter-American Foundation (Parts 1000--1099)
        XI  International Boundary and Water Commission, United 
                States and Mexico, United States Section (Parts 
                1100--1199)
       XII  United States International Development Cooperation 
                Agency (Parts 1200--1299)
       XIV  Foreign Service Labor Relations Board; Federal Labor 
                Relations Authority; General Counsel of the 
                Federal Labor Relations Authority; and the Foreign 
                Service Impasse Disputes Panel (Parts 1400--1499)
        XV  African Development Foundation (Parts 1500--1599)
       XVI  Japan-United States Friendship Commission (Parts 
                1600--1699)
      XVII  United States Institute of Peace (Parts 1700--1799)

                          Title 23--Highways

         I  Federal Highway Administration, Department of 
                Transportation (Parts 1--999)
        II  National Highway Traffic Safety Administration and 
                Federal Highway Administration, Department of 
                Transportation (Parts 1200--1299)
       III  National Highway Traffic Safety Administration, 
                Department of Transportation (Parts 1300--1399)

                Title 24--Housing and Urban Development

            Subtitle A--Office of the Secretary, Department of 
                Housing and Urban Development (Parts 0--99)
            Subtitle B--Regulations Relating to Housing and Urban 
                Development
         I  Office of Assistant Secretary for Equal Opportunity, 
                Department of Housing and Urban Development (Parts 
                100--199)
        II  Office of Assistant Secretary for Housing-Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Parts 200--299)
       III  Government National Mortgage Association, Department 
                of Housing and Urban Development (Parts 300--399)
        IV  Office of Housing and Office of Multifamily Housing 
                Assistance Restructuring, Department of Housing 
                and Urban Development (Parts 400--499)
         V  Office of Assistant Secretary for Community Planning 
                and Development, Department of Housing and Urban 
                Development (Parts 500--599)
        VI  Office of Assistant Secretary for Community Planning 
                and Development, Department of Housing and Urban 
                Development (Parts 600--699) [Reserved]

[[Page 405]]

       VII  Office of the Secretary, Department of Housing and 
                Urban Development (Housing Assistance Programs and 
                Public and Indian Housing Programs) (Parts 700--
                799)
      VIII  Office of the Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Section 8 Housing Assistance 
                Programs, Section 202 Direct Loan Program, Section 
                202 Supportive Housing for the Elderly Program and 
                Section 811 Supportive Housing for Persons With 
                Disabilities Program) (Parts 800--899)
        IX  Office of Assistant Secretary for Public and Indian 
                Housing, Department of Housing and Urban 
                Development (Parts 900--1699)
         X  Office of Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Interstate Land Sales 
                Registration Program) (Parts 1700--1799)
       XII  Office of Inspector General, Department of Housing and 
                Urban Development (Parts 2000--2099)
        XX  Office of Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Parts 3200--3899)
       XXV  Neighborhood Reinvestment Corporation (Parts 4100--
                4199)

                           Title 25--Indians

         I  Bureau of Indian Affairs, Department of the Interior 
                (Parts 1--299)
        II  Indian Arts and Crafts Board, Department of the 
                Interior (Parts 300--399)
       III  National Indian Gaming Commission, Department of the 
                Interior (Parts 500--599)
        IV  Office of Navajo and Hopi Indian Relocation (Parts 
                700--799)
         V  Bureau of Indian Affairs, Department of the Interior, 
                and Indian Health Service, Department of Health 
                and Human Services (Part 900)
        VI  Office of the Assistant Secretary-Indian Affairs, 
                Department of the Interior (Parts 1000--1199)
       VII  Office of the Special Trustee for American Indians, 
                Department of the Interior (Part 1200)

                      Title 26--Internal Revenue

         I  Internal Revenue Service, Department of the Treasury 
                (Parts 1--899)

           Title 27--Alcohol, Tobacco Products and Firearms

         I  Alcohol and Tobacco Tax and Trade Bureau, Department 
                of the Treasury (Parts 1--399)
        II  Bureau of Alcohol, Tobacco, Firearms, and Explosives, 
                Department of Justice (Parts 400--699)

[[Page 406]]

                   Title 28--Judicial Administration

         I  Department of Justice (Parts 0--299)
       III  Federal Prison Industries, Inc., Department of Justice 
                (Parts 300--399)
         V  Bureau of Prisons, Department of Justice (Parts 500--
                599)
        VI  Offices of Independent Counsel, Department of Justice 
                (Parts 600--699)
       VII  Office of Independent Counsel (Parts 700--799)
      VIII  Court Services and Offender Supervision Agency for the 
                District of Columbia (Parts 800--899)
        IX  National Crime Prevention and Privacy Compact Council 
                (Parts 900--999)
        XI  Department of Justice and Department of State (Parts 
                1100--1199)

                            Title 29--Labor

            Subtitle A--Office of the Secretary of Labor (Parts 
                0--99)
            Subtitle B--Regulations Relating to Labor
         I  National Labor Relations Board (Parts 100--199)
        II  Office of Labor-Management Standards, Department of 
                Labor (Parts 200--299)
       III  National Railroad Adjustment Board (Parts 300--399)
        IV  Office of Labor-Management Standards, Department of 
                Labor (Parts 400--499)
         V  Wage and Hour Division, Department of Labor (Parts 
                500--899)
        IX  Construction Industry Collective Bargaining Commission 
                (Parts 900--999)
         X  National Mediation Board (Parts 1200--1299)
       XII  Federal Mediation and Conciliation Service (Parts 
                1400--1499)
       XIV  Equal Employment Opportunity Commission (Parts 1600--
                1699)
      XVII  Occupational Safety and Health Administration, 
                Department of Labor (Parts 1900--1999)
        XX  Occupational Safety and Health Review Commission 
                (Parts 2200--2499)
       XXV  Employee Benefits Security Administration, Department 
                of Labor (Parts 2500--2599)
     XXVII  Federal Mine Safety and Health Review Commission 
                (Parts 2700--2799)
        XL  Pension Benefit Guaranty Corporation (Parts 4000--
                4999)

                      Title 30--Mineral Resources

         I  Mine Safety and Health Administration, Department of 
                Labor (Parts 1--199)
        II  Minerals Management Service, Department of the 
                Interior (Parts 200--299)
       III  Board of Surface Mining and Reclamation Appeals, 
                Department of the Interior (Parts 300--399)

[[Page 407]]

        IV  Geological Survey, Department of the Interior (Parts 
                400--499)
       VII  Office of Surface Mining Reclamation and Enforcement, 
                Department of the Interior (Parts 700--999)

                 Title 31--Money and Finance: Treasury

            Subtitle A--Office of the Secretary of the Treasury 
                (Parts 0--50)
            Subtitle B--Regulations Relating to Money and Finance
         I  Monetary Offices, Department of the Treasury (Parts 
                51--199)
        II  Fiscal Service, Department of the Treasury (Parts 
                200--399)
        IV  Secret Service, Department of the Treasury (Parts 
                400--499)
         V  Office of Foreign Assets Control, Department of the 
                Treasury (Parts 500--599)
        VI  Bureau of Engraving and Printing, Department of the 
                Treasury (Parts 600--699)
       VII  Federal Law Enforcement Training Center, Department of 
                the Treasury (Parts 700--799)
      VIII  Office of International Investment, Department of the 
                Treasury (Parts 800--899)
        IX  Federal Claims Collection Standards (Department of the 
                Treasury--Department of Justice) (Parts 900--999)

                      Title 32--National Defense

            Subtitle A--Department of Defense
         I  Office of the Secretary of Defense (Parts 1--399)
         V  Department of the Army (Parts 400--699)
        VI  Department of the Navy (Parts 700--799)
       VII  Department of the Air Force (Parts 800--1099)
            Subtitle B--Other Regulations Relating to National 
                Defense
       XII  Defense Logistics Agency (Parts 1200--1299)
       XVI  Selective Service System (Parts 1600--1699)
     XVIII  National Counterintelligence Center (Parts 1800--1899)
       XIX  Central Intelligence Agency (Parts 1900--1999)
        XX  Information Security Oversight Office, National 
                Archives and Records Administration (Parts 2000--
                2099)
       XXI  National Security Council (Parts 2100--2199)
      XXIV  Office of Science and Technology Policy (Parts 2400--
                2499)
     XXVII  Office for Micronesian Status Negotiations (Parts 
                2700--2799)
    XXVIII  Office of the Vice President of the United States 
                (Parts 2800--2899)

               Title 33--Navigation and Navigable Waters

         I  Coast Guard, Department of Homeland Security (Parts 
                1--199)
        II  Corps of Engineers, Department of the Army (Parts 
                200--399)

[[Page 408]]

        IV  Saint Lawrence Seaway Development Corporation, 
                Department of Transportation (Parts 400--499)

                          Title 34--Education

            Subtitle A--Office of the Secretary, Department of 
                Education (Parts 1--99)
            Subtitle B--Regulations of the Offices of the 
                Department of Education
         I  Office for Civil Rights, Department of Education 
                (Parts 100--199)
        II  Office of Elementary and Secondary Education, 
                Department of Education (Parts 200--299)
       III  Office of Special Education and Rehabilitative 
                Services, Department of Education (Parts 300--399)
        IV  Office of Vocational and Adult Education, Department 
                of Education (Parts 400--499)
         V  Office of Bilingual Education and Minority Languages 
                Affairs, Department of Education (Parts 500--599)
        VI  Office of Postsecondary Education, Department of 
                Education (Parts 600--699)
        XI  National Institute for Literacy (Parts 1100--1199)
            Subtitle C--Regulations Relating to Education
       XII  National Council on Disability (Parts 1200--1299)

                        Title 35--Panama Canal

         I  Panama Canal Regulations (Parts 1--299)

             Title 36--Parks, Forests, and Public Property

         I  National Park Service, Department of the Interior 
                (Parts 1--199)
        II  Forest Service, Department of Agriculture (Parts 200--
                299)
       III  Corps of Engineers, Department of the Army (Parts 
                300--399)
        IV  American Battle Monuments Commission (Parts 400--499)
         V  Smithsonian Institution (Parts 500--599)
       VII  Library of Congress (Parts 700--799)
      VIII  Advisory Council on Historic Preservation (Parts 800--
                899)
        IX  Pennsylvania Avenue Development Corporation (Parts 
                900--999)
         X  Presidio Trust (Parts 1000--1099)
        XI  Architectural and Transportation Barriers Compliance 
                Board (Parts 1100--1199)
       XII  National Archives and Records Administration (Parts 
                1200--1299)
        XV  Oklahoma City National Memorial Trust (Part 1501)
       XVI  Morris K. Udall Scholarship and Excellence in National 
                Environmental Policy Foundation (Parts 1600--1699)

[[Page 409]]

             Title 37--Patents, Trademarks, and Copyrights

         I  United States Patent and Trademark Office, Department 
                of Commerce (Parts 1--199)
        II  Copyright Office, Library of Congress (Parts 200--299)
        IV  Assistant Secretary for Technology Policy, Department 
                of Commerce (Parts 400--499)
         V  Under Secretary for Technology, Department of Commerce 
                (Parts 500--599)

           Title 38--Pensions, Bonuses, and Veterans' Relief

         I  Department of Veterans Affairs (Parts 0--99)

                       Title 39--Postal Service

         I  United States Postal Service (Parts 1--999)
       III  Postal Rate Commission (Parts 3000--3099)

                  Title 40--Protection of Environment

         I  Environmental Protection Agency (Parts 1--1099)
        IV  Environmental Protection Agency and Department of 
                Justice (Parts 1400--1499)
         V  Council on Environmental Quality (Parts 1500--1599)
        VI  Chemical Safety and Hazard Investigation Board (Parts 
                1600--1699)
       VII  Environmental Protection Agency and Department of 
                Defense; Uniform National Discharge Standards for 
                Vessels of the Armed Forces (Parts 1700--1799)

          Title 41--Public Contracts and Property Management

            Subtitle B--Other Provisions Relating to Public 
                Contracts
        50  Public Contracts, Department of Labor (Parts 50-1--50-
                999)
        51  Committee for Purchase From People Who Are Blind or 
                Severely Disabled (Parts 51-1--51-99)
        60  Office of Federal Contract Compliance Programs, Equal 
                Employment Opportunity, Department of Labor (Parts 
                60-1--60-999)
        61  Office of the Assistant Secretary for Veterans' 
                Employment and Training Service, Department of 
                Labor (Parts 61-1--61-999)
            Subtitle C--Federal Property Management Regulations 
                System
       101  Federal Property Management Regulations (Parts 101-1--
                101-99)
       102  Federal Management Regulation (Parts 102-1--102-299)
       105  General Services Administration (Parts 105-1--105-999)
       109  Department of Energy Property Management Regulations 
                (Parts 109-1--109-99)
       114  Department of the Interior (Parts 114-1--114-99)
       115  Environmental Protection Agency (Parts 115-1--115-99)

[[Page 410]]

       128  Department of Justice (Parts 128-1--128-99)
            Subtitle D--Other Provisions Relating to Property 
                Management [Reserved]
            Subtitle E--Federal Information Resources Management 
                Regulations System
       201  Federal Information Resources Management Regulation 
                (Parts 201-1--201-99) [Reserved]
            Subtitle F--Federal Travel Regulation System
       300  General (Parts 300-1--300-99)
       301  Temporary Duty (TDY) Travel Allowances (Parts 301-1--
                301-99)
       302  Relocation Allowances (Parts 302-1--302-99)
       303  Payment of Expenses Connected with the Death of 
                Certain Employees (Part 303-70)
       304  Payment of Travel Expenses from a Non-Federal Source 
                (Parts 304-1--304-99)

                        Title 42--Public Health

         I  Public Health Service, Department of Health and Human 
                Services (Parts 1--199)
        IV  Centers for Medicare & Medicaid Services, Department 
                of Health and Human Services (Parts 400--499)
         V  Office of Inspector General-Health Care, Department of 
                Health and Human Services (Parts 1000--1999)

                   Title 43--Public Lands: Interior

            Subtitle A--Office of the Secretary of the Interior 
                (Parts 1--199)
            Subtitle B--Regulations Relating to Public Lands
         I  Bureau of Reclamation, Department of the Interior 
                (Parts 200--499)
        II  Bureau of Land Management, Department of the Interior 
                (Parts 1000--9999)
       III  Utah Reclamation Mitigation and Conservation 
                Commission (Parts 10000--10010)

             Title 44--Emergency Management and Assistance

         I  Federal Emergency Management Agency, Department of 
                Homeland Security (Parts 0--399)
        IV  Department of Commerce and Department of 
                Transportation (Parts 400--499)

                       Title 45--Public Welfare

            Subtitle A--Department of Health and Human Services 
                (Parts 1--199)
            Subtitle B--Regulations Relating to Public Welfare

[[Page 411]]

        II  Office of Family Assistance (Assistance Programs), 
                Administration for Children and Families, 
                Department of Health and Human Services (Parts 
                200--299)
       III  Office of Child Support Enforcement (Child Support 
                Enforcement Program), Administration for Children 
                and Families, Department of Health and Human 
                Services (Parts 300--399)
        IV  Office of Refugee Resettlement, Administration for 
                Children and Families, Department of Health and 
                Human Services (Parts 400--499)
         V  Foreign Claims Settlement Commission of the United 
                States, Department of Justice (Parts 500--599)
        VI  National Science Foundation (Parts 600--699)
       VII  Commission on Civil Rights (Parts 700--799)
      VIII  Office of Personnel Management (Parts 800--899)
         X  Office of Community Services, Administration for 
                Children and Families, Department of Health and 
                Human Services (Parts 1000--1099)
        XI  National Foundation on the Arts and the Humanities 
                (Parts 1100--1199)
       XII  Corporation for National and Community Service (Parts 
                1200--1299)
      XIII  Office of Human Development Services, Department of 
                Health and Human Services (Parts 1300--1399)
       XVI  Legal Services Corporation (Parts 1600--1699)
      XVII  National Commission on Libraries and Information 
                Science (Parts 1700--1799)
     XVIII  Harry S. Truman Scholarship Foundation (Parts 1800--
                1899)
       XXI  Commission on Fine Arts (Parts 2100--2199)
     XXIII  Arctic Research Commission (Part 2301)
      XXIV  James Madison Memorial Fellowship Foundation (Parts 
                2400--2499)
       XXV  Corporation for National and Community Service (Parts 
                2500--2599)

                          Title 46--Shipping

         I  Coast Guard, Department of Homeland Security (Parts 
                1--199)
        II  Maritime Administration, Department of Transportation 
                (Parts 200--399)
       III  Coast Guard (Great Lakes Pilotage), Department of 
                Homeland Security (Parts 400--499)
        IV  Federal Maritime Commission (Parts 500--599)

                      Title 47--Telecommunication

         I  Federal Communications Commission (Parts 0--199)
        II  Office of Science and Technology Policy and National 
                Security Council (Parts 200--299)

[[Page 412]]

       III  National Telecommunications and Information 
                Administration, Department of Commerce (Parts 
                300--399)

           Title 48--Federal Acquisition Regulations System

         1  Federal Acquisition Regulation (Parts 1--99)
         2  Department of Defense (Parts 200--299)
         3  Department of Health and Human Services (Parts 300--
                399)
         4  Department of Agriculture (Parts 400--499)
         5  General Services Administration (Parts 500--599)
         6  Department of State (Parts 600--699)
         7  United States Agency for International Development 
                (Parts 700--799)
         8  Department of Veterans Affairs (Parts 800--899)
         9  Department of Energy (Parts 900--999)
        10  Department of the Treasury (Parts 1000--1099)
        12  Department of Transportation (Parts 1200--1299)
        13  Department of Commerce (Parts 1300--1399)
        14  Department of the Interior (Parts 1400--1499)
        15  Environmental Protection Agency (Parts 1500--1599)
        16  Office of Personnel Management, Federal Employees 
                Health Benefits Acquisition Regulation (Parts 
                1600--1699)
        17  Office of Personnel Management (Parts 1700--1799)
        18  National Aeronautics and Space Administration (Parts 
                1800--1899)
        19  Broadcasting Board of Governors (Parts 1900--1999)
        20  Nuclear Regulatory Commission (Parts 2000--2099)
        21  Office of Personnel Management, Federal Employees 
                Group Life Insurance Federal Acquisition 
                Regulation (Parts 2100--2199)
        23  Social Security Administration (Parts 2300--2399)
        24  Department of Housing and Urban Development (Parts 
                2400--2499)
        25  National Science Foundation (Parts 2500--2599)
        28  Department of Justice (Parts 2800--2899)
        29  Department of Labor (Parts 2900--2999)
        30  Department of Homeland Security, Homeland Security 
                Acquisition Regulation (HSAR) (Parts 3000--3099)
        34  Department of Education Acquisition Regulation (Parts 
                3400--3499)
        35  Panama Canal Commission (Parts 3500--3599)
        44  Federal Emergency Management Agency (Parts 4400--4499)
        51  Department of the Army Acquisition Regulations (Parts 
                5100--5199)
        52  Department of the Navy Acquisition Regulations (Parts 
                5200--5299)
        53  Department of the Air Force Federal Acquisition 
                Regulation Supplement (Parts 5300--5399)

[[Page 413]]

        54  Defense Logistics Agency, Department of Defense (Parts 
                5400--5499)
        57  African Development Foundation (Parts 5700--5799)
        61  General Services Administration Board of Contract 
                Appeals (Parts 6100--6199)
        63  Department of Transportation Board of Contract Appeals 
                (Parts 6300--6399)
        99  Cost Accounting Standards Board, Office of Federal 
                Procurement Policy, Office of Management and 
                Budget (Parts 9900--9999)

                       Title 49--Transportation

            Subtitle A--Office of the Secretary of Transportation 
                (Parts 1--99)
            Subtitle B--Other Regulations Relating to 
                Transportation
         I  Research and Special Programs Administration, 
                Department of Transportation (Parts 100--199)
        II  Federal Railroad Administration, Department of 
                Transportation (Parts 200--299)
       III  Federal Motor Carrier Safety Administration, 
                Department of Transportation (Parts 300--399)
        IV  Coast Guard, Department of Homeland Security (Parts 
                400--499)
         V  National Highway Traffic Safety Administration, 
                Department of Transportation (Parts 500--599)
        VI  Federal Transit Administration, Department of 
                Transportation (Parts 600--699)
       VII  National Railroad Passenger Corporation (AMTRAK) 
                (Parts 700--799)
      VIII  National Transportation Safety Board (Parts 800--999)
         X  Surface Transportation Board, Department of 
                Transportation (Parts 1000--1399)
        XI  Bureau of Transportation Statistics, Department of 
                Transportation (Parts 1400--1499)
       XII  Transportation Security Administration, Department of 
                Homeland Security (Parts 1500--1599)

                   Title 50--Wildlife and Fisheries

         I  United States Fish and Wildlife Service, Department of 
                the Interior (Parts 1--199)
        II  National Marine Fisheries Service, National Oceanic 
                and Atmospheric Administration, Department of 
                Commerce (Parts 200--299)
       III  International Fishing and Related Activities (Parts 
                300--399)
        IV  Joint Regulations (United States Fish and Wildlife 
                Service, Department of the Interior and National 
                Marine Fisheries Service, National Oceanic and 
                Atmospheric Administration, Department of 
                Commerce); Endangered Species Committee 
                Regulations (Parts 400--499)

[[Page 414]]

         V  Marine Mammal Commission (Parts 500--599)
        VI  Fishery Conservation and Management, National Oceanic 
                and Atmospheric Administration, Department of 
                Commerce (Parts 600--699)

                      CFR Index and Finding Aids

            Subject/Agency Index
            List of Agency Prepared Indexes
            Parallel Tables of Statutory Authorities and Rules
            List of CFR Titles, Chapters, Subchapters, and Parts
            Alphabetical List of Agencies Appearing in the CFR

[[Page 415]]





           Alphabetical List of Agencies Appearing in the CFR




                      (Revised as of July 1, 2004)

                                                  CFR Title, Subtitle or 
                     Agency                               Chapter

Administrative Committee of the Federal Register  1, I
Advanced Research Projects Agency                 32, I
Advisory Council on Historic Preservation         36, VIII
African Development Foundation                    22, XV
  Federal Acquisition Regulation                  48, 57
Agency for International Development, United      22, II
     States
  Federal Acquisition Regulation                  48, 7
Agricultural Marketing Service                    7, I, IX, X, XI
Agricultural Research Service                     7, V
Agriculture Department                            5, LXXIII
  Agricultural Marketing Service                  7, I, IX, X, XI
  Agricultural Research Service                   7, V
  Animal and Plant Health Inspection Service      7, III; 9, I
  Chief Financial Officer, Office of              7, XXX
  Commodity Credit Corporation                    7, XIV
  Cooperative State Research, Education, and      7, XXXIV
       Extension Service
  Economic Research Service                       7, XXXVII
  Energy, Office of                               7, XXIX
  Environmental Quality, Office of                7, XXXI
  Farm Service Agency                             7, VII, XVIII
  Federal Acquisition Regulation                  48, 4
  Federal Crop Insurance Corporation              7, IV
  Food and Nutrition Service                      7, II
  Food Safety and Inspection Service              9, III
  Foreign Agricultural Service                    7, XV
  Forest Service                                  36, II
  Grain Inspection, Packers and Stockyards        7, VIII; 9, II
       Administration
  Information Resources Management, Office of     7, XXVII
  Inspector General, Office of                    7, XXVI
  National Agricultural Library                   7, XLI
  National Agricultural Statistics Service        7, XXXVI
  Natural Resources Conservation Service          7, VI
  Operations, Office of                           7, XXVIII
  Procurement and Property Management, Office of  7, XXXII
  Rural Business-Cooperative Service              7, XVIII, XLII
  Rural Development Administration                7, XLII
  Rural Housing Service                           7, XVIII, XXXV
  Rural Telephone Bank                            7, XVI
  Rural Utilities Service                         7, XVII, XVIII, XLII
  Secretary of Agriculture, Office of             7, Subtitle A
  Transportation, Office of                       7, XXXIII
  World Agricultural Outlook Board                7, XXXVIII
Air Force Department                              32, VII
  Federal Acquisition Regulation Supplement       48, 53
Air Transportation Stabilization Board            14, VI
Alcohol and Tobacco Tax and Trade Bureau          27, I
Alcohol, Tobacco, Firearms, and Explosives,       27, II
     Bureau of
AMTRAK                                            49, VII
American Battle Monuments Commission              36, IV
American Indians, Office of the Special Trustee   25, VII
Animal and Plant Health Inspection Service        7, III; 9, I
Appalachian Regional Commission                   5, IX

[[Page 416]]

Architectural and Transportation Barriers         36, XI
     Compliance Board
Arctic Research Commission                        45, XXIII
Armed Forces Retirement Home                      5, XI
Army Department                                   32, V
  Engineers, Corps of                             33, II; 36, III
  Federal Acquisition Regulation                  48, 51
Benefits Review Board                             20, VII
Bilingual Education and Minority Languages        34, V
     Affairs, Office of
Blind or Severely Disabled, Committee for         41, 51
     Purchase From People Who Are
Broadcasting Board of Governors                   22, V
  Federal Acquisition Regulation                  48, 19
Census Bureau                                     15, I
Centers for Medicare & Medicaid Services          42, IV
Central Intelligence Agency                       32, XIX
Chief Financial Officer, Office of                7, XXX
Child Support Enforcement, Office of              45, III
Children and Families, Administration for         45, II, III, IV, X
Civil Rights, Commission on                       45, VII
Civil Rights, Office for                          34, I
Coast Guard                                       33, I; 46, I; 49, IV
Coast Guard (Great Lakes Pilotage)                46, III
Commerce Department                               44, IV
  Census Bureau                                   15, I
  Economic Affairs, Under Secretary               37, V
  Economic Analysis, Bureau of                    15, VIII
  Economic Development Administration             13, III
  Emergency Management and Assistance             44, IV
  Federal Acquisition Regulation                  48, 13
  Fishery Conservation and Management             50, VI
  Foreign-Trade Zones Board                       15, IV
  Industry and Security, Bureau of                15, VII
  International Trade Administration              15, III; 19, III
  National Institute of Standards and Technology  15, II
  National Marine Fisheries Service               50, II, IV, VI
  National Oceanic and Atmospheric                15, IX; 50, II, III, IV, 
       Administration                             VI
  National Telecommunications and Information     15, XXIII; 47, III
       Administration
  National Weather Service                        15, IX
  Patent and Trademark Office, United States      37, I
  Productivity, Technology and Innovation,        37, IV
       Assistant Secretary for
  Secretary of Commerce, Office of                15, Subtitle A
  Technology, Under Secretary for                 37, V
  Technology Administration                       15, XI
  Technology Policy, Assistant Secretary for      37, IV
Commercial Space Transportation                   14, III
Commodity Credit Corporation                      7, XIV
Commodity Futures Trading Commission              5, XLI; 17, I
Community Planning and Development, Office of     24, V, VI
     Assistant Secretary for
Community Services, Office of                     45, X
Comptroller of the Currency                       12, I
Construction Industry Collective Bargaining       29, IX
     Commission
Consumer Product Safety Commission                5, LXXI; 16, II
Cooperative State Research, Education, and        7, XXXIV
     Extension Service
Copyright Office                                  37, II
Corporation for National and Community Service    45, XII, XXV
Cost Accounting Standards Board                   48, 99
Council on Environmental Quality                  40, V
Court Services and Offender Supervision Agency    28, VIII
     for the District of Columbia
Customs and Border Protection Bureau              19, I
Defense Contract Audit Agency                     32, I
Defense Department                                5, XXVI; 32, Subtitle A; 
                                                  40, VII

[[Page 417]]

  Advanced Research Projects Agency               32, I
  Air Force Department                            32, VII
  Army Department                                 32, V; 33, II; 36, III, 
                                                  48, 51
  Defense Intelligence Agency                     32, I
  Defense Logistics Agency                        32, I, XII; 48, 54
  Engineers, Corps of                             33, II; 36, III
  Federal Acquisition Regulation                  48, 2
  National Imagery and Mapping Agency             32, I
  Navy Department                                 32, VI; 48, 52
  Secretary of Defense, Office of                 32, I
Defense Contract Audit Agency                     32, I
Defense Intelligence Agency                       32, I
Defense Logistics Agency                          32, XII; 48, 54
Defense Nuclear Facilities Safety Board           10, XVII
Delaware River Basin Commission                   18, III
District of Columbia, Court Services and          28, VIII
     Offender Supervision Agency for the
Drug Enforcement Administration                   21, II
East-West Foreign Trade Board                     15, XIII
Economic Affairs, Under Secretary                 37, V
Economic Analysis, Bureau of                      15, VIII
Economic Development Administration               13, III
Economic Research Service                         7, XXXVII
Education, Department of                          5, LIII
  Bilingual Education and Minority Languages      34, V
       Affairs, Office of
  Civil Rights, Office for                        34, I
  Educational Research and Improvement, Office    34, VII
       of
  Elementary and Secondary Education, Office of   34, II
  Federal Acquisition Regulation                  48, 34
  Postsecondary Education, Office of              34, VI
  Secretary of Education, Office of               34, Subtitle A
  Special Education and Rehabilitative Services,  34, III
       Office of
  Vocational and Adult Education, Office of       34, IV
Educational Research and Improvement, Office of   34, VII
Elementary and Secondary Education, Office of     34, II
Emergency Oil and Gas Guaranteed Loan Board       13, V
Emergency Steel Guarantee Loan Board              13, IV
Employee Benefits Security Administration         29, XXV
Employees' Compensation Appeals Board             20, IV
Employees Loyalty Board                           5, V
Employment and Training Administration            20, V
Employment Standards Administration               20, VI
Endangered Species Committee                      50, IV
Energy, Department of                             5, XXIII; 10, II, III, X
  Federal Acquisition Regulation                  48, 9
  Federal Energy Regulatory Commission            5, XXIV; 18, I
  Property Management Regulations                 41, 109
Energy, Office of                                 7, XXIX
Engineers, Corps of                               33, II; 36, III
Engraving and Printing, Bureau of                 31, VI
Environmental Protection Agency                   5, LIV; 40, I, IV, VII
  Federal Acquisition Regulation                  48, 15
  Property Management Regulations                 41, 115
Environmental Quality, Office of                  7, XXXI
Equal Employment Opportunity Commission           5, LXII; 29, XIV
Equal Opportunity, Office of Assistant Secretary  24, I
     for
Executive Office of the President                 3, I
  Administration, Office of                       5, XV
  Environmental Quality, Council on               40, V
  Management and Budget, Office of                5, III, LXXVII; 14, VI; 
                                                  48, 99
  National Drug Control Policy, Office of         21, III
  National Security Council                       32, XXI; 47, 2
  Presidential Documents                          3
  Science and Technology Policy, Office of        32, XXIV; 47, II

[[Page 418]]

  Trade Representative, Office of the United      15, XX
       States
Export-Import Bank of the United States           5, LII; 12, IV
Family Assistance, Office of                      45, II
Farm Credit Administration                        5, XXXI; 12, VI
Farm Credit System Insurance Corporation          5, XXX; 12, XIV
Farm Service Agency                               7, VII, XVIII
Federal Acquisition Regulation                    48, 1
Federal Aviation Administration                   14, I
  Commercial Space Transportation                 14, III
Federal Claims Collection Standards               31, IX
Federal Communications Commission                 5, XXIX; 47, I
Federal Contract Compliance Programs, Office of   41, 60
Federal Crop Insurance Corporation                7, IV
Federal Deposit Insurance Corporation             5, XXII; 12, III
Federal Election Commission                       11, I
Federal Emergency Management Agency               44, I
  Federal Acquisition Regulation                  48, 44
Federal Employees Group Life Insurance Federal    48, 21
     Acquisition Regulation
Federal Employees Health Benefits Acquisition     48, 16
     Regulation
Federal Energy Regulatory Commission              5, XXIV; 18, I
Federal Financial Institutions Examination        12, XI
     Council
Federal Financing Bank                            12, VIII
Federal Highway Administration                    23, I, II
Federal Home Loan Mortgage Corporation            1, IV
Federal Housing Enterprise Oversight Office       12, XVII
Federal Housing Finance Board                     12, IX
Federal Labor Relations Authority, and General    5, XIV; 22, XIV
     Counsel of the Federal Labor Relations 
     Authority
Federal Law Enforcement Training Center           31, VII
Federal Management Regulation                     41, 102
Federal Maritime Commission                       46, IV
Federal Mediation and Conciliation Service        29, XII
Federal Mine Safety and Health Review Commission  5, LXXIV; 29, XXVII
Federal Motor Carrier Safety Administration       49, III
Federal Prison Industries, Inc.                   28, III
Federal Procurement Policy Office                 48, 99
Federal Property Management Regulations           41, 101
Federal Railroad Administration                   49, II
Federal Register, Administrative Committee of     1, I
Federal Register, Office of                       1, II
Federal Reserve System                            12, II
  Board of Governors                              5, LVIII
Federal Retirement Thrift Investment Board        5, VI, LXXVI
Federal Service Impasses Panel                    5, XIV
Federal Trade Commission                          5, XLVII; 16, I
Federal Transit Administration                    49, VI
Federal Travel Regulation System                  41, Subtitle F
Fine Arts, Commission on                          45, XXI
Fiscal Service                                    31, II
Fish and Wildlife Service, United States          50, I, IV
Fishery Conservation and Management               50, VI
Food and Drug Administration                      21, I
Food and Nutrition Service                        7, II
Food Safety and Inspection Service                9, III
Foreign Agricultural Service                      7, XV
Foreign Assets Control, Office of                 31, V
Foreign Claims Settlement Commission of the       45, V
     United States
Foreign Service Grievance Board                   22, IX
Foreign Service Impasse Disputes Panel            22, XIV
Foreign Service Labor Relations Board             22, XIV
Foreign-Trade Zones Board                         15, IV
Forest Service                                    36, II
General Accounting Office                         4, I
General Services Administration                   5, LVII; 41, 105
  Contract Appeals, Board of                      48, 61
  Federal Acquisition Regulation                  48, 5

[[Page 419]]

  Federal Management Regulation                   41, 102
  Federal Property Management Regulations         41, 101
  Federal Travel Regulation System                41, Subtitle F
  General                                         41, 300
  Payment From a Non-Federal Source for Travel    41, 304
       Expenses
  Payment of Expenses Connected With the Death    41, 303
       of Certain Employees
  Relocation Allowances                           41, 302
  Temporary Duty (TDY) Travel Allowances          41, 301
Geological Survey                                 30, IV
Government Ethics, Office of                      5, XVI
Government National Mortgage Association          24, III
Grain Inspection, Packers and Stockyards          7, VIII; 9, II
     Administration
Harry S. Truman Scholarship Foundation            45, XVIII
Health and Human Services, Department of          5, XLV; 45, Subtitle A
  Centers for Medicare & Medicaid Services        42, IV
  Child Support Enforcement, Office of            45, III
  Children and Families, Administration for       45, II, III, IV, X
  Community Services, Office of                   45, X
  Family Assistance, Office of                    45, II
  Federal Acquisition Regulation                  48, 3
  Food and Drug Administration                    21, I
  Human Development Services, Office of           45, XIII
  Indian Health Service                           25, V; 42, I
  Inspector General (Health Care), Office of      42, V
  Public Health Service                           42, I
  Refugee Resettlement, Office of                 45, IV
Homeland Security, Department of                  6, I
  Coast Guard                                     33, I; 46, I; 49, IV
  Coast Guard (Great Lakes Pilotage)              46, III
  Customs and Border Protection Bureau            19, I
  Federal Emergency Management Agency             44, I
  Immigration and Customs Enforcement Bureau      19, IV
  Immigration and Naturalization                  8, I
  Transportation Security Administration          49, XII
Housing and Urban Development, Department of      5, LXV; 24, Subtitle B
  Community Planning and Development, Office of   24, V, VI
       Assistant Secretary for
  Equal Opportunity, Office of Assistant          24, I
       Secretary for
  Federal Acquisition Regulation                  48, 24
  Federal Housing Enterprise Oversight, Office    12, XVII
       of
  Government National Mortgage Association        24, III
  Housing--Federal Housing Commissioner, Office   24, II, VIII, X, XX
       of Assistant Secretary for
  Housing, Office of, and Multifamily Housing     24, IV
       Assistance Restructuring, Office of
  Inspector General, Office of                    24, XII
  Public and Indian Housing, Office of Assistant  24, IX
       Secretary for
  Secretary, Office of                            24, Subtitle A, VII
Housing--Federal Housing Commissioner, Office of  24, II, VIII, X, XX
     Assistant Secretary for
Housing, Office of, and Multifamily Housing       24, IV
     Assistance Restructuring, Office of
Human Development Services, Office of             45, XIII
Immigration and Customs Enforcement Bureau        19, IV
Immigration and Naturalization                    8, I
Immigration Review, Executive Office for          8, V
Independent Counsel, Office of                    28, VII
Indian Affairs, Bureau of                         25, I, V
Indian Affairs, Office of the Assistant           25, VI
     Secretary
Indian Arts and Crafts Board                      25, II
Indian Health Service                             25, V; 42, I
Industry and Security, Bureau of                  15, VII
Information Resources Management, Office of       7, XXVII
Information Security Oversight Office, National   32, XX
     Archives and Records Administration
Inspector General

[[Page 420]]

  Agriculture Department                          7, XXVI
  Health and Human Services Department            42, V
  Housing and Urban Development Department        24, XII
Institute of Peace, United States                 22, XVII
Inter-American Foundation                         5, LXIII; 22, X
Interior Department
  American Indians, Office of the Special         25, VII
       Trustee
  Endangered Species Committee                    50, IV
  Federal Acquisition Regulation                  48, 14
  Federal Property Management Regulations System  41, 114
  Fish and Wildlife Service, United States        50, I, IV
  Geological Survey                               30, IV
  Indian Affairs, Bureau of                       25, I, V
  Indian Affairs, Office of the Assistant         25, VI
       Secretary
  Indian Arts and Crafts Board                    25, II
  Land Management, Bureau of                      43, II
  Minerals Management Service                     30, II
  National Indian Gaming Commission               25, III
  National Park Service                           36, I
  Reclamation, Bureau of                          43, I
  Secretary of the Interior, Office of            43, Subtitle A
  Surface Mining and Reclamation Appeals, Board   30, III
       of
  Surface Mining Reclamation and Enforcement,     30, VII
       Office of
Internal Revenue Service                          26, I
International Boundary and Water Commission,      22, XI
     United States and Mexico, United States 
     Section
International Development, United States Agency   22, II
     for
  Federal Acquisition Regulation                  48, 7
International Development Cooperation Agency,     22, XII
     United States
International Fishing and Related Activities      50, III
International Investment, Office of               31, VIII
International Joint Commission, United States     22, IV
     and Canada
International Organizations Employees Loyalty     5, V
     Board
International Trade Administration                15, III; 19, III
International Trade Commission, United States     19, II
Interstate Commerce Commission                    5, XL
James Madison Memorial Fellowship Foundation      45, XXIV
Japan-United States Friendship Commission         22, XVI
Joint Board for the Enrollment of Actuaries       20, VIII
Justice Department                                5, XXVIII; 28, I, XI; 40, 
                                                  IV
  Alcohol, Tobacco, Firearms, and Explosives,     27, II
       Bureau of
  Drug Enforcement Administration                 21, II
  Federal Acquisition Regulation                  48, 28
  Federal Claims Collection Standards             31, IX
  Federal Prison Industries, Inc.                 28, III
  Foreign Claims Settlement Commission of the     45, V
       United States
  Immigration Review, Executive Office for        8, V
  Offices of Independent Counsel                  28, VI
  Prisons, Bureau of                              28, V
  Property Management Regulations                 41, 128
Labor Department                                  5, XLII
  Benefits Review Board                           20, VII
  Employee Benefits Security Administration       29, XXV
  Employees' Compensation Appeals Board           20, IV
  Employment and Training Administration          20, V
  Employment Standards Administration             20, VI
  Federal Acquisition Regulation                  48, 29
  Federal Contract Compliance Programs, Office    41, 60
       of
  Federal Procurement Regulations System          41, 50
  Labor-Management Standards, Office of           29, II, IV
  Mine Safety and Health Administration           30, I
  Occupational Safety and Health Administration   29, XVII
  Public Contracts                                41, 50
  Secretary of Labor, Office of                   29, Subtitle A

[[Page 421]]

  Veterans' Employment and Training Service,      41, 61; 20, IX
       Office of the Assistant Secretary for
  Wage and Hour Division                          29, V
  Workers' Compensation Programs, Office of       20, I
Labor-Management Standards, Office of             29, II, IV
Land Management, Bureau of                        43, II
Legal Services Corporation                        45, XVI
Library of Congress                               36, VII
  Copyright Office                                37, II
Local Television Loan Guarantee Board             7, XX
Management and Budget, Office of                  5, III, LXXVII; 14, VI; 
                                                  48, 99
Marine Mammal Commission                          50, V
Maritime Administration                           46, II
Merit Systems Protection Board                    5, II
Micronesian Status Negotiations, Office for       32, XXVII
Mine Safety and Health Administration             30, I
Minerals Management Service                       30, II
Minority Business Development Agency              15, XIV
Miscellaneous Agencies                            1, IV
Monetary Offices                                  31, I
Morris K. Udall Scholarship and Excellence in     36, XVI
     National Environmental Policy Foundation
National Aeronautics and Space Administration     5, LIX; 14, V
  Federal Acquisition Regulation                  48, 18
National Agricultural Library                     7, XLI
National Agricultural Statistics Service          7, XXXVI
National and Community Service, Corporation for   45, XII, XXV
National Archives and Records Administration      5, LXVI; 36, XII
  Information Security Oversight Office           32, XX
National Bureau of Standards                      15, II
National Capital Planning Commission              1, IV
National Commission for Employment Policy         1, IV
National Commission on Libraries and Information  45, XVII
     Science
National Council on Disability                    34, XII
National Counterintelligence Center               32, XVIII
National Credit Union Administration              12, VII
National Crime Prevention and Privacy Compact     28, IX
     Council
National Drug Control Policy, Office of           21, III
National Foundation on the Arts and the           45, XI
     Humanities
National Highway Traffic Safety Administration    23, II, III; 49, V
National Imagery and Mapping Agency               32, I
National Indian Gaming Commission                 25, III
National Institute for Literacy                   34, XI
National Institute of Standards and Technology    15, II
National Labor Relations Board                    5, LXI; 29, I
National Marine Fisheries Service                 50, II, IV, VI
National Mediation Board                          29, X
National Oceanic and Atmospheric Administration   15, IX; 50, II, III, IV, 
                                                  VI
National Park Service                             36, I
National Railroad Adjustment Board                29, III
National Railroad Passenger Corporation (AMTRAK)  49, VII
National Science Foundation                       5, XLIII; 45, VI
  Federal Acquisition Regulation                  48, 25
National Security Council                         32, XXI
National Security Council and Office of Science   47, II
     and Technology Policy
National Telecommunications and Information       15, XXIII; 47, III
     Administration
National Transportation Safety Board              49, VIII
National Weather Service                          15, IX
Natural Resources Conservation Service            7, VI
Navajo and Hopi Indian Relocation, Office of      25, IV
Navy Department                                   32, VI
  Federal Acquisition Regulation                  48, 52
Neighborhood Reinvestment Corporation             24, XXV
Northeast Interstate Low-Level Radioactive Waste  10, XVIII
   Commission
[[Page 422]]

Nuclear Regulatory Commission                     5, XLVIII; 10, I
  Federal Acquisition Regulation                  48, 20
Occupational Safety and Health Administration     29, XVII
Occupational Safety and Health Review Commission  29, XX
Offices of Independent Counsel                    28, VI
Oklahoma City National Memorial Trust             36, XV
Operations Office                                 7, XXVIII
Overseas Private Investment Corporation           5, XXXIII; 22, VII
Panama Canal Commission                           48, 35
Panama Canal Regulations                          35, I
Patent and Trademark Office, United States        37, I
Payment From a Non-Federal Source for Travel      41, 304
     Expenses
Payment of Expenses Connected With the Death of   41, 303
     Certain Employees
Peace Corps                                       22, III
Pennsylvania Avenue Development Corporation       36, IX
Pension Benefit Guaranty Corporation              29, XL
Personnel Management, Office of                   5, I, XXXV; 45, VIII
  Federal Acquisition Regulation                  48, 17
  Federal Employees Group Life Insurance Federal  48, 21
       Acquisition Regulation
  Federal Employees Health Benefits Acquisition   48, 16
       Regulation
Postal Rate Commission                            5, XLVI; 39, III
Postal Service, United States                     5, LX; 39, I
Postsecondary Education, Office of                34, VI
President's Commission on White House             1, IV
     Fellowships
Presidential Documents                            3
Presidio Trust                                    36, X
Prisons, Bureau of                                28, V
Procurement and Property Management, Office of    7, XXXII
Productivity, Technology and Innovation,          37, IV
     Assistant Secretary
Public Contracts, Department of Labor             41, 50
Public and Indian Housing, Office of Assistant    24, IX
     Secretary for
Public Health Service                             42, I
Railroad Retirement Board                         20, II
Reclamation, Bureau of                            43, I
Refugee Resettlement, Office of                   45, IV
Regional Action Planning Commissions              13, V
Relocation Allowances                             41, 302
Research and Special Programs Administration      49, I
Rural Business-Cooperative Service                7, XVIII, XLII
Rural Development Administration                  7, XLII
Rural Housing Service                             7, XVIII, XXXV
Rural Telephone Bank                              7, XVI
Rural Utilities Service                           7, XVII, XVIII, XLII
Saint Lawrence Seaway Development Corporation     33, IV
Science and Technology Policy, Office of          32, XXIV
Science and Technology Policy, Office of, and     47, II
     National Security Council
Secret Service                                    31, IV
Securities and Exchange Commission                17, II
Selective Service System                          32, XVI
Small Business Administration                     13, I
Smithsonian Institution                           36, V
Social Security Administration                    20, III; 48, 23
Soldiers' and Airmen's Home, United States        5, XI
Special Counsel, Office of                        5, VIII
Special Education and Rehabilitative Services,    34, III
     Office of
State Department                                  22, I; 28, XI
  Federal Acquisition Regulation                  48, 6
Surface Mining and Reclamation Appeals, Board of  30, III
Surface Mining Reclamation and Enforcement,       30, VII
     Office of
Surface Transportation Board                      49, X
Susquehanna River Basin Commission                18, VIII
Technology Administration                         15, XI
Technology Policy, Assistant Secretary for        37, IV

[[Page 423]]

Technology, Under Secretary for                   37, V
Tennessee Valley Authority                        5, LXIX; 18, XIII
Thrift Supervision Office, Department of the      12, V
     Treasury
Trade Representative, United States, Office of    15, XX
Transportation, Department of                     5, L
  Commercial Space Transportation                 14, III
  Contract Appeals, Board of                      48, 63
  Emergency Management and Assistance             44, IV
  Federal Acquisition Regulation                  48, 12
  Federal Aviation Administration                 14, I
  Federal Highway Administration                  23, I, II
  Federal Motor Carrier Safety Administration     49, III
  Federal Railroad Administration                 49, II
  Federal Transit Administration                  49, VI
  Maritime Administration                         46, II
  National Highway Traffic Safety Administration  23, II, III; 49, V
  Research and Special Programs Administration    49, I
  Saint Lawrence Seaway Development Corporation   33, IV
  Secretary of Transportation, Office of          14, II; 49, Subtitle A
  Surface Transportation Board                    49, X
  Transportation Statistics Bureau                49, XI
Transportation, Office of                         7, XXXIII
Transportation Security Administration            49, XII
Transportation Statistics Bureau                  49, XI
Travel Allowances, Temporary Duty (TDY)           41, 301
Treasury Department                               5, XXI; 12, XV; 17, IV; 
                                                  31, IX
  Alcohol and Tobacco Tax and Trade Bureau        27, I
  Community Development Financial Institutions    12, XVIII
       Fund
  Comptroller of the Currency                     12, I
  Customs and Border Protection Bureau            19, I
  Engraving and Printing, Bureau of               31, VI
  Federal Acquisition Regulation                  48, 10
  Federal Law Enforcement Training Center         31, VII
  Fiscal Service                                  31, II
  Foreign Assets Control, Office of               31, V
  Internal Revenue Service                        26, I
  International Investment, Office of             31, VIII
  Monetary Offices                                31, I
  Secret Service                                  31, IV
  Secretary of the Treasury, Office of            31, Subtitle A
  Thrift Supervision, Office of                   12, V
Truman, Harry S. Scholarship Foundation           45, XVIII
United States and Canada, International Joint     22, IV
     Commission
United States and Mexico, International Boundary  22, XI
     and Water Commission, United States Section
Utah Reclamation Mitigation and Conservation      43, III
     Commission
Veterans Affairs Department                       38, I
  Federal Acquisition Regulation                  48, 8
Veterans' Employment and Training Service,        41, 61; 20, IX
     Office of the Assistant Secretary for
Vice President of the United States, Office of    32, XXVIII
Vocational and Adult Education, Office of         34, IV
Wage and Hour Division                            29, V
Water Resources Council                           18, VI
Workers' Compensation Programs, Office of         20, I
World Agricultural Outlook Board                  7, XXXVIII

[[Page 425]]



List of CFR Sections Affected



All changes in this volume of the Code of Federal Regulations which were 
made by documents published in the Federal Register since January 1, 
2001, are enumerated in the following list. Entries indicate the nature 
of the changes effected. Page numbers refer to Federal Register pages. 
The user should consult the entries for chapters and parts as well as 
sections for revisions.
Title 40 was established at 36 FR 12213, June 29, 1971. For the period 
before January 1, 2001, see the ``List of CFR Sections Affected, 1964-
1972, 1964-1972, 1973-1985, and 1986--2000'' published in 10 separate 
volumes.

                                  2001

40 CFR
                                                                   66 FR
                                                                    Page
Chapter I
63 Appendix C amended6936.........................................

                                  2002

40 CFR
                                                                   67 FR
                                                                    Page
Chapter I
63.9480--63.9579 (Subpart QQQQQ) Added64506.......................

                                  2003

40 CFR
                                                                   68 FR
                                                                    Page
Chapter I
63.8980--63.9075 (Subpart NNNNN) Added19090.......................
63.9280--63.9375 (Subpart PPPPP) Added28785.......................
    Heading corrected..............................................51830
63.9580--63.9652 (Subpart RRRRR) Added61888.......................
63.9780--63.9824 (Subpart SSSSS) Added18747.......................
63.9880--63.9942 (Subpart TTTTT) Added58620.......................

                                  2004

    (Regulations published from January 1, 2004 through July 1, 2004)

40 CFR
                                                                   69 FR
                                                                    Page
Title 40 Nomenclature change18803.................................


                                  [all]