[Federal Register Volume 85, Number 9 (Tuesday, January 14, 2020)]
[Proposed Rules]
[Pages 2234-2277]
[FR Doc No: 2019-27842]

Vol. 85

Tuesday,

No. 9

January 14, 2020

Part II

Environmental Protection Agency

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40 CFR Parts 60, 63, and 266

EPA Method 23--Determination of Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans From Stationary Sources; Proposed Rule

Federal Register / Vol. 85, No. 9 / Tuesday, January 14, 2020 /
Proposed Rules

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 60, 63, and 266

[EPA-HQ-OAR-2016-0677; FRL-10003-67-OAR]
RIN 2060-AT09

EPA Method 23--Determination of Polychlorinated Dibenzo-p-Dioxins
and Polychlorinated Dibenzofurans From Stationary Sources

AGENCY: Environmental Protection Agency.

ACTION: Proposed rule.

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SUMMARY: This action proposes editorial and technical revisions to the
Environmental Protection Agency's Method 23 (Determination of
Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans
from Stationary Sources). Proposed revisions include incorporating
isotope dilution for quantifying all target compounds and changing the
method quality control from the current prescriptive format to a more
flexible performance-based approach with specified performance
criteria. We are also proposing revisions that will expand the list of
target compounds of Method 23 to include polycyclic aromatic
hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs). The proposed
revisions will improve the accuracy of Method 23 and will provide
flexibility to stack testers and analytical laboratories who measure
semivolatile organic compounds (SVOC) from stationary sources while
ensuring that the stack testing community can consistently implement
the method across emissions sources and facilities.

DATES: Comments. Comments must be received on or before March 16, 2020.

ADDRESSES: Comments: Submit your comments, identified by Docket ID No.
EPA-HQ-OAR-2016-0677, at https://www.regulations.gov. Follow the online
instructions for submitting comments. Once submitted, comments cannot
be edited or removed from Regulations.gov. See SUPPLEMENTARY
INFORMATION section for details about how the Environmental Protection
Agency (EPA) treats submitted comments. Regulations.gov is our
preferred method of receiving comments. However, the following other
submission methods are also accepted:
     Email<EMAIL_ADDRESS>Include Docket ID No. EPA-
HQ-OAR-2016-0677 in the subject line of the message.
     Fax:<PHONE_NUMBER>. Attention Docket ID No. EPA-HQ-OAR-
2016-0677.
     Mail: To ship or send mail via the United States Postal
Service, use the following address: U.S. Environmental Protection
Agency, EPA Docket Center, Docket ID No. EPA-HQ-OAR-2016-0677, Mail
Code 28221T, 1200 Pennsylvania Avenue NW, Washington, DC 20460.
     Hand/Courier Delivery: Use the following Docket Center
address if you are using express mail, commercial delivery, hand
delivery, or courier: EPA Docket Center, EPA WJC West Building, Room
3334, 1301 Constitution Avenue NW, Washington, DC 20004. Delivery
verification signatures will be available only during regular business
hours.

FOR FURTHER INFORMATION CONTACT: Dr. Raymond Merrill, Office of Air
Quality Planning and Standards, Air Quality Assessment Division (E143-
02), Environmental Protection Agency, Research Triangle Park, NC 27711;
telephone number:<PHONE_NUMBER>; fax number:<PHONE_NUMBER>; email
address<EMAIL_ADDRESS>
SUPPLEMENTARY INFORMATION:

Public Participation

A. Written Comments

    Submit your comments, identified by Docket ID No. EPA-HQ-OAR-2016-
0677, at https://www.regulations.gov (our preferred method), or the
other methods identified in the ADDRESSES section. Once submitted,
comments cannot be edited or removed from the docket. The EPA may
publish any comment received to its public docket. Do not submit
electronically any information you consider to be Confidential Business
Information (CBI) or other information whose disclosure is restricted
by statute. Multimedia submissions (audio, video, etc.) must be
accompanied by a written comment. The written comment is considered the
official comment and should include discussion of all points you wish
to make. The EPA will generally not consider comments or comment
contents located outside of the primary submission (i.e., on the Web,
cloud, or other file sharing system). For additional submission
methods, the full EPA public comment policy, information about CBI or
multimedia submissions, and general guidance on making effective
comments, please visit https://www.epa.gov/dockets/commenting-epa-dockets.
    Submitting CBI: Clearly mark the part or all of the information
that you claim to be CBI. For CBI information in a disk or CD-ROM that
you mail to the EPA, mark the outside of the disk or CD-ROM as CBI and
then identify electronically within the disk or CD-ROM the specific
information that is claimed as CBI. In addition to one complete version
of the comment that includes information claimed as CBI, a copy of the
comment that does not contain the information claimed as CBI must be
submitted for inclusion in the public docket. Information marked as CBI
will not be disclosed except in accordance with procedures set forth in
Title 40 Code of Federal Regulations (CFR) part 2.
    Do not submit information that you consider to be CBI or otherwise
protected through https://www.regulations.gov or email. Send or deliver
information identified as CBI to only the following address: OAQPS
Document Control Officer (Room C404-02), U.S. EPA, Research Triangle
Park, NC 27711, Attention Docket ID No. EPA-HQ-OAR-2016-0677.
    If you have any questions about CBI or the procedures for claiming
CBI, please consult the person identified in the FOR FURTHER
INFORMATION CONTACT section.
    Docket: All documents in the docket are listed in the https://www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI (Confidential Business
Information) or other information whose disclosure is restricted by
statute. Certain other material, such as copyrighted material, will be
publicly available only in hard copy. Publicly available docket
materials are available either electronically in https://www.regulations.gov or in hard copy at the EPA Docket Center, EPA/DC,
EPA WJC West Building, Room 3334, 1301 Constitution Ave. NW,
Washington, DC. This Docket Facility is open from 8:30 a.m. to 4:30
p.m., Monday through Friday, excluding legal holidays. The telephone
number for the Public Reading Room is<PHONE_NUMBER>, and the telephone
number for the Air Docket is<PHONE_NUMBER>.

B. Participation at Public Hearing

    Public hearing. If a public hearing is requested by January 21,
2020, then we will hold a public hearing at the EPA William Jefferson
Clinton (WJC) East Building, 1201 Constitution Avenue NW, Washington,
DC 20004. If a public hearing is requested, additional details about
the public hearing will be provided in a separate Federal Register
notice and on our website at https://www3.epa.gov/ttn/emc/methods. To
request a hearing, to register to speak at a hearing, or to inquire if
a hearing will be held, please contact Raymond Merrill

by email at<EMAIL_ADDRESS>or phone at<PHONE_NUMBER>. The
last day to pre-register in advance to speak at the public hearing will
be January 27, 2020. If held, the public hearing will convene at 9:00
a.m. (local time) and will conclude at 4:00 p.m. (local time).
    Because this hearing is being held at a U.S. government facility,
individuals planning to attend the hearing should be prepared to show
valid picture identification to the security staff in order to gain
access to the meeting room. Please note that the REAL ID Act, passed by
Congress in 2005, established new requirements for entering federal
facilities. For purposes of the REAL ID Act, EPA will accept
government-issued IDs, including drivers' licenses, from the District
of Columbia and all states and territories except from American Samoa.
If your identification is issued by American Samoa, you must present an
additional form of identification to enter the federal building where
the public hearing will be held. Acceptable alternative forms of
identification include: Federal employee badges, passports, enhanced
driver's licenses, and military identification cards. For additional
information for the status of your state regarding REAL ID, go to:
https://www.dhs.gov/real-id-enforcement-brieffrequently-asked-questions. Any objects brought into the building need to fit through
the security screening system, such as a purse, laptop bag, or small
backpack. Demonstrations will not be allowed on federal property for
security reasons.

Table of Contents

    The following outline is provided to aid in locating information in
this preamble.

I. General Information

A. Does this action apply to me?
B. Where can I get a copy of this document and other related
information?

II. Background

III. Incorporation by Reference

IV. Summary of Proposed Revisions to Method 23

A. Section 1.0
B. Section 2.0
C. Section 3.0
D. Section 4.0
E. Section 5.0
F. Section 6.0
G. Section 7.0
H. Section 8.0
I. Section 9.0
J. Section 10.0
K. Section 11.0
L. Section 12.0
M. Section 13.0
N. Section 14.0
O. Section 15.0
P. Section 16.0
Q. Section 17.0

V. Summary of Proposed Revisions Related to 40 CFR Parts 60, 63, and
266

A. 40 CFR Part 60--Standards of Performance for New Stationary
Sources
B. 40 CFR Part 63--National Emission Standards for Hazardous Air
Pollutants for Source Categories
C. 40 CFR Part 266--Standards for the Management of Specific
Hazardous Wastes and Specific Types of Hazardous Waste Management
Facilities

VI. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review and
Executive Order 13563: Improving Regulation and Regulatory Review
B. Executive Order 13771: Reducing Regulations and Controlling
Regulatory Costs
C. Paperwork Reduction Act (PRA)
D. Regulatory Flexibility Act (RFA)
E. Unfunded Mandates Reform Act (UMRA)
F. Executive Order 13132: Federalism
G. Executive Order 13175: Consultation and Coordination With Indian
Tribal Governments
H. Executive Order 13045: Protection of Children From Environmental
Health Risks and Safety Risks
I. Executive Order 13211: Actions that Significantly Affect Energy
Supply, Distribution, or Use
J. National Technology Transfer and Advancement Act (NTTAA)
K. Executive Order 12898: Federal Actions To Address Environmental
Justice in Minority Populations and Low-Income Populations

I. General Information

A. Does this action apply to me?

    The proposed amendments to Method 23 apply to industries that are
subject to certain provisions of parts 60, 62, 63, 79, and 266. The
source categories and entities potentially affected are listed in Table
1. This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be regulated by this
action. This table lists the types of entities that EPA is now aware
could potentially be affected by this action. Other types of entities
not listed in the table could also be regulated.

             Table 1--Potentially Affected Source Categories
------------------------------------------------------------------------
                                                 Examples of regulated
             Category              NAICSY \a\           entities
------------------------------------------------------------------------
Industry.........................      332410  Fossil fuel steam
                                                generators.
                                       332410  Industrial, commercial,
                                                institutional steam
                                                generating units.
                                       562213  Municipal Waste
                                                Combustors.
                                       322110  Hazardous Waste
                                                Combustors.
                                       325211  Polyvinyl Chloride Resins
                                                Manufacturing.
                                       327310  Portland cement plants.
                                       324122  Asphalt Shingle and
                                                Coating Materials
                                                Manufacturing.
                                       331314  Secondary aluminum
                                                plants.
                                       327120  Clay Building Material
                                                and Refractories
                                                Manufacturing.
                                       331410  Nonferrous Metal (except
                                                Aluminum) Smelting and
                                                Refining.
------------------------------------------------------------------------
\a\ North American Industry Classification System.

    If you have any questions regarding the applicability of the
proposed changes to Method 23, contact the person listed in the
preceding FOR FURTHER INFORMATION CONTACT section.

B. Where can I get a copy of this document and other related
information?

    The docket number for this action is Docket ID No. EPA-HQ-OAR-2016-
0677. In addition to being available in the docket, an electronic copy
of the proposed method revisions is available on the Technology
Transfer Network (TTN) website at https://www3.epa.gov/ttn/emc/methods/. The TTN provides information and technology exchange in
various areas of air pollution control.

II. Background

    The EPA's Method 23 (Determination of Polychlorinated Dibenzo-p-
Dioxins and Polychlorinated Dibenzofurans from Stationary Sources) is
our current reference test method for determination

of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated
dibenzofurans (PCDFs) emitted from stationary sources.
    The EPA promulgated Method 23 (Appendix A of 40 CFR part 60, Test
Methods) on February 13, 1991 (56 FR 5758). Since promulgation, the
measurement of PCDDs and PCDFs has evolved as analytical laboratories,
EPA, and state entities have developed new standard operating
procedures and methods to reflect improvements in sampling and
analytical techniques. Examples of newer PCDD/PCDF methods include:
     Office of Land and Emergency Management (OLEM) Solid Waste
(SW) SW-846 EPA Method 8290A, Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans (PCDFs) by High-Resolution Gas
Chromatography/High-Resolution Mass Spectrometry (HRGC/HRMS);
     Office of Water (OW) EPA Method 1613, Tetra- through Octa-
Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS; and
     California Environmental Protection Agency Air Resources
Board (CARB) Method 428, Determination of Polychlorinated Dibenzo-p-
Dioxin (PCDD), Polychlorinated Dibenzofuran (PCDF), and Polychlorinated
Biphenyls Emissions from Stationary Sources.
    Beginning in 2016, the EPA held a series of informal discussions
with stakeholders in the measurement community to identify technical
issues related to the sampling and analysis of PCDD and PCDF and
potential revisions to Method 23. The stakeholders consisted of a cross
section of interested parties including representatives from state
regulatory entities, various EPA offices, analytical laboratories,
emission testing firms, analytical standards vendors, instrument
vendors, and others with experience in sampling and analysis of PCDD
and PCDF and with the equipment, materials, and performance of Method
23 and other PCDD/PCDF methods. In the discussions, EPA also sought
stakeholder input regarding their experience combining procedures for
sampling and analysis of PCDD and PCDF with procedures for sampling and
analysis of PAHs and PCBs emitted from stationary sources. The docket
contains summaries of the stakeholder discussions.

III. Incorporation by Reference

    The EPA proposes to incorporate by reference ASTM D6911-15 and ASTM
D4840-99(2018)e1 in Method 23. The ASTM D6911-15 includes a guide for
packaging and shipping environmental samples for laboratory analysis
and ASTM D4840-99(2018)e1 includes a standard guide for sample chain-
of-custody procedures. These standards were developed and adopted by
the American society for Testing and Materials and may be obtained from
https://www.astm.org or from the ASTM at 100 Barr Harbor Drive, P.O.
Box C700, West Conshohocken, PA 19428-2959.

IV. Summary of Proposed Revisions to Method 23

    In this action, we are proposing technical revisions and editorial
changes to clarify and update the requirements and procedures specified
in Method 23. We are also proposing to reformat the method to conform
with EPA's current method format (see https://www.epa.gov/measurements-modeling/method-development#format). We are proposing to expand the
applicability of Method 23 to include procedures for sampling and
analyzing PAHs and PCBs. In addition, we are proposing revisions to
various sections of the CFR that either require Method 23 or require
the analysis of PCDDs/PCDFs, PAHs, or PCBs.
    Our intent for the proposed revisions is to ensure that Method 23
is implemented consistently and to update the method procedures to
include performance-based quality requirements that add flexibility
rather than the prescriptive requirements currently described in the
method.
    The primary focus of the proposed revisions to Method 23 is to
change the method from a prescriptive method to a performance-based
method, which will allow users to have flexibility in implementing the
method (e.g., choice of gas chromatograph (GC) column, the procedures
used for sample cleanup) while still meeting performance criteria that
the EPA believes are necessary for demonstrating and documenting the
quality of the measurements for the target compounds. The proposed
revisions also address concerns over recovery of target compounds from
particulate matter by requiring a pre-extraction filter spike recovery
procedure and acceptance criteria for the filter spike recovery. These
new requirements resolve the concerns that led to the criteria in 40
CFR 63.1208 that required Administrator approval prior to use of Method
23 for measurement of PCDDs/PCDFs.
    The EPA's second focus for the proposed revisions is to convert the
method entirely to quantitation based on isotope dilution. These
revisions to the method are possible because additional isotopically
labeled standards for the target compounds have become available from
vendors since the original promulgation of Method 23.
    The third major focus for the EPA's proposed revision to Method 23
is to include options for combining sampling and analysis of PCDDs/
PCDFs with PAHs and PCBs to allow the measurement of toxic SVOC. In
addition, adding PCBs and PAHs to the list of target compounds measured
by Method 23 is responsive to multiple requests for alternative method
approval from facilities and source test teams that are responding to
EPA information collection requests (ICRs).
    The EPA's proposed amendments to Method 23 are presented below for
each section of Method 23.

A. Section 1.0

    In this action, EPA is proposing to rename section 1.0 from
``Applicability and Principle'' to ``Scope and Application,'' and
revise the text to expand the target compounds for Method 23 to include
PCBs and PAHs. We are also proposing to add statements that emphasize
the need for working knowledge of the EPA Methods 1 through 5 of
appendices A-1, A-2, and A-3 to 40 CFR part 60, and the use of high-
resolution gas chromatography/high-resolution mass spectrometry (HRGC/
HRMS) when applying Method 23. We are also proposing language to
specify that Method 23 is performance-based and to allow users to
modify parts of the method to overcome interferences or to substitute
alternative materials and equipment provided that all performance
criteria in the method are met.

B. Section 2.0

    The EPA is proposing to rename section 2.0 from ``Apparatus'' to
``Summary of Method,'' and revise section 2.0 with language to provide
an overview of the method's sampling and analytical procedures. We are
also proposing to move the current language in section 2.0, which
describes the materials needed to conduct Method 23, to a proposed new
section 6.0.

C. Section 3.0

    The current version of Method 23 does not include definitions of
key terms and variables used in Method 23. In this action, we are
proposing to add a new section 3.0 titled ``Definitions,'' absent in
the current promulgated version of Method 23. We are providing
definitions to acronyms and technical terms to improve the clarity of
the method principles and procedures. We also propose to move language
from the

current section 3.0 to a proposed new section 7.0.

D. Section 4.0

    The current version of Method 23 does not discuss the conditions
that can potentially interfere with measurements obtained when using
the method. In this action, we are proposing to add a new section 4.0
titled ``Interferences,'' that would present the potential causes and
recommendations for avoiding or mitigating interferences or sample
contamination. We also propose to move language from the current
section 4.0 to a proposed new section 8.0.

E. Section 5.0

    Currently, Method 23 does not provide procedures for safety. In
this action, we are proposing to add a new section 5.0 titled
``Safety,'' that would present the health hazards and procedures for
minimizing risks to field and laboratory personnel when conducting
Method 23. We also propose to move language from the current section
5.0 to a proposed new section 11.0.

F. Section 6.0

    In this action, we are proposing to renumber and move the text in
section 2.0 (Apparatus) of the current method to section 6.0 titled
``Equipment and Supplies,'' and to make clarifying edits and technical
revisions to the specifications in this section. Table 2 of this
preamble identifies the proposed new numbering for the subsections
currently in section 2.0 and Table 3 of this preamble identifies new
specifications (and the associated subsection) we are proposing to
include in section 6.0.

  Table 2--Crosswalk for Proposed Revisions to Current Method Sections
------------------------------------------------------------------------
            Description              Current section    Proposed section
------------------------------------------------------------------------
Filter holder.....................              2.1.1              6.1.3
Condenser.........................              2.1.2              6.1.7
Water circulating bath............              2.1.3              6.1.8
Absorbent module..................              2.1.4              6.1.9
Fitting cap.......................              2.2.1              6.2.1
Wash bottles......................              2.2.2              6.2.2
Filter storage container..........              2.2.4              6.2.4
Field balance.....................              2.2.5              6.2.5
Aluminum foil.....................              2.2.6              6.2.6
Glass sample storage containers...              2.2.9              6.2.8
Extraction thimble................              2.3.4            <IP_ADDRESS>
Pasteur pipette...................              2.3.5              6.4.1
GC oven...........................           <IP_ADDRESS>            <IP_ADDRESS>
Temperature monitor for GC oven...           <IP_ADDRESS>            <IP_ADDRESS>
GC Flow system....................           <IP_ADDRESS>            <IP_ADDRESS>
Capillary column..................           <IP_ADDRESS>              6.5.2
Mass spectrometer.................             2.3.11              6.5.3
Mass spectrometer data system.....             2.3.12              6.5.4
------------------------------------------------------------------------

       Table 3--Proposed Additional Specifications for Section 6.0
------------------------------------------------------------------------
                     Description                        Proposed section
------------------------------------------------------------------------
Probe liner..........................................              6.1.2
Filter heating system................................              6.1.4
Filter temperature sensor............................              6.1.5
Sample transfer line.................................              6.1.6
Impingers............................................             6.1.10
Soxhlet extraction apparatus.........................            <IP_ADDRESS>
Moisture trap of extraction apparatus................            <IP_ADDRESS>
Kuderna-Danish concentrator..........................              6.3.4
Heating mantle.......................................            <IP_ADDRESS>
Chromatography column................................              6.4.2
Injection port.......................................            <IP_ADDRESS>
PCDD/PCDF column system..............................            <IP_ADDRESS>
PAH column system....................................            <IP_ADDRESS>
PCB column system....................................            <IP_ADDRESS>
------------------------------------------------------------------------

    In this section, we are also proposing to:
     Prohibit the use of brominated flame-retardant coated tape
in assembling the sampling train to avoid sample contamination;
     Revise the specification for a rotary evaporator with
specifications for a Kuderna-Danish concentrator to avoid the loss of
higher vapor pressure target compounds;
     Remove specifications for the graduated cylinder to
improve the accuracy of moisture measurements and to make Method 23
more consistent with other isokinetic sampling methods; and
     Remove the volume requirement for wash bottles to allow
greater flexibility in field sample recovery.
    We are also proposing to move language from Method 23's current
section 6.0 to a proposed new section 10.0.

G. Section 7.0

    In this action, the EPA is proposing to renumber and move the text
in section 3.0 (Reagents) of the current method to a new section 7.0
titled ``Reagents, Media and Standards,'' and to make clarifying edits
and technical revisions to the specifications in this section. Table 4
of this preamble identifies the

proposed new numbering for the subsections currently in section 3.0 and
Table 5 of this preamble identifies new specifications (and the
associated subsection) we are proposing to include in section 7.

  Table 4--Crosswalk for Proposed Revisions to Current Method Sections
------------------------------------------------------------------------
            Description              Current section    Proposed section
------------------------------------------------------------------------
Filter............................              3.1.1                7.1
Adsorbent resin...................              3.1.2                7.2
Glass wool........................              3.1.3                7.3
Water.............................              3.1.4                7.4
Methylene chloride................              3.2.2                7.6
Sodium sulfate....................              3.3.2              7.8.2
Basic alumina.....................             3.3.13          <IP_ADDRESS>.2
Silica gel........................             3.3.14            <IP_ADDRESS>
Carbon/Celite[supreg].............             3.3.17            <IP_ADDRESS>
Nitrogen..........................             3.3.18             7.8.10
------------------------------------------------------------------------

       Table 5--Proposed Additional Specifications for Section 7.0
------------------------------------------------------------------------
                     Description                        Proposed section
------------------------------------------------------------------------
High-boiling alkanes used as keeper solvents.........              7.8.8
Liquid column packing materials......................              7.8.9
Acidic alumina.......................................          <IP_ADDRESS>.1
Florisil[supreg].....................................            <IP_ADDRESS>
Helium...............................................              7.9.1
Spiking standards....................................              7.9.2
Pre-sampling recovery standard solution..............              7.9.3
Filter recovery spike standard solution..............              7.9.4
Pre-extraction recovery standard solution............              7.9.5
Pre-analysis recovery standard solution..............              7.9.6
------------------------------------------------------------------------

    We are proposing to replace the filter precleaning procedures of
the current method with specifications for conducting a filter quality
control check. We are proposing to delete unnecessary specifications
presented in Table 6 to reflect modern methods. We are also proposing
to rename the isotopic spiking standard mixtures to simple English
names that relate the standards to their use in the proposed method.

  Table 6--Proposed Deletions of Material Specifications in the Current
                                Method 23
------------------------------------------------------------------------
                       Material                         Current section
------------------------------------------------------------------------
Chromic acid cleaning solution.......................              3.1.6
Benzene..............................................              3.3.7
Ethyl acetate........................................              3.3.8
Nonane...............................................             3.3.11
Cyclohexane..........................................             3.3.12
Hydrogen.............................................             3.3.19
Internal standard solution...........................             3.3.20
Surrogate standard solution..........................             3.3.21
Recovery standard solution...........................             3.3.22
------------------------------------------------------------------------

    We are also proposing to move the current section 7.0 to a proposed
new section 9.0.

H. Section 8.0

    In this action, the EPA is proposing to renumber and move the text
in section 4.0 (Procedure) of the current method to a new section 8.0
titled ``Sample Collection, Preservation and Storage,'' and to make
clarifying edits and technical revisions to the current procedures for
sampling and sample recovery. As proposed, the new section 8 also would
include added requirements for sample storage conditions and holding
times.
    Under the sampling procedures of Method 23, we are proposing
revisions to the current requirements in section 4.1.1 for pretest
preparations. Table 7 of this preamble identifies the new numbering to
revise and replace the requirements in section 4.1.

  Table 7--Crosswalk for Proposed Revisions to Current Method Sections
------------------------------------------------------------------------
            Description              Current section    Proposed section
------------------------------------------------------------------------
Glassware cleaning................            <IP_ADDRESS>            <IP_ADDRESS>
Assembling the adsorbent module...            <IP_ADDRESS>            <IP_ADDRESS>
Maintaining the sampling train                <IP_ADDRESS>            <IP_ADDRESS>
 components.......................
Silica Gel........................            <IP_ADDRESS>            <IP_ADDRESS>

Checking and packing filters......            <IP_ADDRESS>            <IP_ADDRESS>
Field preparation of the sampling             <IP_ADDRESS>            <IP_ADDRESS>
 train............................
Impinger assembly.................            <IP_ADDRESS>            <IP_ADDRESS>
Sampling probe and nozzle                     <IP_ADDRESS>            <IP_ADDRESS>
 preparation......................
------------------------------------------------------------------------

    Table 8 of this preamble shows the specifications we are proposing
to add to the new section 8.0. We are proposing a minimum sample volume
to assure that stack testers can attain the detection limits consistent
with current regulations. Sampling time requirements at each traverse
point for continuous industrial processes align Method 23 with other
isokinetic stationary source methods, such as Method 5. The sampling
time at each traverse point for batch industrial processes ensure
measurements are made for the entire process cycle. The proposed filter
check requirements add details that were absent from the original
Method 23 and align the method with the requirements of other
isokinetic stationary source methods, such as Methods 5, 26A, and 29,
also in Appendix A of this part. The proposed absorbent module
orientation requirements clarify the configuration of the absorbent
module to ensure that condensed moisture flows through the module into
the water collection impinger. We are proposing to add filter
monitoring requirements to align Method 23 with other isokinetic
stationary source methods. Also, we are proposing to add adsorbent
module temperature monitoring to confirm that the sorbent material was
not exposed to elevated temperatures that could bias sample collection
and results.

       Table 8--Proposed Additional Specifications for Section 8.1
------------------------------------------------------------------------
                     Description                        Proposed section
------------------------------------------------------------------------
Minimum sample volume................................            <IP_ADDRESS>
Sampling time for continuous processes...............            <IP_ADDRESS>
Sampling time for batch processes....................            <IP_ADDRESS>
Filter assembly......................................            <IP_ADDRESS>
Orientation of the condenser and adsorbent module....            <IP_ADDRESS>
Monitoring the filter temperature....................            <IP_ADDRESS>
Monitoring the adsorbent module temperature..........            <IP_ADDRESS>
------------------------------------------------------------------------

    Under sample recovery procedures, we are proposing technical
revisions as shown in Table 9 of this preamble. In this action, we are
also proposing to add a recommendation to use clean glassware and to
add specifications as shown in Table 10 of this preamble.

  Table 9--Crosswalk for Proposed Revisions to Current Method Sections
------------------------------------------------------------------------
            Description              Current section    Proposed section
------------------------------------------------------------------------
Adsorbent module sample                         4.2.2              8.2.5
 preparation......................
Preparation of Container No. 2....            <IP_ADDRESS>              8.2.6
Rinsing of the filter holder and              <IP_ADDRESS>              8.2.7
 condenser........................
Weighing impinger water...........            <IP_ADDRESS>              8.2.8
Preparation of Container No. 3....            <IP_ADDRESS>              8.2.9
Silica gel........................            <IP_ADDRESS>             8.2.10
------------------------------------------------------------------------

      Table 10--Proposed Additional Specifications for Section 8.2
------------------------------------------------------------------------
                     Description                        Proposed section
------------------------------------------------------------------------
Conducting a post-test leak check....................              8.2.1
Storage conditions for Container No. 1...............              8.2.4
Field sample handling, storage, and transport........             8.2.11
Sample chain of custody..............................             8.2.12
------------------------------------------------------------------------

    In new section 8.2.8, we propose to measure moisture by weight
rather than by volume.

I. Section 9.0

    In this action, the EPA is proposing to move and renumber the
current section 7.0 (Quality Control) to a new section 9.0 titled
``Quality Control,'' and to make clarifying and technical revisions to
the section. We are proposing to add an introductory note that
addresses maintaining and documenting quality control compliance
required in Method 23. We would add a new subsection that clarifies the
recordkeeping and reporting necessary to demonstrate compliance with
quality control requirements of this method. We are also proposing to
add specifications for conducting pre-sampling, pre-extraction, and
pre-analysis spike recoveries of isotopically-labeled standards and to
add specifications for:
     Capillary gas chromatography columns;

     Preparing and analyzing batch blanks;
     Determining the method detection limit; and
     Assessing field train proof blanks.
    We are also proposing to move language from the current section 9.0
to a proposed new section 12.0.

J. Section 10.0

    In this action, the EPA is proposing to renumber and move the text
in section 6.0 (Calibration) of the current method to a new section
10.0 titled ``Calibration and Standardization,'' and to make clarifying
and technical revisions to the specifications for calibrating the
sampling and the HRGC/HRMS systems. We are proposing to add
specifications for tuning the HRGC/HRMS system, to move the
specification for HRMS resolution (currently in section 5) to this
proposed section, to add procedures for assessing the relative standard
deviation for the mean instrument response, and to add procedures for
determining the signal-to-noise ratio of the MS to bring Method 23 up
to date with current laboratory practice. We are also proposing to add
requirements for ion abundance ratio limits, initial calibrations, and
resolution checks under the daily performance check to serve as
performance indicators for analysis quality. We are also proposing to
move language in the current section 10.0 to a proposed new section
16.0.

K. Section 11.0

    In this action, the EPA is proposing to renumber and move the text
in section 5.0 (Analysis) of the current method to a new section 11.0
titled ``Analysis Procedure,'' and to make clarifying and technical
revisions to the current specifications for sample extraction and
sample cleanup and fractionation. We are also proposing to add a new
subsection describing how sample extract aliquots are prepared for
cleanup and analysis.
    We are also proposing to add the specifications and recommendations
for analysis procedures shown in Table 11 of this preamble.

      Table 11--Proposed Additional Specifications for Section 11.0
------------------------------------------------------------------------
                Description                        Proposed section
------------------------------------------------------------------------
Preparing and operating the extraction       11.1.7 through 11.1.9.
 apparatus.
Cooling the extraction apparatus...........  11.2.1.
Performing an initial extract concentration  11.2.2.
Cooling the sample extract.................  11.2.3.
Recommended minimum volume for PCDD/PCDF     11.2.3.
 analysis.
Further concentration of sample (if needed)  11.2.4.
 for cleanup and analysis.
Sample cleanup and fractionation for PAHs    11.3.1.
 and PCDEs.
Sample cleanup and fractionation for PCDD/   11.3.2.
 DFs and PCBs.
Addressing unresolved compounds............  <IP_ADDRESS>.1.
Retention time for PCBs....................  <IP_ADDRESS>.5.
Chlorodiphenyl ether interference of PCDD/   <IP_ADDRESS>.8.
 DFs.
MS lock channels...........................  <IP_ADDRESS>.9.
Calculations of target mass and mass per     <IP_ADDRESS>.1 and <IP_ADDRESS>.2.
 dry standard cubic meter.
Quantifying indigenous PCDD/DFs............  <IP_ADDRESS>.3.
Reporting options compound concentrations..  <IP_ADDRESS>.4 through
                                              <IP_ADDRESS>.6.
Identification criteria for PAHs...........  <IP_ADDRESS>.10.
------------------------------------------------------------------------

L. Section 12.0

    In this action, the EPA is proposing to renumber and move the text
in section 9.0 (Calculations) of the current method to a new section
12.0 titled ``Data Analysis and Calculations,'' and to revise the
equation variable list. We are proposing to revise the equations shown
in Table 12 of this preamble to incorporate isotope dilution
calculations.

         Table 12--Proposed Equation Revisions for Section 12.0
------------------------------------------------------------------------
       Current equation              Description        Proposed section
------------------------------------------------------------------------
23-2..........................  Average relative                    12.3
                                 response factor
                                 (RRF) for each
                                 compound.
23-6..........................  Concentration of                    12.7
                                 individual target
                                 compound i in the
                                 extract by isotope
                                 dilution.
23-9..........................  Recovery of Labeled                12.10
                                 Compound Standards.
23-10.........................  Estimated detection                12.11
                                 limit.
23-11.........................  Total concentration..              12.12
------------------------------------------------------------------------

    We are also proposing to remove and replace the current equations
in Method 23 with the equations shown in Table 13 of this preamble to
accommodate the proposed changes to the method procedures.

        Table 13--Proposed Additional Equations for Section 12.0
------------------------------------------------------------------------
           Equation                  Description        Proposed section
------------------------------------------------------------------------
23-1..........................  Individual compound                 12.2
                                 RRF for each
                                 calibration level.
23-3..........................  Percent relative                    12.4
                                 standard deviation
                                 of the RRFs for a
                                 compound over the
                                 five calibration
                                 levels.
23-4..........................  Standard deviation of               12.5
                                 the RRFs for a
                                 compound over the
                                 five calibration
                                 levels.
23-5..........................  Percent difference of               12.6
                                 the RRF of the
                                 continuing
                                 calibration
                                 verification
                                 compared to the
                                 average RRF from the
                                 initial calibration
                                 for each target
                                 compound.
23-7..........................  Concentration of                    12.8
                                 individual target
                                 compound i in the
                                 sample extract.

23-8..........................  Concentration of the                12.9
                                 Individual Target
                                 Compound or Group i
                                 in the Emission Gas.
------------------------------------------------------------------------

M. Section 13.0

    In this action, the EPA is proposing to add a new section 13.0
titled ``Method Performance,'' that would include the specifications
shown in Table 14 of this preamble.

  Table 14--Proposed Method Performance Specifications for Section 13.0
------------------------------------------------------------------------
                Description                        Proposed section
------------------------------------------------------------------------
Quality control checks of filters,           13.1, 13.2, and 13.14.
 adsorbent resin, glass wool, and batch
 blanks.
Field train proof blanks...................  13.2.
GC column systems used to measure PCDD/F,    13.3 through 13.6.
 PAH, and PCB target compounds.
Acceptability of detection limits..........  13.7.
Tuning HRGC/HRMS systems...................  13.8.
MS lock channels...........................  13.9.
Initial and continuing calibrations........  13.10 and 13.11.
Identification of target compounds.........  13.12 and 13.13.
Pre-sampling, -extraction, and -analysis     13.15 and 13.16.
 spike recoveries.
Pre-analysis spike sensitivity requirements  13.17.
Modifications of the method................  13.18 and 13.19.
------------------------------------------------------------------------

N. Section 14.0

    In this action, the EPA is proposing to add a new section 14.0
titled ``Pollution Prevention,'' that specifies the procedures for
minimizing or preventing pollution associated with preparing and using
Method 23 standards.

O. Section 15.0

    In this action, the EPA is proposing to add a new section 15.0
titled ``Waste Management,'' that specifies the laboratory
responsibilities for managing the waste streams associated with
collecting and analyzing Method 23 samples.

P. Section 16.0

    In this action, the EPA is proposing to renumber and move the text
in section 10.0 (Bibliography) of the current method to a new section
16.0 titled ``References.'' We are proposing to delete previous
reference numbers 3 and 4 that are no longer relevant and to add new
citations for the following references:
     Fishman, V.N., Martin, G.D. and Lamparski, L.L. Comparison
of a variety of gas chromatographic columns with different polarities
for the separation of chlorinated dibenzo-p-dioxins and dibenzofurans
by high-resolution mass spectrometry. Journal of Chromatography A 1139
(2007) 285-300.
     International Agency for Research on Cancer. Environmental
Carcinogens Methods of Analysis and Exposure Measurement, Volume 11--
Polychlorinated Dioxins and Dibenzofurans. IARC Scientific Publications
No. 108, 1991.
     Stieglitz, L., Zwick, G., Roth, W. Investigation of
different treatment techniques for PCDD/PCDF in fly ash. Chemosphere
15: 1135-1140; 1986.
     Triangle Laboratories. Case Study: Analysis of Samples for
the Presence of Tetra Through Octachloro-p-Dibenzodioxins and
Dibenzofurans. Research Triangle Park, NC. 1988. 26 p.
     U.S. Environmental Protection Agency. Office of Air
Programs Publication No. APTD-0576: Maintenance, Calibration, and
Operation of Isokinetic Source Sampling Equipment. Research Triangle
Park, NC. March 1972.
     U.S. Environmental Protection Agency. Method 1625C-
Semivolatile Organic Compounds by Isotope Dilution GCMS.
     U.S. Environmental Protection Agency. Method 1613B-Tetra-
through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/
HRMS.
     U.S. Environmental Protection Agency. Method 1668C-
Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids, and
Tissue by HRGC/HRMS.
     Tondeur, Y., Nestrick, T., Silva, H[eacute]ctor A.,
Vining, B., Hart, J. Analytical procedures for the determination of
polychlorinated-p-dioxins, polychlorinated dibenzofurans, and
hexachlorobenzene in pentachlorophenol. Chemosphere Volume 80, Issue 2,
June 2010, pages 157-164.

Q. Section 17.0

    In this action, the EPA is proposing to add a new section 17 titled
``Tables, Diagrams, Flow Charts, and Validation Data,'' that will
contain all tables, diagrams, flow charts, and validation data
referenced in Method 23. We are proposing to revise Figures 23-1 and
23-2 and to rename and/or renumber the current Method 23 tables as
shown in Table 15 of this preamble.

            Table 15--Proposed Revisions to Method 23 Tables
------------------------------------------------------------------------
             Current method                      Proposed method
------------------------------------------------------------------------
Table 1--Composition of the Sample       Table 23-7. Composition of the
 Fortification and Recovery Standards     Sample Fortification and
 Solutions.                               Recovery Standard Solutions
                                          for PCDDs and PCDFs.
Table 2--Composition of the Initial      Table 23-11. Composition of the
 Calibration Solutions.                   Initial Calibration Standard
                                          Solutions for PCDDs and PCDFs.

Table 3--Elemental Compositions and      Table 23-4. Elemental
 Exact Masses of the Ions Monitored by    Compositions and Exact Masses
 High Resolution Mass Spectrometry for    of the Ions Monitored by High-
 PCDD's and PCDF's.                       Resolution Mass Spectrometry
                                          for PCDDs and PCDFs.
Table 4--Acceptable Ranges for Ion-      Table 23-15. Recommended Ion
 Abundance Ratios of PCDD's and PCDF's.   Type and Acceptable Ion
                                          Abundance Ratios.
Table 5--Minimum Requirements for        Table 23-14. Minimum
 Initial and Daily Calibration Response   Requirements for Initial and
 Factors.                                 Daily Calibration Response
                                          Factors for Isotopically
                                          Labeled and Native Compounds.
------------------------------------------------------------------------

    We are also proposing to add Figure 23-3 (Soxhlet/Dean-Stark
Extractor) and Figure 23-4 (Sample Preparation Flow Chart) and to add
the tables specified in Table 16 of this preamble.

            Table 16--Additional Proposed Tables to Method 23
------------------------------------------------------------------------
          Proposed table                         Description
------------------------------------------------------------------------
23-1..............................  Polychlorinated Dibenzo-p-dioxin and
                                     Polychlorinated Dibenzofuran Target
                                     Analytes.
23-2..............................  Polycyclic Aromatic Hydrocarbon
                                     Target Analytes.
23-3..............................  Polychlorinated Biphenyl Target
                                     Analytes.
23-5..............................  Elemental Compositions and Exact
                                     Masses of the Ions Monitored by
                                     High-Resolution Mass Spectrometry
                                     for PAHs.
23-6..............................  Elemental Compositions and Exact
                                     Masses of the Ions Monitored by
                                     High-Resolution Mass Spectrometry
                                     for PCBs.
23-8..............................  Composition of the Sample
                                     Fortification and Recovery Standard
                                     Solutions for PAHs.
23-9..............................  Composition of the Sample
                                     Fortification and Recovery Standard
                                     Solutions for PCBs.
23-10.............................  Sample Storage Conditions and
                                     Laboratory Hold Times.
23-12.............................  Composition of the Initial
                                     Calibration Standard Solutions for
                                     PAHs.
23-13.............................  Composition of the Initial
                                     Calibration Standard Solutions for
                                     PCBs.
23-16.............................  Typical DB5-MS Column Conditions.
23-17.............................  Assignment of Pre-extraction
                                     Standards for Quantitation of
                                     Target PCBs.
23-18.............................  Estimated Method Detection Limits
                                     for PCDDs and PCDFs.
23-19.............................  Target Detection Limits for PAHs.
23-20.............................  Estimated Method Detection Limits
                                     for PCBs.
------------------------------------------------------------------------

V. Summary of Proposed Revisions Related to 40 CFR Parts 60, 63, and
266

A. 40 CFR Part 60--Standards of Performance for New Stationary Sources

    In 40 CFR 60.17(h), we propose to incorporate by reference ASTM
D4840-99(2018)e1, Standard Guide for Sample Chain-of-Custody
Procedures, and to amend the reference to ASTM D6911-15, Guide for
Packaging and Shipping Environmental Samples for Laboratory Analysis,
to include for use in Method 23.
    In Subpart CCCC, we propose to revise Sec.  60.2125(g)(2) and
(j)(2) to realign the requirement for quantifying isomers to the
reorganized section <IP_ADDRESS> in the proposed revision of Method 23.
    In Subpart DDDD, we propose to revise Sec.  60.2690(g)(2) and
(j)(2) to realign the requirement for identifying isomers to the
reorganized section <IP_ADDRESS> in the proposed revision of Method 23.

B. 40 CFR Part 63--National Emission Standards for Hazardous Air
Pollutants for Source Categories

    In 40 CFR 63.849(a)(13), we propose to replace California Air
Resources Board (CARB) Method 428 with Method 23 for the measurement of
PCB emissions from roof monitors not employing wet roof scrubbers.
    In 40 CFR 63.1208, we propose to remove the requirement for
administrator's approval to use Method 23 for measuring PCDD/PCDF
emissions from hazardous waste combustors.
    In 40 CFR 63.1625(b)(10), we propose to replace CARB Method 429
with Method 23 for measuring the emissions of PAH from ferromanganese
electric arc furnaces.
    In Subpart AAAAAAA, Table 3, we propose to replace the requirement
for analysis of PAH by SW-846 Method 8270 with a requirement to use
Method 23. Specifically, we are deleting ``with analysis by SW 846
Method 8270D'' in row 6 of Table 3. Since revisions to Method 23
propose to eliminate the use of methylene chloride, we also propose to
remove footnote ``b'' in Table 3.

C. 40 CFR Part 266--Standards for the Management of Specific Hazardous
Wastes and Specific Types of Hazardous Waste Management Facilities

    In 40 CFR 266.104, we propose to add Method 23 as an alternative to
SW-846 Method 0023A.

VI. Statutory and Executive Order Reviews

    Additional information about these statutes and Executive Orders
can be found at https://www2.epa.gov/laws-regulations/laws-and-executive-orders.

A. Executive Order 12866: Regulatory Planning and Review and Executive
Order 13563: Improving Regulation and Regulatory Review

    This action is not a significant regulatory action and was,
therefore, not submitted to the Office of Management and Budget (OMB)
for review.

B. Executive Order 13771: Reducing Regulations and Controlling
Regulatory Costs

    This action is expected to be an Executive Order 13771 deregulatory
action. This proposed rule is expected to provide meaningful burden
reduction by improving the accuracy of Method 23, improving data
quality, and providing source testers flexibility by providing a
performance-based approach and incorporating approved alternative
procedures into the regulatory measurement method. This proposed action
does not impose any requirements on owners/operators to

use Method 23 but provides instruction on how to use Method 23 if
required to do so by an EPA source category regulation.

C. Paperwork Reduction Act (PRA)

    This proposed action does not impose an information collection
burden under the PRA. The revisions being proposed in this action to
Method 23 do not add information collection requirements but make
corrections, clarifications and updates to existing testing
methodology.

D. Regulatory Flexibility Act (RFA)

    I certify that this proposed action will not have a significant
economic impact on a substantial number of small entities under the
RFA. This action will not impose any requirements on small entities.
The proposed revisions to Method 23 do not impose any requirements on
regulated entities. Rather the proposed changes improve the quality of
the results when required by other rules to use Method 23. Revisions
proposed for Method 23 allow contemporary advances in analysis
techniques to be used. Further, the proposed changes in Method 23
analysis procedures reduce the impact of this method by bringing it
into alignment with other agency methods.

E. Unfunded Mandates Reform Act (UMRA)

    This proposed action does not contain any unfunded mandate of $100
million or more as described in UMRA, 2 U.S.C. 1531-1538. The proposed
action imposes no enforceable duty on any State, local or tribal
governments or the private sector.

F. Executive Order 13132: Federalism

    This proposed action does not have federalism implications. It will
not have substantial direct effects on the states, on the relationship
between the national government and the states, or on the distribution
of power and responsibilities among the various levels of government.

G. Executive Order 13175: Consultation and Coordination With Indian
Tribal Governments

    This proposed action does not have tribal implications, as
specified in Executive Order 13175. It will not have substantial direct
effects on the Indian Tribal Governments, on the relationship between
the national government and the Indian Tribal Governments, or on the
distribution of power and responsibilities among Indian Tribal
Governments and the various levels of government.

H. Executive Order 13045: Protection of Children From Environmental
Health Risks and Safety Risks

    The EPA interprets Executive Order 13045 as applying only to those
regulatory actions that concern environmental health or safety risks
that the EPA has reason to believe may disproportionately affect
children, per the definition of ``covered regulatory action'' in
section 2-202 of the Executive Order. This proposed action is not
subject to Executive Order 13045 because it does not establish or
revise a standard that provides protection to children against
environmental health and safety risks.

I. Executive Order 13211: Actions That Significantly Affect Energy
Supply, Distribution or Use

    This proposed action is not subject to Executive Order 13211,
because it is not a significant regulatory action under Executive Order
12866.

J. National Technology Transfer and Advancement Act (NTTAA)

    This proposed action involves technical standards. The EPA proposes
to use ASTM D6911-15 (Guide for Packaging and Shipping Environmental
Samples for Laboratory Analysis) and ASTM D4840-99(2018)e1 (Standard
Guide for Sample Chain-of-Custody Procedures). These ASTM standards
cover best practices that guide sample shipping and tracking from
collection through analysis.
    These standards were developed and adopted by the American society
for Testing and Materials. The standard may be obtained from https://www.astm.org or from the ASTM at 100 Barr Harbor Drive, P.O. box C700,
West Conshohocken, PA 19428-2959.

K. Executive Order 12898: Federal Actions To Address Environmental
Justice in Minority Populations and Low-Income Populations

    This proposed action will not have potential disproportionately
high and adverse human health or environmental effects on minority,
low-income or indigenous populations because it does not establish or
revise a standard that provides protection to human health or the
environment.

List of Subjects

40 CFR Part 60

    Environmental protection, Air pollution control, Hazardous air
pollutants, Incorporation by reference, Method 23, Polychlorinated
biphenyls, Polychlorinated dibenzofurans, Polychlorinated dibenzo-p-
dioxins, Polycyclic aromatic compounds, Test methods.

40 CFR Part 63

    Environmental protection, Air pollution control, Method 23, New
source performance, Polychlorinated biphenyls, Polychlorinated
dibenzofurans, Polychlorinated dibenzo-p-dioxins, Polycyclic aromatic
compounds, Test methods.

40 CFR Part 266

    Environmental protection, Air pollution control, Hazardous air
pollutants, Hazardous waste, Method 23, Polychlorinated biphenyls,
Polychlorinated dibenzofurans, Polychlorinated dibenzo-p-dioxins,
Polycyclic aromatic compounds, Test methods, Waste management.

    Dated: December 17, 2019.
Andrew R. Wheeler,
Administrator.
    For the reasons stated in the preamble, the Environmental
Protection Agency proposes to amend title 40, chapter I of the Code of
Federal Regulations as follows:

PART 60--STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES

0
1. The authority citation for part 60 continues to read as follows:

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

0
2. In Sec.  60.17:
0
a. Redesignate paragraphs (h)(167) through (h)(209) as (h)(168) through
(h)(210);
0
b. Add paragraph (h)(167); and
0
c. Revise newly redesignated paragraph (h)(192).
    The addition and revision read as follows:

Sec.  60.17  Incorporations by reference.

* * * * *
    (h) * * *
    (167) ASTM D4840-99(2018)e1 Standard Guide for Sample Chain-of-
Custody Procedures, approved August 2018, IBR approved for appendix A-
8: Method 30B, IBR approved for Appendix A-7: Method 23.
* * * * *
    (192) ASTM D6911-15 Standard Guide for Packaging and Shipping
Environmental Samples for Laboratory Analysis, approved January 15,
2015, IBR approved for appendix A-7: Method 23 and appendix A-8: Method
30B.
* * * * *
0
3. In Sec.  60.2125, revise paragraphs (g)(2) and (j)(2) to read as
follows:

Sec.  60.2125  How do I conduct the initial and annual performance
test?

* * * * *
    (g) * * * (2) Quantify isomers meeting identification criteria 2,
3, 4, and 5 in Section <IP_ADDRESS> of Method 23, regardless of whether the
isomers meet identification criteria in Section <IP_ADDRESS>.1 of Method
23. You must quantify the isomers per Section <IP_ADDRESS> of Method 23.
(Note: You may reanalyze the sample aliquot or split to reduce the
number of isomers to meet the identification criteria in Section
<IP_ADDRESS> of Method 23.)
* * * * *
    (j) * * *
    (2) Quantify isomers meeting identification criteria 2, 3, 4, and 5
in Section <IP_ADDRESS> of Method 23, regardless of whether the isomers
meet identification Section <IP_ADDRESS>.1 of Method 23. You must quantify
the isomers per Section <IP_ADDRESS> of Method 23. (Note: You may reanalyze
the sample aliquot or split to reduce the number of isomers to meet the
identification criteria in Section <IP_ADDRESS> of Method 23.)
* * * * *
0
4. In Sec.  60.2690, revise paragraphs (g)(2) and (j)(2) to read as
follows:

Sec.  60.2690  How do I conduct the initial and annual performance
test?

* * * * *
    (g) * * *
    (2) Quantify isomers meeting identification criteria 2, 3, 4, and 5
in Section <IP_ADDRESS> of Method 23, regardless of whether the isomers
meet identification Section <IP_ADDRESS>.1 of Method 23. You must quantify
the isomers per Section <IP_ADDRESS> of Method 23. (Note: You may reanalyze
the sample aliquot or split to reduce the number of isomers to meet the
identification criteria in Section <IP_ADDRESS> of Method 23.)
* * * * *
    (j) * * *
    (2) Quantify isomers meeting identification criteria 2, 3, 4, and 5
in Section <IP_ADDRESS> of Method 23, regardless of whether the isomers
meet identification Section <IP_ADDRESS>.1 of Method 23. You must quantify
the isomers per Section <IP_ADDRESS> of Method 23. (Note: You may reanalyze
the sample aliquot or split to reduce the number of isomers to meet the
identification criteria in Section <IP_ADDRESS> of Method 23.); and
* * * * *
0
5. Revise Method 23 of appendix A-7 to part 60 and to read as follows:

Appendix A-7 to Part 60--Test Methods 19 through 25E

* * * * *

Method 23--Determination of Polychlorinated Dibenzo-p-Dioxins,
Polychlorinated Dibenzofurans, Polychlorinated Biphenyls, and
Polycyclic Aromatic Hydrocarbons From Stationary Sources

1.0 Scope and Application

    1.1 Applicability. This method applies to measuring emissions of
polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans
(PCDDs/PCDFs), polychlorinated biphenyls (PCBs), and/or polycyclic
aromatic hydrocarbons (PAHs) in emissions from stationary sources.
Using this method, you can measure these analyte groups individually or
in any combination using a single sample acquisition. Tables 23-1
through 23-3 of this method list the applicable targets analytes for
Method 23.
    1.2 Scope. This method describes the sampling and analytical
procedures used to measure selected PCDDs, PCDFs, PCBs, and PAHs from
stationary source air emissions. However, Method 23 incorporates by
reference some of the specifications (e.g., equipment and supplies) and
procedures (e.g., sampling and analytical) from other methods in this
part that are essential to conducting Method 23. To obtain reliable
samples, source sampling teams should be trained and experienced with
the following additional EPA test methods: Method 1, Method 2, Method
3, Method 4, and Method 5 of appendices A-1, A-2, and A-3 to 40 CFR
part 60. Laboratory analysis teams should be trained and experienced
with Method 1668C found at: https://www.epa.gov/sites/production/files/2015-09/documents/method_1668c_2010.pdf and Method 1613B of 40 CFR part
136 appendix A.
    1.3 The high-resolution gas chromatography and high-resolution mass
spectrometry (HRGC/HRMS) portions of this method are for use by
laboratory analysts experienced with HRGC/HRMS analysis of PCDDs,
PCDFs, PCBs, and PAHs or under the close supervision of such qualified
persons. Each source testing team, including the sampling and
laboratory organization(s) that use this method, must demonstrate the
ability to generate acceptable results that meet the performance
criteria in Section 13 of this method.
    1.4 This method is ``performance-based'' and includes acceptability
criteria for assessing sampling and analytical procedures. Users may
modify the method to overcome interferences or to substitute superior
materials and equipment, provided that they meet all performance
criteria in this method. Section 13 of this method presents
requirements for method performance.

2.0 Summary of Method

    This method identifies and determines the concentration of specific
PCDD, PCDF, PCBs, and PAHs compounds. Gaseous and particulate bound
target pollutants are withdrawn from the gas stream isokinetically and
collected in the sample probe, on a glass fiber or quartz filter, and
on a packed column of adsorbent material. This method is not intended
to differentiate between target compounds in particle or vapor
fractions. The target compounds are extracted from the combined sample
collection media. Portions of the extract are chromatographically
fractionated to remove interferences, separated into individual
compounds or simple mixtures by HRGC, and measured with HRMS. This
method uses isotopically labeled standards to improve method accuracy
and precision.

3.0 Definitions

    3.1 Alternate Recovery Standards. A group of isotopically labeled
compounds that is not otherwise designated in this method for quality
control purposes. Use alternative recovery standards to assess the
recovery of a compound class relative to a step in the sampling and
analysis procedure that is not already assessed as a mandatory part of
this method.
    3.2 Batch Blank Sample. A laboratory blank sample composed of clean
filter and XAD-2 media processed and analyzed using the same procedures
as a field sample.
    3.3 Benzo[a]pyrene Toxic Equivalent Factor (B[a]P-TEF). One of
several schemes that express the toxicity for PAH compounds in terms of
the most toxic form of PAH, benzo[a]pyrene, as specified in applicable
regulations, permits, or other requirements.
    3.4 Continuing Calibration Verification Standard (CCV). The mid-
point calibration standard used to verify calibration. Prepare CCV
standards from a second source, when possible.
    3.5 Congener. An individual compound with a common structure
(dioxin, furan, or biphenyl), only differing by the number of chlorine
atoms attached to the structure.
    3.6 Estimated Detection Limit (EDL). The minimum qualitatively
recognizable signal above background for a target compound. The EDL is
a

mathematically-derived detection limit (MDL) specific to each sample
analysis based on the noise signal measured near the mass of a target
compound or target isomer group. Being sample specific, the EDL is
affected by sample size, dilution, etc.
    3.7 Estimated Possible Concentration (EPC). Report the results as
EPC when the ion abundance ratio for a target analyte is outside the
performance criteria. Calculate the EPC separately for each
quantitation ion, if present, and report the lower value as the EPC.
    3.8 Homolog. A compound belonging to a series of compounds with the
same general molecular formula, differing from each other by the number
of repeating units.
    3.9 Isomer. An individual compound with a common structure (dioxin,
furan, or biphenyl), only differing by the position of chlorine atoms
attached to the structure.
    3.10 Polychlorinated Biphenyl (PCB) Isomers. Any or all 209
chlorinated biphenyl congeners and their isomers. Table 23-3 of this
method lists the primary target compounds and appendix A to this method
provides the full list of 209 PCB congeners and isomers.
    3.10.1 Monochlorobiphenyl (MoCB). Any or all three monochlorinated
biphenyl isomers.
    3.10.2 Dichlorobiphenyl (DiCB). Any or all 12 dichlorinated
biphenyl isomers.
    3.10.3 Trichlorobiphenyl (TrCB). Any or all 24 trichlorinated
biphenyl isomers.
    3.10.4 Tetrachlorobiphenyl (TeCB). Any or all 42 tetrachlorinated
biphenyl isomers.
    3.10.5 Pentachlorobiphenyl (PeCB). Any or all 46 pentachlorinated
biphenyl isomers.
    3.10.6 Hexachlorobiphenyl (HxCB). Any or all 42 hexachlorinated
biphenyl isomers.
    3.10.7 Heptachlorobiphenyl (HpCB). Any or all 24 heptachlorinated
biphenyl isomers.
    3.10.8 Octachlorobiphenyl (OcCB). Any or all 12 octachlorinated
biphenyl isomers.
    3.10.9 Nonachlorobiphenyl (NoCB). Any or all three nonachlorinated
biphenyl isomers.
    3.10.10 Decachlorobiphenyl (DeCB). Biphenyl fully chlorinated with
ten chlorine atom substituents replacing hydrogen in the parent
compound.
    3.11 Polychlorinated dibenzo-p-dioxin (PCDD) isomers. Any or all 75
chlorinated dibenzo-p-dioxin isomers. There are 11 required target PCDD
analytes listed in Table 23-1 of this method. This method does not
measure mono- through tri-PCDDs and includes non-2,3,7,8 substituted
congeners in the total homolog categories.
    3.11.1 Tetrachlorodibenzo-p-dioxin (TeCDD). Any or all 22
tetrachlorinated dibenzo-p-dioxin isomers.
    3.11.2 Pentachlorodibenzo-p-dioxin (PeCDD). Any or all 14
pentachlorinated dibenzo-p-dioxin isomers.
    3.11.3 Hexachlorodibenzo-p-dioxin (HxCDD). Any or all 10
hexachlorinated dibenzo-p-dioxin isomers.
    3.11.4 Heptachlorodibenzo-p-dioxin (HpCDD). Any or all two
heptachlorinated dibenzo-p-dioxin isomers.
    3.11.5 Octachlorodibenzo-p-dioxin (OCDD). Dibenzodioxin fully
chlorinated with eight chlorine atom substituents replacing hydrogen in
the parent compound.
    3.12 Polychlorinated dibenzofuran (PCDF) isomers. Any or all
chlorinated dibenzofuran isomers. There are 14 required target PCDF
analytes listed in Table 23-1 of this method. This method does not
measure mono- through tri-PCDFs and includes non-2,3,7,8 substituted
congeners in the total homolog categories.
    3.12.1 Tetrachlorodibenzofuran (TeCDF). Any or all 38
tetrachlorinated dibenzofuran isomers.
    3.12.2 Pentachlorodibenzofuran (PeCDF). Any or all 28
pentachlorinated dibenzofuran isomers.
    3.12.3 Hexachlorodibenzofuran (HxCDF). Any or all 16
hexachlorinated dibenzofuran isomers.
    3.12.4 Heptachlordibenzofuran (HpCDF). Any or all four
heptachlorinated dibenzofuran isomers.
    3.12.5 Octachlorodibenzofuran (OCDF). Dibenzofuran fully
chlorinated with eight chlorine atom substituents replacing hydrogen in
the parent compound.
    3.13 Polychlorinated diphenyl ethers (PCDEs). Any or all
chlorinated substituted diphenyl ethers.
    3.13.1 Hexachlorodiphenyl ether (HxCDPE). Any or all 42
hexachlorinated diphenyl ether isomers.
    3.13.2 Heptachlorodiphenyl ether (HpCDPE). Any or all 24
heptachlorinated diphenyl ether isomers.
    3.13.3 Octachlorodiphenyl ether (OCDPE). Any or all 12
octachlorinated diphenyl ether isomers.
    3.13.4 Nonachlorodiphenyl ether (NCDPE). Any or all three
nonachlorinated diphenyl ether isomers.
    3.13.5 Decachlorodiphenyl ether (DCDPE).
    3.14 Polycyclic Aromatic Hydrocarbons (PAHs). Any or all aromatic
compounds with two or more fused six-member rings. Table 23-2 of this
method lists the target PAH compounds for this method. You may add and
analyze additional PAH compounds by adding the appropriate \13\ C
isotopically labeled compound to the pre-extraction spike mixture and
by following the other requirements for target PAH compounds in this
method.
    3.15 Pre-analysis Standard(s). A group of isotopically labeled
compounds added at a known amount immediately prior to analysis and
used to correct instrument response, injection errors, instrument drift
and to determine the recovery of the pre-extraction isotopically
labeled spike compounds. Add pre-analysis standards to every sample
(including blank, quality control sample, and calibration solutions) at
a known amount.
    3.16 Pre-extraction Filter Recovery Standard(s). A group of
isotopically labeled compounds added at a known amount to the filter
used to indicate the extraction efficiency of the filter media. Add
pre-extraction filter recovery standard(s) to the filter samples just
prior extraction.
    3.17 Pre-extraction Standard(s). A group of isotopically labeled
compounds added in a known amount to the XAD-2 adsorbent sample
immediately before extraction to correct the quantity of the native
target compounds present in the sample for extraction, cleanup, and
concentration recovery. These isotopically labeled compounds constitute
a matrix spike in each sample.
    3.18 Pre-sampling Adsorbent Standard(s). A group of isotopically
labeled compounds added in a known amount to the XAD-2 adsorbent prior
to sampling used to indicate the sample collection and recovery
efficiency of the method.
    3.19 Pre-transport Standard(s). Spiking compound(s) from the list
of alternative recovery standards that can be added by the laboratory
to the sample shipping containers used to transport field equipment
rinse and recovery samples. The measured concentration of the pre-
transport recovery standard provides a quality check on potential probe
rinse sample spillage or mishandling after sample collection and during
shipping.
    3.20 Relative Response Factor (RRF). The response of the mass
spectrometer to a known amount of an analyte relative to a known amount
of an isotopically labeled standard.
    3.21 2,3,7,8-Tetrachlorodibenzo-p-dioxin Toxic Equivalent Factor(s)
(2,3,7,8-TeCDD-TEF). A procedure that expresses the toxicity of PCDDs,
PCDFs,

and PCBs in terms of the most toxic dioxin, as specified in applicable
regulations, permits, or other requirements.

4.0 Interferences

    4.1 PCBs and PCDEs have similar molecular weight and
chromatographic properties to PCDDs and PCDFs. PCBs produce an
interfering mass-to-charge ratio (m/z) when losing chlorine
(Cl2) or Cl4 upon fragmenting during ionization
processes. PCDEs also produce interfering m/z values when losing
Cl2 in the PCDF homolog group with two fewer chlorine atoms
(i.e., an octachlorinated PCDE can interfere with a hexachlorinated
PCDF). The latter interferences are potentially detected by monitoring
an m/z corresponding to the potentially interfering PCDE; however, the
fragmentation patterns of all PCDEs may not be known, complicating any
attempt to quantify the extent of ether interference.
    4.2 Very high amounts of other organic compounds in the matrix may
interfere with the analysis. This method provides examples of column-
chromatographic cleanup as procedures to reduce, but not necessarily
eliminate, matrix effects due to high concentrations of organic
compounds (International Agency for Research on Cancer 1991).
    4.3 Target compound contaminants or related organics in solvents,
reagents, glassware, isotopically labeled spiking standards, and other
sample processing hardware are potential method interferences.
Routinely evaluate all these materials to demonstrate that they are
either free from interferences under the conditions of the analysis, or
that the interference does not compromise the quality of the analysis
results. Evaluate chemical interference through the preparation and
analysis of batch blank samples. Use high purity reagents, solvents,
and standards to minimize interference problems in sample analysis.
    4.4 PAHs are subject to degradation when exposed to ultraviolet
light. Take precautions to shield samples from sunlight or fluorescent
light sources during sample collection, recovery, extraction, cleanup,
and concentration.

5.0 Safety

    Note: Develop a strict laboratory safety program for the
handling of PCDDs, PCDFs, PCBs, and/or PAHs.

    5.1 Compounds in the PCDD and PCDF classes such as 2,3,7,8-TeCDD
are aneugenic, carcinogenic, and teratogenic in laboratory animal
studies. Other PCDDs and PCDFs containing chlorine atoms in positions
2,3,7,8 have toxicities comparable to that of 2,3,7,8-TeCDD.
    5.2 PCBs are classified as known or suspected human or mammalian
carcinogens. Be aware of the potential for inhalation and ingestion
exposure to laboratory analysts.
    5.3 This method recommends that the laboratory purchase dilute
standard solutions of the analytes required for this method. However,
if preparing primary solutions, use a hood or glove box. Laboratory
personnel handling primary solutions should wear personal protective
equipment including a toxic gas respirator mask fitted with charcoal
filters approved by the National Institute for Occupational Safety and
Health (NIOSH)/Mine Safety Health Administration (MSHA) to prevent the
inhalation of airborne particulates if not working in an approved hood
or glove box.
    5.4 The toxicity or carcinogenicity of other reagents or chemicals
used in this method is not precisely defined. However, treat each
chemical as a potential health hazard and minimize exposure to these
chemicals. The laboratory is responsible for maintaining a current
awareness file of Occupational Safety and Health Administration (OSHA)
regulations regarding the safe handling of the chemicals specified in
this method. Ensure that a reference file or list of internet sites
that contain safety data sheets (SDS) is available to all personnel
involved in the sampling and chemical analysis of samples known or
suspected to contain PCDDs, PCDFs, PCBs, and PAHs.

6.0 Equipment and Supplies

    Note: Brand names, suppliers, and part numbers are for
illustration purposes only and no endorsement is implied. Apparatus
and materials other than those specified in this method may achieve
equivalent performance. Meeting the performance requirements of this
method is the responsibility of the source testing team and
laboratory team.

    6.1 Sampling Apparatus. Figure 23-1 of this method shows a
schematic of the Method 23 sampling train. Do not use sealing greases
or brominated flame retardant-coated tape in assembling the train. The
train is identical to that described in section 6.1.1 of Method 5 of
appendix A-3 to 40 CFR part 60 with the following additions:
    6.1.1 Nozzle. The nozzle must be made of quartz or borosilicate
glass or titanium. Stainless steel nozzles should not be used.
    6.1.2 Probe Liner. Use either polytetrafluoroethylene (PTFE),
borosilicate, or quartz glass probe liners with a heating system
capable of maintaining a probe gas temperature of 120  14
[deg]C (248  25 [deg]F) during sampling, or such other
temperature as specified by an applicable subpart of the standards or
as approved by the Administrator. Use a PTFE ferrule or single-use PTFE
coated O-ring to achieve the seal at the nozzle end of the probe for
stack temperatures up to about 300 [deg]C (572 [deg]F). Use a quartz
glass liner and integrated quartz nozzle for stack temperatures between
300 and 1,200 [deg]C (572 and 2,192 [deg]F).
    6.1.3 Filter Holder. Use a filter holder of borosilicate glass with
a PTFE frit or PTFE-coated wire filter support. The holder design
should provide a positive seal against leakage from the outside or
around the filter. The holder should be durable, easy to load, leak-
free in normal applications, and positioned immediately following the
probe and cyclone bypass (or cyclone, if used) with the active side of
the filter perpendicular to the source of the flow.
    6.1.4 Filter Heating System. Use any heating system capable of
monitoring and maintaining the temperature around the filter to ensure
that the sample gas temperature exiting the filter is 120
14 [deg]C (248  25 [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.
    6.1.5 Filter Temperature Sensor. Install a temperature sensor
capable of measuring temperature to within  3 [deg]C (5.4
[deg]F) so that the sensing tip protrudes at least 1.3 centimeters (cm)
(1-2 in.) into the sample gas exiting the filter. Encase the sensing
tip of the sensor in glass or PTFE if needed.
    6.1.6 Sample Transfer Line. The sample transfer line transports
gaseous emissions from the heated filter holder to the condenser and
must be heat traced and constructed of glass or PTFE with connecting
fittings that form leak-free, vacuum-tight connections without using
sealing greases or tapes. Keep the sample transfer lines as short as
possible and maintain the lines at a temperature of 120 [deg]C  14 [deg]C (248 [deg]F  25 [deg]F) using active
heating when necessary. Orient the sample transfer lines with the
downstream end lower than the upstream end so that any condensate will
flow away from the filter and into the condenser.
    6.1.7 Condenser. Glass, water-jacketed, coil-type with compatible
fittings. Orient the condenser to cause moisture to flow down to the
adsorbent module to facilitate condensate drainage. Figure 23-2 of this
method shows a schematic diagram of the condenser.

    6.1.8 Water Circulating Bath. Use a bath pump circulating system
capable of providing chilled water flow to the condenser and adsorbent
module water jackets. Typically, a submersible pump is placed in the
impinger ice water bath to circulate the ice water contained in the
bath. Verify the function of this system by measuring the gas
temperature at the entrance to the adsorbent module. Maintain this
temperature at < 20 [deg]C (68 [deg]F).
    6.1.9 Adsorbent Module. Use a water-jacketed glass container to
hold up to 40 grams (g) of the solid adsorbent. Figure 23-2 of this
method shows a schematic diagram of the adsorbent module. Other
physical configurations of the adsorbent resin module/condenser
assembly are acceptable if the configuration contains the requisite
amount of solid adsorbent and maintains the minimum length-to-width
adsorbent bed ratio of two-to-one. Orient the adsorbent module
vertically to facilitate condensate drainage. The connecting fittings
must form leak-free, vacuum-tight seals. Include a coarse glass frit in
the adsorbent module to retain the adsorbent.
    6.1.10 Impingers. Use five impingers connected in series with leak-
free ground glass fittings or any similar leak-free noncontaminating
fittings. The first impinger must be a short-stem stem (water-dropout)
design or equivalent. The second, fourth, and fifth impingers must be
of the Greenburg-Smith design, modified by replacing the tip with a 1.3
cm (1-2 in.) inside diameter (ID) glass tube extending to approximately
1.3 cm (1-2 in.) from the bottom of the flask. The third impinger must
be of the Greenburg-Smith design with the standard tip. The second and
third impingers must contain known quantities of water, and the fifth
impinger must contain a known weight of silica gel or equivalent
desiccant. Alternatively, you may omit the first impinger if you do not
expect excess moisture in the sample gas.
    6.2 Sample Recovery Equipment.
    6.2.1 Fitting Caps. Use leak-free ground glass fittings or any
similar leak-free non-contaminating fitting to cap the sections of the
sampling train exposed to the sample gas. Alternatively, use PTFE tape
or contaminant-free aluminum foil for this purpose (see Section 6.2.6
of this method).
    6.2.2 Wash Bottles. Use PTFE bottles.
    6.2.3 Probe-Liner, Probe-Nozzle, and Filter-Holder Brushes. Use
inert bristle brushes with precleaned stainless steel or PTFE handles.
Extensions of the probe brush must be made of stainless steel or PTFE
and be at least as long as the probe. Use brushes that are properly
sized and shaped to remove accumulated material from the nozzle and
probe liner if used.
    6.2.4 Filter Storage Container. Use a sealed filter holder, wide-
mouth amber glass jar with PTFE-lined cap, or glass petri dish sealed
with PTFE tape. Purchase precleaned amber glass jars and petri dishes
or clean according to the glassware cleaning procedures listed in
Section <IP_ADDRESS> of this method.
    6.2.5 Field Balance. Use a weighing device capable of measurements
to an accuracy of 0.5g.
    6.2.6 Aluminum Foil. Use heavy duty aluminum foil cleaned by
rinsing three times with hexane or toluene and stored in a pre-cleaned
glass petri dish or glass jar. Do not use aluminum foil to wrap or
contact filter samples due to the possibility of reaction between the
sample and the aluminum.
    6.2.7 Adsorbent Storage Containers. Use an air-tight container to
store silica gel.
    6.2.8 Glass Sample Storage Containers. Recover samples in amber
glass bottles, 500- or 1000-milliliters (mL) with leak-free PTFE-lined
caps. Either purchase precleaned bottles or clean containers according
to glassware cleaning procedures listed in Section <IP_ADDRESS> of this
method.
    6.3 Sample Extraction Equipment.
    6.3.1 Sample Containers. Use 125- and 250-mL amber glass bottles
with PTFE-lined caps.
    6.3.2 Test Tubes. Use glass test tubes or small (e.g., 5 to 10 mL)
amber vials.
    6.3.3 Soxhlet/Dean-Stark Extraction Apparatus.
    <IP_ADDRESS> Soxhlet Apparatus. Use 200-mL capacity capable of holding
43 x 123-millimeter (mm) extraction thimbles, with receiving flask
(typically round-bottom).
    <IP_ADDRESS> Moisture Trap. Use Dean-Stark or Barret with fluoropolymer
stopcock trap to fit between the Soxhlet extractor body and the
condenser as shown in Figure 23-3 of this method. Note: Dean-Stark or
Barret traps are used to remove water with extraction solvents that are
less dense and insoluble in water.
    <IP_ADDRESS> Extraction Thimble. Use quartz, glass, or glass fiber
thimble, typically 43 x 123 mm to fit Soxhlet apparatus.
    <IP_ADDRESS> Heating Mantle. Use a hemispherical shaped heating mantle
to fit round-bottom flask.
    6.3.4 Kuderna-Danish Concentrator. Use an apparatus consisting of a
three-ball Snyder column, a flask with leak-free joint to accept the
three-ball Snyder column at the top, a leak-free joint to receive a
graduated concentration tube at the bottom and a heating mantle.
    6.3.5 Nitrogen Evaporative Concentrator. Use a nitrogen evaporative
concentrator equipped with a water bath with the temperature controlled
in the range of 30 to 60 [deg]C (86 to 140 [deg]F) (N-Evap Organomation
Associates, Inc., South Berlin, MA, or equivalent).
    6.3.6 Separatory Funnels. Use glass or PTFE 2-liter separatory
funnels.
    6.4 Glass Liquid Chromatography Columns.
    6.4.1 Pasteur Pipettes. Use disposable pipettes, or glass
serological pipettes typically 150 mm long x 6 mm ID.
    6.4.2 Chromatography Columns. 200 to 300 mm long x 20 mm ID with
250-mL reservoir.
    6.5 Analytical Equipment.
    6.5.1 Gas Chromatograph. Use a gas chromatograph consisting of the
following components:
    <IP_ADDRESS> Oven. Use an oven capable of maintaining the separation
column at the proper operating temperature  1.0 [deg]C (1.8
[deg]F) and performing programmed increases in temperature at rates of
at least 20 [deg]C/min with isothermal hold.
    <IP_ADDRESS> Temperature Monitor. Use a temperature monitor to measure
column oven temperature to  1.0 [deg]C (1.8 [deg]F).
    <IP_ADDRESS> Flow System. Use an electronic pressure control or
equivalent gas metering system to control carrier gas flow or pressure.
    <IP_ADDRESS> Use a split/splitless injection port in the splitless mode
or on-column injection port for the capillary column.
    6.5.2 Capillary Gas Chromatography Columns. Use different columns
for the analysis of the different target compound classes in this
method, if needed. Perform the resolution checks in Sections <IP_ADDRESS>
and <IP_ADDRESS> of this method to document the required resolution.
Compound separation must meet the resolution specifications in Section
<IP_ADDRESS> of this method and the identification specifications found in
Section <IP_ADDRESS> of this method.
    <IP_ADDRESS> Recommended column systems for measuring PCDDs/PCDFs should
be capable of achieving separation of the 17 PCDD/PCDF target compounds
from the nearest eluting congener with no more than 10 percent peak
overlap. The system must meet the performance specifications for
compound separation and quantitation in calibration, performance check,
and isotopically labeled standards added to field samples. Use a
variety of bonded-phase capillary gas chromatography columns to meet
these requirements, if needed.

    Note:  Fishman, et al. (see Section 16.3 of this method)
demonstrated that all TEF isomers can be fully differentiated from
closely eluting isomers using either of two sets of non-polar and
polar stationary phase combinations. One set consisted of 5-percent
phenyl methylpolysiloxane (DB-5, HP-5MS, Rtx-5MS, Equity-5) and 50-
percent cyanopropylmethyl, 50-percent phenylmethylsiloxane (DB-225,
SP 2331) GC columns and the other set consisted of 5-percent phenyl,
94-percent methyl, 1-percent vinyl silicone bonded-phase (DB-5MS,
ZB-5MS, VF-5MS, CP-Sil 8 CB LowBleed/MS) with 50-percent
cyanopropylmethyl, 50-percent phenylmethylsiloxane (SP-2331).

    <IP_ADDRESS> Use column systems for measuring PAHs that can achieve
separation of anthracene and phenanthrene at m/z 178 such that the
valley between the peaks does not exceed 50 percent of the taller of
the two peaks, and benzo[b]fluoranthene and benzo[k]fluoranthene such
that the valley between the peaks is less than 60 percent of the height
of the taller peak. These requirements are achievable using a 30-m
narrow bore (0.25 mm ID) 5-percent phenyl polysilphenylene-siloxane
(BPX5 or equivalent) bonded-phase, fused-silica capillary column.
    <IP_ADDRESS> PCB Columns.
    <IP_ADDRESS>.1 Use column systems for measuring PCBs that can achieve
unique resolution and identification of the toxics for determination of
a TEQPCB using TEFs (American Society of Mechanical
Engineers 1984). Isomers may be unresolved if they have the same TEF
and response factor and if these unresolved isomers are uniquely
resolved from all other congeners. These requirements are achievable
using several 30-meter (m) narrow bore (0.25 mm ID) columns including
8-percent phenyl polycarborane-siloxane (HT8), DB-XLB, and poly (50-
percent n-octyl/50-percent methyl siloxane) (SPB-Octyl).
    <IP_ADDRESS>.2 If using an SPB-Octyl column for PCB analysis, the column
should also uniquely resolve isomers 34 from 23 and 187 from 182.
Resolution for these PCBs is shown by the valley between the peaks not
exceeding 40 percent of the taller of the two peaks that result when
these congeners are analyzed in the same calibration sample.
    6.5.3 Mass Spectrometer. Use 28 to 70 electron volt impact
ionization capable of repetitive selective monitoring of 12 exact m/z
values with a mass resolution defined in section 10.2.1 of this method
for fragments in the range of 300 to 350 m/z. The deviation between
each monitored mass lock m/z and the monoisotopic m/z (Tables 23-4, 23-
5, and 23-6 of this method for PCDDs/PCDFs, PAHs, and PCBs,
respectively) must be less than 5 parts per million.
    6.5.4 Mass Spectrometer Data System. Use a data system compatible
with the mass spectrometer and capable of sequencing and monitoring
multiple groups of selected ions.
    6.5.5 Analytical Balance. Use an analytical balance to measure
within 0.1 milligram (mg).

7.0 Reagents, Media, and Standards

    Note:  The quality checks described in this section are
recommended but not required. They are provided to help ensure data
will meet the required performance specifications in Section 13 of
this method.

    7.1 Filter. 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.
    7.1.1 Extraction. Conduct a quality control check on the filter lot
prior to the field test to demonstrate that filters are free from
contamination or interference. Perform Soxhlet extraction on a minimum
of three filters with toluene for 16 hours. After extraction, allow the
Soxhlet apparatus to cool. Remove the filters and remove the solvent
from the filters under clean conditions (e.g., a clean nitrogen
stream).
    7.1.2 Analysis. Analyze the individual extracts of a minimum of
three filters from each lot used for sampling according to the
procedures in Section 11 of this method. The blank filter check
analysis must meet the performance requirements in Section 13.14 of
this method.
    7.2 Adsorbent Resin. Amberlite[supreg] XAD-2 resin. All adsorbent
resin must meet the cleanliness criteria in Section 13.14 of this
method for all target compounds on the analysis list (i.e., native
PCDD/PCDF, PCB, and/or PAH) following the same extraction,
concentration, cleanup, and analysis steps as field samples. This
method recommends using the procedures provided in appendix B to this
method to clean the resin before use, if needed. However, this method
allows alternative cleanup procedures that use automated extraction
equipment if the adsorbent meets the required performance criteria in
Section 13.14 of this method.
    7.2.1 Conduct a quality control check on the cleaned adsorbent
using HRGC/HRMS techniques following procedures in Section 11 of this
method. The cleaned adsorbent must meet the criteria in Section 13.14
of this method. A batch blank conducted on the filter and adsorbent lot
combination used for a test can serve this purpose.
    7.2.2 Storage. Store adsorbent in its original purchase container,
a clean wide-mouth amber glass container with a PTFE-lined cap, or in
glass adsorbent modules tightly sealed with glass caps.
    7.3 Glass Wool. Clean the glass wool to meet the specifications in
Section 13.14 of this method. Using sequential immersion in three clean
aliquots of toluene, drying in a 110 [deg]C (230 [deg]F) oven, and
storing in a toluene-rinsed glass jar with a PTFE-lined screw cap can
meet these requirements.
    7.4 Water. Use deionized or distilled water meeting requirements in
Section 13.14 of this method and store in its original container or in
a toluene-rinsed glass container with a PTFE-lined screw cap.
    7.5 Silica Gel. Indicating type, 6-16 mesh. If previously used, dry
at 175 [deg]C (347 [deg]F) for two hours. Use new silica gel as
received. As an alternative, use other types of desiccants (equivalent
or better), subject to the approval of the Administrator.
    7.6 Methylene Chloride. Pesticide grade or better.
    7.7 Sample Recovery Reagents.
    7.7.1 Acetone. Pesticide grade or better.
    7.7.2 Toluene. Pesticide grade or better.
    7.8 Sample Extraction and Cleanup.
    7.8.1 Potassium Hydroxide. American Chemical Society (ACS) grade, 2
percent (weight/volume) in water.
    7.8.2 Sodium Sulfate. Granulated or powdered, reagent grade. Use as
received, include in batch blank evaluation prior to use, or purify as
necessary prior to use by rinsing with methylene chloride or toluene
and oven drying. The batch blank must meet the requirements in Section
13.14 of this method. Store the cleaned material in a glass container
with a PTFE-lined screw cap.
    7.8.3 Sulfuric Acid. Reagent grade.
    7.8.4 Sodium Hydroxide. 1.0 N. Weigh 40 g of sodium hydroxide into
a 1-liter volumetric flask. Dilute to 1 liter with water.
    7.8.5 Hexane. Pesticide grade or better.
    7.8.6 Methanol. Pesticide grade or better.
    7.8.7 Toluene. Pesticide grade or better.
    7.8.8 High-Boiling Alkanes Used as Keeper Solvents (e.g.,
tetradecane, nonane, decane). Pesticide grade. Note: Lower homologous
series alkanes (nonane or decane) are necessary for higher volatility
targets such as MoCBs and naphthalene to maintain retention during
concentration procedures. However, do not take samples to

dryness when using these lower alkane homologs.
    7.8.9 Liquid Column Chromatography Packing Materials. Use the
following column chromatography packing materials, as needed, to
prepare sample extracts and remove interfering compounds. Commercially
prepacked cleaning columns may be available for this purpose. All
procedures for preparing column chromatography packing materials are
recommendations shown to meet the performance specifications required
for the recovery of labeled compounds described in Section 13 of this
method.
    <IP_ADDRESS> Alumina. Use either acidic or basic alumina in the cleanup
of sample extracts. Use the same type of alumina for all samples in an
analytical sequence, including those used to demonstrate batch blank
performance.
    <IP_ADDRESS>.1 Acidic Alumina (Sigma-Aldrich[supreg] 199966 or
equivalent). Brockmann activity grade 1, 100-200 mesh. Prior to use,
activate the alumina by heating for 12 hours at 130 [deg]C (266
[deg]F). Store in a desiccator. You may use pre-activated alumina
purchased from a supplier as received.
    <IP_ADDRESS>.2 Basic Alumina (Sigma-Aldrich[supreg] 19943 or
equivalent). Brockmann activity grade 1. Activate by heating to 600
[deg]C (1,112 [deg]F) for a minimum of 24 hours. Do not heat to over
700 [deg]C (1,292 [deg]F) because this can lead to reduced capacity for
retaining the analytes. Store at 130 [deg]C (266 [deg]F) in a covered
flask. Use within five days of baking. Use prepacked alumina columns
immediately after opening the vacuum sealed pouch or container.
    <IP_ADDRESS> Florisil[supreg]. Activated, 60-100 mesh recommended. Heat
previously activated Florisil[supreg] in a glass container loosely
covered with aluminum foil in an oven at 130 to 150 [deg]C (266 to 302
[deg]F) for a minimum of 24 hours. Upon cooling, store activated
Florisil[supreg] silica prior to use in a desiccator.
    <IP_ADDRESS> Silica Gel. Use either activated, acidic or basic silica
gel in the cleanup of sample extracts. Use the same type of silica gel
for all samples in an analytical sequence, including those used to
demonstrate batch blank performance.
    <IP_ADDRESS>.1 Activated Silica Gel. Supelco[supreg] 1-3651, Bio-
Sil[supreg] A, 100-200 mesh (or equivalent). Prior to use, rinse with
methylene chloride and activate the silica gel by heating for at least
1 hour at 180 [deg]C (356 [deg]F). After cooling, rinse the silica gel
sequentially with methanol and toluene. Heat the rinsed silica gel at
50 [deg]C (122 [deg]F) for 10 minutes, then increase the temperature
gradually to 180 [deg]C (356 [deg]F) over 25 minutes and maintain the
gel at this temperature for 90 minutes. Cool in a desiccator to room
temperature and store in a glass container with a PTFE-lined screw cap.
    <IP_ADDRESS>.2 Acidic Silica Gel (30 percent weight/weight). Combine 100
g of activated silica gel with 44 g of concentrated sulfuric acid in a
clean screw-capped glass container and agitate thoroughly. Disperse the
solids with a stirring rod until obtaining a uniform mixture. Store the
mixture in a glass container with a PTFE-lined screw cap.
    <IP_ADDRESS>.3 Basic Silica Gel. Combine 30 g of 1 N sodium hydroxide
with 100 g of activated silica gel in a clean screw-capped glass
container and agitate thoroughly. Disperse solids with a stirring rod
until obtaining a uniform mixture. Store the mixture in glass container
with a PTFE-lined screw cap.
    <IP_ADDRESS> Carbon/Celite[supreg] 545 (or equivalent solid support).
Use a carbon-based column cleanup material (e.g., one of the many
Carbopack[supreg] B or C) to remove impurities from the samples prior
to analysis. Thoroughly mix 9.0 g Carbopack[supreg] C and 41.0 g
Celite[supreg] 545 to produce an 18-percent weight/weight mixture.
Activate the mixture at 130 [deg]C (266 [deg]F) for a minimum of 6
hours. Store in a desiccator.
    7.8.10 Nitrogen. 99.999 percent (ultra-high) purity.
    7.9 Sample Analysis.
    7.9.1 Helium. 99.999 percent (ultra-high) purity.
    7.9.2 Spiking Standards. Prepare spiking standards quantitatively
at a convenient concentration (e.g.,10 nanograms (ng)/mL) or use
commercial standards if available, to enable accurate spiking of a
labeled standard at various stages of the sample preparation. You may
adjust the spiking concentrations from those recommended in Tables 23-
7, 23-8 and 23-9 of this method to accommodate the concentration of
target compounds anticipated in samples if the performance criteria in
Section 13 of this method are met.
    7.9.3 Pre-Sampling Recovery Standard Solution. Prepare stock
standard solutions in nonane to enable spiking of the isotopically
labelled compounds for target compound classes in Tables 23-7, 23-8,
and 23-9 of this method at the mass shown under the heading ``Pre-
sampling Adsorbent Standards.''
    7.9.4 Pre-extraction Filter Recovery Spike Standard Solution.
Prepare stock standard solutions in nonane to enable spiking of the
isotopically labelled compounds for target compound classes in Tables
23-7, 23-8, and 23-9 of this method at the mass shown under the heading
``Pre-extraction Filter Recovery Spike Standards.''
    7.9.5 Pre-extraction Recovery Standard Solution. Prepare stock
standard solutions in nonane to enable spiking of the isotopically
labelled compounds for target compound classes in Tables 23-7, 23-8,
and 23-9 of this method at the mass shown under the heading ``Pre-
extraction Standards.''
    7.9.6 Pre-analysis Standard Solution. Prepare stock standard
solutions in nonane to enable spiking of the isotopically labelled
compounds for target compound classes in Tables 23-7, 23-8, and 23-9 of
this method at the mass shown under the heading ``Pre-analysis
Standards.''

8.0 Sample Collection, Preservation and Storage

    8.1 Sampling. This method involves collection and recovery of trace
concentrations of semivolatile organic compounds. Therefore, train
field sampling and recovery staff in the best practices for handling
and using organic solvents in field environments to recover and protect
samples from contamination.
    8.1.1 Pretest Preparation.
    <IP_ADDRESS> Cleaning Glassware. Clean glassware thoroughly before
using. This section provides a recommended procedure, but any protocol
that consistently results in contamination-free glassware meeting the
batch blank criteria in Section 13.2 of this method is acceptable.
    <IP_ADDRESS>.1 Soak all glassware in hot soapy water (Alconox[supreg] or
equivalent).
    <IP_ADDRESS>.2 Rinse with hot tap water.
    <IP_ADDRESS>.3 Rinse with deionized/distilled water.
    <IP_ADDRESS>.4 Rinse with methanol.
    <IP_ADDRESS>.5 Rinse with toluene.
    <IP_ADDRESS>.6 Baking glassware at 300 [deg]C (572 [deg]F) for a minimum
of 2 hours may be necessary to remove contaminants or interferents from
particularly dirty samples. Cool glassware after baking.

    Note:  Repeated baking of glassware may cause active sites on
the glass surface that may irreversibly absorb target compounds.

    <IP_ADDRESS>.7 Cover glassware openings with clean glass fitting caps or
cleaned aluminum foil (see Section 6.2.6 of this method).
    <IP_ADDRESS>.8 Rinse glassware immediately before use with acetone and
toluene.

    Note:  To prepare heavily soiled glassware, remove surface
residuals from the glassware by soaking in hot soapy water, rinsing
with hot water, then soaking with a non-chromic acid oxidizing
cleaning reagent in a strong acid (e.g., NOCHROMIX[supreg] prepared
according to manufacturer's directions). After the acid soak, rinse
with hot water and repeat the

cleaning procedures in Section <IP_ADDRESS> of this method.

    <IP_ADDRESS> Adsorbent Module. Load the modules in a clean area to avoid
contamination. Spike modules before the sampling event, but do not
spike the modules in the field. Fill a module with 20 to 40 g of XAD-2.
Add the pre-sampling standard spike for each of the compound classes to
be measured to the top quarter of the adsorbent bed. Add sufficient
spike (picograms (pg)/module) to result in the final theoretical
concentrations specified in Tables 23-7, 23-8, and 23-9 of this method
for PCDDs/PCDFs, PAHs, and PCBs, respectively. For samples with known
or anticipated target compound concentration significantly higher or
lower than the specified amount in these tables, add a pre-sampling
spike amount appropriate to the expected native compound concentration,
but no less than 10 times the EDL. Follow the XAD-2 with cleaned glass
wool and tightly cap both ends of the module. For analysis that include
PAH, use spiked modules within 14 days of preparation. See Table 23-10
of this method for storage conditions.
    <IP_ADDRESS> Sampling Train. Figure 23-1 of this method shows the
complete sampling train. Follow the best practices by maintaining all
sampling train components according to the procedure described in APTD-
0576 Maintenance, Calibration, and Operation of Isokinetic Source-
sampling Equipment (U.S. EPA 1972).
    <IP_ADDRESS> Silica Gel. Weigh several 200 to 300 g portions of silica
gel in an air-tight container to the nearest 0.5 g. Record the total
weight of the silica gel plus container on the outside of each
container. As an alternative, directly weigh the silica gel in its
impinger or sampling holder just prior to sampling.
    <IP_ADDRESS> Filter. Check each filter against light for irregularities
and flaws or pinhole leaks. Pack the filters flat in a clean glass
container. Do not mark filters with ink or any other contaminating
substance.
    8.1.2 Preliminary Determinations. Use the procedures specified in
Section 8.2 of Method 5 of appendix A-3 to 40 CFR part 60.
    <IP_ADDRESS> Sample Volume. Unless otherwise specified in an applicable
rule, permit, or other requirement, sample for a minimum of 2 minutes
at each traverse point. This method recommends sampling a minimum of
2.5 dry standard cubic meters (dscm).
    <IP_ADDRESS> For continuously operating processes, use the same sampling
time at each traverse point. To avoid timekeeping errors, use an
integer, or an integer plus one-half minute, for each traverse point.
    <IP_ADDRESS> For batch processes, determine the minimum operating cycle
duration, dividing the sampling time evenly between the required
numbers of traverse points. After sampling all traverse points once,
sample each point again for the same duration of time per sampling
point in reverse order until the operating cycle is completed. Sample
all traverse points at least once during each test run.
    8.1.3 Preparation of Sampling Train.
    <IP_ADDRESS> During field preparation and assembly of the sampling
train, keep all train openings where contamination can enter sealed
until just prior to assembly or until sampling is about to begin. To
protect the adsorbent module from radiant heat and sunlight, you must
wrap the module with aluminum foil or other suitable material capable
of shielding the module from light. The XAD-2 adsorbent resin
temperature must never exceed 50 [deg]C (122 [deg]F) because thermal
decomposition will occur. Clean and prepare a complete set of sampling
train components that will contact the sample for each sampling run,
including one complete set to be used as a field train proof blank as
described in Section 9.6 of this method.
    <IP_ADDRESS> Place approximately 100 mL of water in the second and third
impingers but leave the first and fourth impingers empty. Transfer
approximately 200 g or more of silica gel from its container to the
fifth impinger. Weigh each impinger and the adsorbent module, including
the fitting caps, to the nearest 0.5 g using the field balance and
record the weight for moisture determination. Remove the aluminum foil
from the adsorbent module before weighing. Keep the module out of
direct sunlight and rewrap the module with foil immediately after
recording the module weight.
    <IP_ADDRESS> Using tweezers or clean disposable surgical gloves, place a
filter in the filter holder. Be sure that the filter is properly
centered, and the gasket properly placed, to prevent the sample gas
stream from circumventing the filter. Check the filter for tears after
completing the assembly.
    <IP_ADDRESS> Prepare the inside of the sampling probe and nozzle by
brushing each component while rinsing three times each with acetone and
toluene. Install the selected nozzle. You may use connecting systems
described in Section 6.1.2 of this method. 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. Assemble the train as
shown in Figure 23-1 of this method. Orient the adsorbent module
vertically so condensed moisture drains into the first impinger. See
APTD-0576 Maintenance, Calibration, and Operation of Isokinetic Source-
sampling Equipment (U.S. EPA 1972) for details.
    <IP_ADDRESS> Turn on the recirculation pump to the adsorbent module and
condenser coil and begin monitoring the temperature of the gas entering
the adsorbent module. Ensure proper temperature of the gas entering the
adsorbent module before proceeding.
    8.1.4 Leak-Check Procedure. Same as Section 8.4 of Method 5 of
appendix A-3 to 40 CFR part 60.
    8.1.5 Sampling Train Operation. Same as Sections 8.5.1 through
8.5.9 of Method 5 of appendix A-3 to 40 CFR part 60.
    <IP_ADDRESS> Monitor the filter temperature sensor and record the filter
temperature during sampling to ensure a sample gas temperature exiting
the filter of 120 [deg]C  14 [deg]C (248 [deg]F  25 [deg]F), or such other temperature as specified by an
applicable subpart of the standards or approved by the Administrator
for an application of this method.
    <IP_ADDRESS> During testing, you must record the temperature of the gas
entering the XAD-2 adsorbent module. The temperature of the gas must
not exceed 20 [deg]C (68 [deg]F) for efficient capture of the target
compounds.
    8.2 Sample Recovery. Begin the cleanup procedure as soon as the
probe is removed from the stack at the end of the sampling period. Seal
the nozzle end of the sampling probe with PTFE tape or clean (e.g.,
toluene rinsed) aluminum foil. This method recommends using clean
glassware prepared following Section <IP_ADDRESS> of this method for each
sample set in a test series.
    8.2.1 When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe. Conduct a post-test leak
check. Remove the probe from the train and close off both ends with
PTFE tape or clean aluminum foil. Seal off the inlet to the train with
PTFE tape, a ground glass cap, or clean aluminum foil.
    8.2.2 Transfer the probe and impinger assembly to the cleanup area.
This method recommends cleaning and enclosing this area to minimize the
chances of losing or contaminating the sample. To avoid sample
contamination and unnecessary exposure to toxic chemicals, smoking or
eating in the sample recovery area shall not be allowed.
    8.2.3 Inspect the train prior to and during disassembly. Note and
record

any abnormal conditions (e.g., broken filters, colored impinger
liquid). Recover and prepare samples for shipping as follows in
Sections 8.2.4 through 8.2.12 of this method.
    8.2.4 Container No. 1. Either seal the filter holder or carefully
remove the filter from the filter holder and place it in its identified
container. If it is necessary to remove the filter, use a pair of
cleaned tweezers to handle the filter. If necessary fold the filter
such that the particulate cake is inside the fold. Carefully transfer
to the container any particulate matter and filter fibers that adhere
to the filter holder gasket by using a dry inert bristle brush and a
sharp-edged blade. Seal the container and store cool (<= 20  3 [deg]C, 68  5 [deg]F) for transport to the
laboratory.
    8.2.5 Adsorbent Module Sample. Remove the module from the train,
tightly cover both ends with fitting caps and PTFE tape, remove the
foil, drain the recirculating water from the module, weigh and record
the module weight, and label the adsorbent module. Moisture measurement
in the field using the Method 23 train requires weighing the adsorbent
module before the sampling run and after sampling as part of the sample
recovery.
    8.2.6 Container No. 2. Quantitatively recover material deposited in
the nozzle, the front half of the filter holder, and the cyclone, if
used, by brushing while rinsing three times with acetone followed by
three rinses with toluene. Collect all the rinses in Container No. 2.
    8.2.7 Rinse the back half of the filter holder three times with
acetone followed by three rinses with toluene. Rinse the sample
transfer line between the filter and the condenser three times with
acetone followed by three rinses with toluene. If using a separate
condenser and adsorbent module, rinse the condenser three times with
acetone followed by three rinses with toluene. Collect all the rinses
in Container No. 2 and mark the level of the liquid on the container.
    8.2.8 Moisture Weight. Weigh the adsorbent module, impingers, and
silica gel impinger to within  0.5 g using the field
balance and record the weights. This information is required to
calculate the moisture content of the effluent gas. For PCDD/PCDF-only
measurements, discard the liquid after measuring and recording the
weight.
    8.2.9 Container No. 3. You must save and analyze impinger water
samples if PAHs and/or PCBs are the target compounds. Quantitatively
recover impinger water samples for analysis if PAHs and/or PCBs are the
target compounds by rinsing three times with acetone followed by three
rinses with toluene. Collect impinger water and rinses in Container No.
3 and mark the level of the liquid on the container.
    8.2.10 Silica Gel. Note the color of the indicating silica gel to
determine if it has been completely spent and report its condition on
the field data sheet.
    8.2.11 Field Sample Handling, Preservation, Storage, and Transport.
Store all field samples temporarily in cool (<= 20  3
[deg]C, 68  5 [deg]F) and dark conditions prior to
transport to the laboratory. Ship samples cool (<= 20  3
[deg]C, 68  5 [deg]F), shielded from ultraviolet light. In
addition, follow the procedures in ASTM D6911-15 (Guide for Packaging
and Shipping Environmental Samples for Laboratory Analysis) for all
samples, where appropriate. To avoid contamination of the samples, pay
special attention to cleanliness during transport, field handling,
sampling, recovery, and laboratory analysis, as well as during
preparation of the adsorbent cartridges.
    8.2.12 Sample Custody. Proper procedures and documentation for
sample chain of custody are critical to ensuring data integrity. Follow
the chain of custody procedures in ASTM D4840-99(2018)e1 (Standard
Guide for Sample Chain-of-Custody Procedures) for all samples
(including field samples and blanks).
    8.3 Sample Storage Conditions and Laboratory Hold Times.
    8.3.1 Table 23-10 of this method summarizes the sample storage
conditions and laboratory hold times.
    8.3.2 Store sampling train rinses and filter samples in the dark at
6 [deg]C (43 [deg]F) or less from the time the laboratory receives the
samples until analysis.
    8.3.3 You may store adsorbent samples for PCDDs/PCDFs or PCBs prior
to extraction in the dark at 6 [deg]C (43 [deg]F) or less for up to one
year from the time the laboratory receives the samples.
    8.3.4 Protect adsorbent samples destined for PAH analysis from
ultraviolet light. You may store adsorbent samples for PAH analysis at
6 [deg]C (43 [deg]F) or less for up to 30 days from the time the
laboratory receives the samples.
    8.3.5 Analyze PAH extracts within 45 days of extraction.
    8.3.6 You may store sample aliquots including archived extracts of
PCDD/PCDF, PAH and/or PCB samples in the dark at -10 [deg]C (14 [deg]F)
or less for up to one year.

9.0 Quality Control

    Note:  In recognition of advances that are occurring in sampling
and analytical technology, and to allow the test team to overcome
analyte sensitivity and matrix interferences, this method allows
certain options to increase sample collection volume and to improve
separations and the quality of the analysis results for target
analytes. It is the laboratory's responsibility to establish the
conditions for optimum sample extraction, cleanup, and concentration
to meet the performance criteria in this method. However, you may
not change the fundamental sampling and analysis techniques,
isokinetic sampling with an adsorbent collection media followed by
sample extraction, and HRMS detection and isotopic dilution
quantification procedures. Section 13 of this method specifies the
performance criteria to ensure that options employed for a sample
set and analytes of interest are equal to or better than the
specificity of the techniques in this method. This method recommends
performing a media blank (i.e., batch blank) assessment to evaluate
an individual laboratory's performance against the performance
criteria in this method. At a minimum, evaluate changes within the
alternatives allowed in this method using a media blank sample to
re-demonstrate that the performance criteria are achieved.

    9.1 Record and report data and information that will allow an
independent reviewer to validate the determination of each target
compound concentration. At a minimum, record and report the data as
described in Sections 9.1.1 through 9.1.7 of this method.
    9.1.1 Sample numbers and other sample identifiers. Each sample must
have a unique identifier.
    9.1.2 Field sample volume.
    9.1.3 Field sampling date.
    9.1.4 Extraction dates.
    9.1.5 Analysis dates and times.
    9.1.6 Analysis sequence/run chronology.
    9.1.7 Quantitation Reports.
    <IP_ADDRESS> This method does not consider EPC-flagged data to be zero
concentrations. Calculate the EPC separately for each quantitation ion,
if present, and report the lower value as the EPC.
    <IP_ADDRESS> In determining compliance with any PCDD and PCDF standard
developed using zero for values that are below the detection level of
the method, including federal emission standards using Method 23
promulgated under 40 CFR parts 60 and 63 prior to [DATE OF PUBLICATION
OF THE FINAL RULE], use zero for the determination of total and
weighted concentrations when the target compound is not detected. For
all other circumstances, unless otherwise specified in applicable
regulations, permits, or other requirements, when a target compound is
measured at or below EDL, use EDL as the concentration for calculating
compliance.
    <IP_ADDRESS> You must report your EDLs with analysis results.

    9.1.8 Performance criteria results (See Section 13 of this method).
    9.2 Isotopically Labeled Spike Recovery Results.
    9.2.1 Pre-sampling Adsorbent Spike and Pre-extraction Filter Spike
Recoveries. Pre-sampling adsorbent and pre-extraction filter spike
recoveries must demonstrate on a per sample basis that recovery of the
labeled standard achieved the requirements in Section 13 of this
method. Recoveries below the acceptable range for the pre-sampling
spikes may be an indication of breakthrough in the sampling train.
    <IP_ADDRESS> If the recovery of all the pre-sampling adsorbent spike
standards is below 70 percent, the sampling runs are not valid, and you
must repeat the invalid runs. As an alternative, you do not have to
repeat the invalid sampling runs if the average pre-sampling adsorbent
spike recovery is 25 percent or more and you divide the final results
by the average fraction of pre-sampling adsorbent spike recovery.
    <IP_ADDRESS> If the recovery of the pre-extraction filter spike is below
70 percent, the filter sampling extraction recovery is not valid, and
you must flag the test run results.
    9.2.2 Pre-extraction Spike Recoveries. Pre-extraction spike
recoveries must demonstrate on a per sample basis that recovery of the
labeled standard achieved the requirements in Section 13 of this
method. Recoveries below the acceptable range for pre-extraction spikes
are an indication that sample preparation procedures did not adequately
address sample and or sample matrix processing to recover native target
compounds.
    9.2.3 Pre-analysis Spike Recoveries. Pre-analysis spike recoveries
must demonstrate on a per sample basis that adequate labeled standard
signal meets the requirements in Section 13 of this method. Add pre-
analysis standards to every sample (including blanks, quality control
samples, and calibration solutions) in a known concentration. You may
analyze archive samples to attempt meeting requirements for the
compounds that do not meet the pre-analysis recovery criteria.
Recoveries below the acceptable range for pre-analysis spikes are an
indication that sample injection or instrument drift has failed beyond
the ability to correct using pre-analysis standard results.
    9.3 Capillary GC columns must be able to achieve the separation
resolution specified in Sections 13.3, 13.4, and/or 13.5 of this method
for the target compounds analyzed in test samples.
    9.4 Batch Blank Samples. Evaluate chromatographic separation
performance, spiking errors, and continuing calibration checks using a
batch blank sample prepared from typical filter and absorbent media,
spiked with isotopically labeled compounds and extracted identically to
the procedures used to prepare samples. Analyze batch blank samples at
least once during each analytical sequence or every 24 hours, whichever
period is shorter. Section 13.2 of this method describes the
performance criteria for field train proof blank assessment samples and
batch blank samples.
    9.5 Detection Limits. Calculate the EDL using the equation in
Section 12.11 of this method. If the field train proof blank or the
batch blank results are above the EDL, calculate and report the test-
specific and compound-specific DLs equal to the sum of the EDL and the
larger of the batch or field train proof blank results. If the field
train proof blank and the batch blank results are equal to or less than
the EDL, report the test-specific and compound-specific DLs as the EDL.
    9.6 Field Train Proof Blank Assessment. Conduct at least one field
train proof blank for each test series at a single facility. A field
train proof blank train consists of a fully assembled train at the
sampling site. Prepare and assemble the blank train in a manner
identical to that described in Sections 8.1.3 and 8.1.4 of this method.
The blank train must remain assembled for the same average amount of
time samples are collected. Recover the blank train as described in
Section 8.2 of this method. Follow all subsequent steps for blank train
sample preparation and analysis used for field train samples including
data reporting.

10.0 Calibration and Standardization

    10.1 Sampling System. Same as Sections 6.1 and 10.1 through 10.7 of
Method 5 of appendix A-3 to 40 CFR part 60.
    10.2 HRGC/HRMS System.
    10.2.1 Mass Resolution. Tune the HRMS instrument to a mass
resolution (R) of at least 10,000 at 5 percent of the peak height or
25,000 at 50 percent of the peak height where resolution is calculated
as an R = M/[Delta]M, where M is the resolving power and [Delta]M is
the peak width. You may use peak matching and the chosen perfluoro-
kerosene (PFK) or perfluorotributylamine (FC43) reference peak to
verify that the exact mass is within 5 ppm of the required value.
Assess the resolution at three m/z ranges representing the low, mid and
high m/z range of the masses used to measure the target compound class.
    10.2.2 Initial Calibration. Calibrate the HRGC/HRMS system using a
minimum of five concentrations over a range that brackets typical field
sample concentrations and the concentration of isotopically labeled
standards in spiked samples. Tables 23-11, 23-12, and/or 23-13 of this
method, as applicable to the compound classes analyzed, show the
calibration concentrations recommended by this method. Perform
calibration and subsequent analyses on an absolute mass (pg/microliter
([mu]L)) basis. The recommended calibration range ensures isotopic
labels can be accurately distinguished from native compounds and
provides the initial response factors that are corrected by isotopic
recovery.
    <IP_ADDRESS> Lock Channels. Tables 23-4, 23-5, and 23-6 of this method