[Federal Register Volume 82, Number 173 (Friday, September 8, 2017)]
[Proposed Rules]
[Pages 42508-42530]
[FR Doc No: 2017-18425]

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 51

[EPA-HQ-OAR-2016-0456; FRL-9966-75-OAR]
RIN 2060-AS91

Method 202--Dry Impinger Method for Determining Condensable
Particulate Emissions From Stationary Sources

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule.

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SUMMARY: In this action, the Environmental Protection Agency (EPA)
proposes editorial and technical revisions to the EPA's Method 202--Dry
Impinger Method for Determining Condensable Particulate Emissions from
Stationary Sources to improve the consistency in results achieved
across the testing community.

DATES:
    Comments. Comments must be received on or before November 7, 2017.
    Public Hearing. If a public hearing is requested by September 18,
2017, then we will hold a public hearing on October 10, 2017 at the
location described in the ADDRESSES section. The last day to pre-
register in advance to speak at the public hearing will be October 6,
2017.

ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-
OAR-2016-0456, to the Federal eRulemaking Portal at http://www.regulations.gov. Follow the online instructions for submitting
comments. Once submitted, comments cannot be edited or withdrawn. 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 http://www2.epa.gov/dockets/commenting-epa-dockets.
    Public Hearing. If a public hearing is requested, it will be held
at EPA Headquarters, William Jefferson Clinton East Building, 1201
Constitution Avenue NW., Washington, DC 20004. If a public hearing is
requested, then we will provide details about the public hearing on our
Web site at: https://www.epa.gov/emc/emc-proposed-test-methods. The EPA
does not intend to publish another document in the Federal Register
announcing any updates on the request for a public hearing. Please
contact Mr. Ned Shappley at<PHONE_NUMBER> or by email at
<EMAIL_ADDRESS>to request a public hearing, to register to speak
at the public hearing, or to inquire as to whether a public hearing
will be held.
    Docket: All documents in the docket are listed in the http://www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI 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 http://www.regulations.gov or in hard copy at the EPA Docket Center,
EPA/DC, EPA WJC West Building, Room 3334, 1301 Constitution Avenue 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>.

FOR FURTHER INFORMATION CONTACT: Mr. Ned Shappley, Office of Air
Quality Planning and Standards, Air Quality Assessment Division,
Measurement Technology Group (E143-02), Environmental Protection
Agency, Research Triangle Park, NC 27711; telephone number: (919) 541-
5225; fax number:<PHONE_NUMBER>; email address<EMAIL_ADDRESS>
SUPPLEMENTARY INFORMATION: The following topics are discussed in this
preamble.

I. General Information

    A. Does this action apply to me?
    B. What should I consider as I prepare my comments?

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

II. Background

III. Summary of Proposed Revisions

    A. Blank Correction
    B. Procedures for the Field Train Proof Blank
    C. Configuration of the Vertical Condenser
    D. Use of Graduated Cylinders
    E. Limitations of Method 202
    F. Required Use of Method 202
    G. Sample Container Material
    H. Weighing Containers
    I. Laboratory Analytical Balance Requirements
    J. Field Balance Requirements
    K. pH Measurement
    L. Glassware Cleaning Procedures
    M. Reagent Blanks
    N. Nitrogen Purge Requirements
    O. Data Record Requirements
    P. Method Detection Limits
    Q. Alternative Blank Procedure and Correction Value

IV. Request for Comments

V. 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?

    This action applies to you if you operate a stationary source that
is subject to applicable requirements to control or measure condensable
particulate matter (CPM) emissions where EPA Method 202 is incorporated
as a component of the applicable test method. In addition, this action
applies to you if federal, state, tribal, or local agencies take
certain additional independent actions. For example, this action
applies to sources through actions by state and local agencies that
implement CPM control measures to attain the National Ambient Air
Quality Standards (NAAQS) for particles less than 2.5 micrometers in
diameter (PM2.5) and specify the use of EPA Method 202 to
demonstrate compliance with the control measures. State, tribal, and
local agencies that specify the use of EPA Method 202 would have to
implement the following requirements: (1) Adopt this method in rules or
permits (either by incorporation by reference or by duplicating the
method in its entirety) and (2) promulgate an emissions limit requiring
the use of EPA Method 202 (or a method that incorporates EPA Method
202). This action also applies to stationary sources that are required
to meet applicable CPM requirements established through federal, state,
or tribal rules or permitting programs such as New Source Performance
Standards and New Source Review (NSR), which specify the use of EPA
Method 202 to demonstrate compliance with the control measures.
    The source categories and entities potentially affected include,
but are not limited to, the following:

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                Category                     NAICS \a\                                    Examples of regulated entities
--------------------------------------------------------------------------------------------------------------------------------------------------------
Industry................................          332410  Fossil fuel steam generators.
                                                  332410  Industrial, commercial, institutional steam generating units.
                                                  332410  Electricity generating units.
                                                  324110  Petroleum refineries.
                                                  562213  Municipal waste combustors.
                                                  322110  Pulp and paper mills.
                                                  325188  Sulfuric acid plants.
                                                  327310  Portland cement plants.
                                                  327410  Lime manufacturing plants.
                                                  211111  Coal preparation plants.
                                                  212111
                                                  212112
                                                  212113
                                                  331312  Primary and secondary aluminum plants.
                                                  331314
                                                  331111  Iron and steel plants.
                                                  331513
                                                  321219  Plywood and reconstituted products plants.
                                                  321211
                                                  321212
--------------------------------------------------------------------------------------------------------------------------------------------------------
\a\ North American Industrial Classification System.

    If you have any questions regarding the applicability of the
proposed changes to Method 202, contact the person listed in the
preceding FOR FURTHER INFORMATION CONTACT section.

B. What should I consider as I prepare my comments?

1. 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 40 Code of
Federal Regulations (CFR) part 2.
    Do not submit information that you consider to be CBI or otherwise
protected through http://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-2016-0456.
    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.
2. Docket
    The docket number for the Method 202 revisions is Docket ID No.
EPA-HQ-OAR-2016-0456.

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

    World Wide Web (WWW). In addition to being available in the docket,
an electronic copy of the proposed method revisions is available on the
Air Emission Measurement Center (EMC) Web site at https://www.epa.gov/emc/emc-proposed-test-methods.

II. Background

    Section 110 of the Clean Air Act, as amended (42 U.S.C. 7410),
requires state and local air pollution control agencies to develop, and
submit for EPA approval, State Implementation Plans (SIPs) that provide
for the attainment, maintenance, and enforcement of the NAAQS in each
air quality control region (or portion thereof) within each state. The
emissions inventory and analyses used in the state's attainment
demonstrations must consider PM2.5 and particles less than
10 micrometers in diameter (PM10) emissions from stationary
sources that are significant contributors of primary PM10
and PM2.5 emissions. Primary or direct PM emissions are the
solid particles or liquid droplets emitted directly from an air
emissions source or activity and the gaseous emissions or liquid
droplets from an air emissions source or activity that condense to form
PM or liquid droplets at ambient temperatures.
    Subpart A of 40 CFR part 51 (Requirements for Preparation,
Adoption, and Submittal of Implementation Plans) defines primary
PM2.5 and PM10 as including both the filterable
and condensable fractions of PM. Filterable PM consists of those
particles that are directly emitted by a source as a solid or liquid at
the stack (or similar release conditions) and captured on the filter of
a stack test sampling train. Condensable PM is the material that is in
vapor phase at stack conditions but condenses and/or reacts upon
cooling and dilution in the ambient air to form solid or liquid PM
immediately after discharge from the stack. In response to the need to
quantify primary PM10 and PM2.5 emissions from
stationary sources, the EPA previously developed and promulgated Method
202 (Determination of Condensable Particulate Emissions from Stationary
Sources) in 40 CFR part 51, appendix M (Recommended Test Methods for
State Implementation Plans).
    Specifically, on December 17, 1991 (56 FR 65433), the EPA first
promulgated Method 202 to provide a test method for measuring CPM from
stationary sources. Method 202, as promulgated in 1991, used water-
filled impingers to cool, condense, and collect materials that are
vaporous at stack conditions and become solid or liquid PM at ambient
air temperatures. Method 202, as promulgated in 1991, contains several
optional procedures that were intended to accommodate the various test
methods in use by state and local regulatory entities at the time
Method 202 was being developed.
    When conducted consistently and carefully, this version of the
method provided improved precision for most emission sources, and has
been successfully implemented in regulatory programs where the emission
limits and compliance demonstrations are established based on a
consistent application of Method 202 and its associated options.
However, when the same emission source is tested using different
combinations of the optional procedures within the method, there were
variations in the measured CPM emissions. Additionally, during
validation of the method, we determined that sulfur dioxide
(SO2) gas (a typical component of emissions from several
types of stationary sources) can be absorbed partially in the impinger
solutions and can react chemically to form sulfuric acid. This sulfuric
acid ``artifact'' is not related to the primary emission of CPM from
the source, but may be counted erroneously as CPM when using Method
202. The EPA conducted additional studies to further examine the
mechanism and the effects of sulfuric acid formation. The results of
our 1989 laboratory study and field evaluation commissioned to evaluate
the impinger approach can be found in ``Laboratory and Field Evaluation
of the EPA Method 5 Impinger Catch for Measuring Condensible Matter
from Stationary Sources.'' The report of that work is available in the
docket as EPA-HQ-OAR-2016-0456-0001. Essentially, the 1989 study
verified the need for a nitrogen purge when SO2 is present
in stack gas and also provided guidance for analyzing the collected
samples. In 2005, an EPA contractor conducted a second study,
``Laboratory Evaluation of Method 202 to Determine Fate of
SO2 in Impinger Water,'' that replicated some of the earlier
EPA work and addressed some additional issues. The report of that work
is available in the docket as EPA-HQ-OAR-2016-0456-0002. In 2009, an
EPA contractor conducted a third study, ``Evaluation and Improvement of
Condensable Particulate Matter Measurement,'' that presents the results
of a laboratory evaluation of a dry impinger modification to Method
202. The report of that work is available in the docket as EPA-HQ-OAR-
2016-0456-0003.
    In 2010, the EPA promulgated amendments to Method 202 (75 FR 80118)
to improve the measurement of fine PM emissions. The final amendments
revised the sample collection and recovery procedures of the method to:
(1) Reduce the potential for CPM formation due to oxidation of
dissolved SO2 when using Method 202 (as promulgated in 1991)
and (2) promote consistent application of the method by eliminating
most of the hardware and analytical options in the existing method. The
most significant procedural changes were the addition of a condenser
prior to the first impinger, the removal of water from the two
impingers between the condenser and the CPM filter, and the addition of
the requirement for a post-test nitrogen purge. These revisions
increased the precision of Method 202 and reduced potential positive
and negative biases by removal of the myriad of options and elimination
of water in the two impingers, which significantly improved the
consistency in the measurements obtained between source tests performed
under different regulatory authorities.
    On April 8, 2014, the EPA issued interim guidance on the treatment
of CPM results in the Prevention of Significant Deterioration (PSD) and
Nonattainment NSR Permitting Programs. The purpose of this guidance was
to address concerns that CPM test results obtained with the method
could include a positive bias that results in the overestimation of
emissions due to the potential for blank contamination associated with
the implementation of Method 202. In this interim guidance, we
recommend to air agencies and permit applicants that it is appropriate
on an interim basis to allow major source permit applicants to depart
from one aspect of Method 202, specifically the current upper limit of
2.0 milligrams (mg) for the field train recovery blank. Consistent with
this guidance, during the prescribed interim period, air agencies may
allow permit applicants to use field train proof blanks, in lieu of the
field train recovery blanks, and blank values as high as 5.1 mg can
then

be used in the calculation of CPM emissions. As part of this guidance,
the EPA announced plans to issue guidance on best practices for Method
202 implementation and to revise Method 202 as necessary. In addition,
this guidance stated that the interim guidance period will end on the
effective date of any revision that the EPA may make for Method 202
regarding the use of blanks in the field train on individual test
results. We intend that the interim guidance will no longer apply as of
the effective date of the final rule resulting from this proposal. A
copy of the interim guidance is available in the docket (EPA-HQ-OAR-
2016-0456-003) and on the EMC Web site at https://www3.epa.gov/ttn/emc/methods/psdnsrinterimcmpmemo4814.pdf.
    On March 10, 2016, the EPA released the EPA Method 202 Best
Practices Handbook. This handbook provides quality control procedures
for evaluating the cause of blank contamination and practices to reduce
contamination, so that testers may achieve the expected results when
using Method 202. A copy of this handbook is available in the docket as
EPA-HQ-OAR-2016-0456-004 and on the EMC Web site at https://www3.epa.gov/ttn/emc/methods/m202-best-practices-handbook.pdf.

III. Summary of Proposed Revisions

    In this action, we are proposing technical revisions and editorial
changes to clarify and update the requirements and procedures specified
in Method 202. Proposed editorial changes include correcting
inconsistent terminology, improving readability, and simplifying text
to aid in consistent implementation of the method. Proposed technical
revisions are discussed below.

A. Blank Correction

    In this action, we propose to replace the field train recovery
blank requirement used to determine the blank correction (up to 2.0 mg)
with a field train proof blank requirement. In the current version of
Method 202, the result of the field train recovery blank is used as the
basis for the blank correction (up to 2.0 mg). Specifically, we propose
to revise section <IP_ADDRESS> (and renumber as section <IP_ADDRESS>) to require
conducting a field train proof blank to demonstrate the cleanliness of
the sampling train. We propose to revise sections 9.9, 12.1, and
12.2.2, and Figures 4, 5, and 6 to replace the field train recovery
blank with the field train proof blank. We also propose to remove the
field train recovery blank requirement and the associated text in
section 9.10 from the method.
    The EPA received technical information and recommendations from the
National Council on Air and Stream Improvement (NCASI) supporting the
use of a field train proof blank to evaluate method blank correction.
The EPA believes the updated field train proof blank is a better
indicator of the total systematic blank error for Method 202 sample
runs. Under the proposed amendments, a clean and prepared sampling
train is transported and fully assembled at the sampling location, leak
checked, left in place without collecting a sample, purged with
nitrogen, and recovered in the same manner as a sample collection
train. All components of the Method 202 sampling train must be included
in the field train proof blank to properly quantify the blank value.
The field train proof blank represents the systematic bias associated
with all of the uncertainty from the reagents, sampling media,
glassware preparation, recovery and analysis procedures, environmental
contamination, leak checks, and test crew sample handling.

B. Procedures for the Field Train Proof Blank

    In the current version of Method 202, the setup and recovery
procedures for the field train proof blank are incomplete. We are
proposing the following revisions for the field train proof blank setup
and recovery procedures specified in sections <IP_ADDRESS>, <IP_ADDRESS>.1,
<IP_ADDRESS>.2, and 9.9:
     Adding a full sampling train setup including the front
half of the train for collecting filterable PM, probe extension and/or
transfer line, condenser, impingers, and filter used to collect the
CPM.
     Requiring that the entire filterable PM and CPM sampling
train is transported to and assembled at the sampling location.
     Adding pre- and post-test leak checks.
     Exposing the assembled field train proof blank sampling
train to the sampling environment for the same duration as the test
runs to be conducted.
     Performing a post-test nitrogen purge of the field train
proof blank.
     Requiring recovery of the sampling train components
identical to how field samples are recovered.
    In this action, we are also proposing to add section <IP_ADDRESS>.3 to
include procedures for handling the CPM filter from the field train
proof blank. We believe that the proposed revisions will generate blank
samples that duplicate sources of possible contamination experienced by
the field samples.

C. Configuration of the Vertical Condenser

    Currently, Method 202 does not specify the orientation of the
moisture condenser located before the first impinger of the sampling
train. Although the sampling trains depicted in Figures 1 through 3
show the placement of the condenser, the incline of the condenser in
the figures is not specified.
    When the condenser is installed horizontally or at an angle,
condensed moisture may pool in the condenser coils, increasing the
potential for SO2 to dissolve into that water and slowly
oxidize to form CPM that is not related to the primary emission of CPM
from the source. We believe that requiring the condenser to be
installed vertically will minimize pooling of condensed moisture in the
condenser coils, thereby reducing the potential for this bias and
promoting consistency in CPM measurement.
    In this action, we propose revisions to sections 2.1.2, 6.1.2, and
8.4.1 to require that the moisture condenser be installed in a vertical
orientation. We propose to revise Figures 1 through 3 to depict the
condenser in the vertical position consistent with the changes to the
method text. We also propose to revise section 6.1.4 (and renumber as
section 6.1.3) to allow other equipment options to purge the water in
the dropout impinger.

D. Use of Graduated Cylinders

    Currently, Method 202 allows the use of a graduated cylinder to
measure the volume of moisture collected in the impingers and the
silica gel trap for the purpose of calculating the moisture content of
the effluent gas. We believe that using a graduated cylinder to measure
the accumulated water is not sensitive enough to measure the moisture
and potentially adds an unnecessary additional source for potential
loss of condensable particulate residual mass in samples measured by
Method 202. Therefore, we propose to revise section <IP_ADDRESS> (and
renumber as section 8.5.3) to remove the option to use graduated
cylinders and to require use of a balance to determine the mass of each
impinger for the purpose of measuring the moisture collected during
sampling. Instructions to weigh each impinger before testing, which is
a necessary step for determining the amount of moisture collected when
using a balance, are proposed for relocation to section 8.4.5. We also
propose to make accompanying

revisions in sections <IP_ADDRESS>, <IP_ADDRESS>, and 11.1(b) to clarify the
procedures for weighing the impingers and captured moisture. Sections
related to transferring the moisture-trap impinger and silica gel
impinger contents in sample containers for measurement using graduated
cylinders are proposed to be removed.

E. Limitations of Method 202

    High moisture in the sampled gas stream can result in the
accumulation of SO2 in the collected moisture resulting in a
positive bias for CPM measurements. As the moisture accumulates in the
sample impingers, the method performs similarly to the original version
of Method 202 where SO2 in the effluent could react in the
condensed moisture and form sulfuric acid that may be counted
erroneously as CPM. In addition, longer sampling times coupled with
high moisture can (in the water-contained impingers) allow more
SO2 conversion to CPM since the conversion of SO2
to CPM has a relatively slow reaction rate.
    Section <IP_ADDRESS> of Method 202 recommends removing moisture from the
sampling train during the test run when the amount of moisture
collected is greater than half the capacity of the water dropout
impinger or the moisture level of the back-up impinger is above the
impinger tip.
    Longer sampling run times also delay the start of the post-test
nitrogen purge. The post-test nitrogen purge is designed to remove
dissolved gasses from the accumulated moisture and thus reduce the
potential chemical reactions. In this action, we propose to amend
Method 202 by adding a recommendation in section 1.5 to limit the
sampling time to 2 hours for Method 202 testing when excessive moisture
collection is expected. We also propose revisions to section <IP_ADDRESS> to
specify that if accumulated water exceeds half of the capacity of the
water dropout impinger, or if water accumulates in the back-up impinger
sufficient to cover the impinger tip, the impinger(s) must be removed
and replaced with new pre-weighed impingers and all resulting impingers
must be weighed, purged and recovered following the procedures of the
method.
    The current version of Method 202 also prohibits the use of certain
filterable particulate test methods in conjunction with Method 202. In
this action, we propose revisions to section 1.4 to state only the
acceptable filterable particulate test methods and to include a note
that you must maintain the gas filtration temperature as specified in
the filterable PM test method unless otherwise specified by an
applicable subpart.

F. Required Use of Method 202

    Condensable PM is formed from gaseous materials that condense and/
or react upon cooling and dilution in the ambient air. Method 202
requires the use of a particulate sampling method (e.g., Method 5, 17,
or 201A) to separately collect the filterable PM from CPM.
    Filterable PM methods that collect particulate out-of-stack have
specified filter temperature requirements and require the addition of a
Method 202 sampling train to collect CPM. Filterable PM methods that
employ in-stack filters collect particulate material at the source gas
temperature.
    If the temperature of the filterable PM sampling equipment,
including the filter, meets Method 202 temperature requirements (i.e.,
<=30 [deg]C (85 [deg]F)), both filterable and CPM are collected
together on the filter and CPM is not quantified independently but
rather as total particulate, total PM10, or total
PM2.5 depending on the filterable collection method.
    In this action, we propose to revise section 1.2 to clearly state
that, if the sample gas filtration temperature never exceeds 30 [deg]C
(85[emsp14][deg]F), then Method 202 is not required to measure total
primary PM because the CPM would be collected with the filterable PM.

G. Sample Container Material

    Currently, section 6.2.1(d) of Method 202 specifies the use of
amber glass sample bottles for sample recovery. In this action, we
propose to revise section 6.2.1(d) to allow the use of sample
containers made from other non-reactive materials (e.g., high density
polyethylene (HDPE), polytetrafluoroethylene (PTFE)) as an alternative
to amber glass bottles for inorganic (aqueous) samples. We also propose
to revise sections 6.2.1(d), <IP_ADDRESS>, <IP_ADDRESS>, and <IP_ADDRESS> to require
cleaning of all sample containers according to the procedures in
section 8.4 prior to use.
    Although we are proposing to revise the method to allow use of
polymer or glass sample containers for inorganic samples, we continue
to require glass containers for organic samples. The proposed revisions
would provide testers with an alternative for storing inorganic samples
to avoid this potential source of contamination.

H. Weighing Containers

    Currently, section 6.2.2(b) of Method 202 specifies that glass
evaporation vials, fluoropolymer beaker liners, or aluminum weighing
tins can be used for final sample evaporation and weighing. In this
action, we propose to include a list of acceptable weighing containers
that includes fluoropolymer beaker liners and other vessels that have
low mass and are unreactive to the sample and the atmosphere.
Laboratories have reported that aluminum weighing tins may oxidize in
contact with some sample matrices. The heavier weight of some glass
beakers or containers may cause difficulty with measurement of trace
amounts of residual mass. We propose to revise sections 6.2.2(b),
<IP_ADDRESS>, 11.2.3, 11.2.4, 11.2.5, and 11.2.6 to remove the connotation
of sampling ``tin'' as an implicit approval of aluminum tins.

I. Laboratory Analytical Balance Requirements

    We propose additional quality control requirements for analytical
balance use. Currently, section 9.6 of Method 202 requires calibration
of the analytical balance on each day that samples are weighed, and
section 10.3 of the Method 202 Best Practices Handbook provides
additional steps that stack testers can use to improve consistency in
analytical balance measurements. In this action, we propose to amend
section 9.6 to specify the correct mass standard to use for the
Analytical Calibration Check, specifications for the temperature and
humidity control in weighing areas and requirements for balance
calibration checks that approximately match the sample measurements to
include the following requirements:
     The laboratory analytical balance must be maintained at a
constant temperature of 20 [deg]C  3 [deg]C
(68[emsp14][deg]F  5[emsp14][deg]F).
     The relative humidity at the location of the laboratory
analytical balance must be maintained at 35 to 50 percent, with the
exception that if the relative humidity is lower than 35 percent, the
relative humidity must be maintained within 10 percent
during sample weighing.
     The results of the calibration check of the laboratory
analytical balance must be within 0.05 percent of the applicable
certified weight.
     The laboratory analytical balance must be checked each day
it is used for gravimetric measurements by weighing at least one ASTM
E617-13 Class 2 tolerance (or better) calibration weight that
corresponds to 50 to 150 percent of the weight of one filter or between
1 gram (g) and 5 g. If the scale cannot reproduce the value of the
calibration weight to within 0.5 mg of the certified mass, perform
corrective measures and

conduct the multipoint calibration before use.

J. Field Balance Requirements

    In this action, we propose to correct section 9.4 to specify the
mass standard with which to conduct the field balance calibration
check. We believe that this additional requirement is necessary to
increase consistency of Method 202 moisture sample measurements. We
propose the requirement that the field balance calibration check be
performed daily with an ASTM E617-13 Class 6 (or better) weight.

K. pH Measurement

    In sections 6.2.2(h) and <IP_ADDRESS> of the current method, pH
measurement by pH meter or colorimetric pH indicator is allowable for
the titration procedure. While the use of a colorimetric (e.g.,
Phenolphthalein) indicator is an acceptable technique for accurately
determining the end-point of an acid-base titration, we are concerned
that determining the pH using colorimetric pH indicators may introduce
additional error in the measurement of CPM due to over-titration.
    In this action, we propose to amend sections 6.2.2(h) and <IP_ADDRESS>
to remove the option of using a colorimetric pH indicator and require
the use of a pH meter whose calibration has been checked immediately
prior to the titration step. We also propose to correct the CPM Sample
Processing Flow Chart for sample analysis (Figure 8). We believe these
revisions will increase the consistency and comparability of Method 202
results between source tests.

L. Glassware Cleaning Procedures

    To obtain reliable CPM data using Method 202 for PSD and NSR
permits, residual mass from sampling and analysis equipment must be
minimized.
    In this action, we propose the following amendments to clarify
equipment and glassware cleaning in section 8.4 of Method 202,
including:
     Adding a specification that all glassware used in the
implementation of Method 202, including the impinger train and sample
containers, should be cleaned sufficiently to meet the blank correction
maximum limit of 2.0 mg in section 9.9.
     Removing the statement referencing cleaning silicone
grease so that it is not mistakenly viewed as acceptable to use such
grease in Method 202 sampling trains.
     Removing the requirement that glassware must be baked
after cleaning (although the EPA is proposing to remove the baking
requirement, we highly recommended baking of glassware as discussed in
the EPA Method 202 Best Practices Handbook).
     Removing the option to use the field train proof blank as
an alternative to baking since the field train proof blank is being
proposed as a requirement of Method 202.
     Adding a recommended procedure for cleaning the probe
liners by heating for a period of at least 3 hours at the maximum
practical temperature.
    These proposed revisions make the glassware cleaning procedures
performance-based, clarify the requirements, and provide testers with
an additional method for ensuring cleanliness of the probe liners.

M. Reagent Blanks

    Currently, Method 202 specifies a volume of 150 milliliters (mL)
for performing reagent blank analyses and specifies that field reagent
blanks are optional. In this action, we propose to revise section 9.7
to specify a minimum volume of 200 mL for these field reagent blank
volumes and to revise section 9.8 to require analysis of field reagent
blanks in the performance of Method 202. We also propose to make
accompanying revisions to sections <IP_ADDRESS>, <IP_ADDRESS>, <IP_ADDRESS>, 11.2.4,
11.2.5, and 11.2.6.
    The original solvent blank volume was intended to represent amounts
typically used during sample recovery. A larger reagent blank volume is
necessary to quantify residual mass using the analytical balance
specified in Method 202 with a sensitivity of 0.0001 g (0.1 mg). These
proposed revisions are based on recommendations received from state
agencies. This change to the method quality control quantifies any
addition to the sample mass from gross contamination originating from
the use of reagents in the field.

N. Nitrogen Purge Requirements

    Method 202, as promulgated in 2010, includes two approaches for
performing the post-test nitrogen purge: (1) A negative pressure purge
using the pump and meter box from the sampling train or (2) a positive
pressure purge using the gas cylinder pressure to propel the nitrogen
gas through the CPM collection components.
    The intent of the multiple purge options was to allow the testing
contractors to either purge the sampling train on or near the sampling
location or to transport the train components to a controlled
environment less susceptible to sources of contamination. We now
believe that a post-test nitrogen purge of the sampling train using the
meter box and a vacuum pump adds steps that could potentially
contaminate samples and outweigh the advantages of train purges done
immediately following the sampling. In this action, we propose to
revise section 8.5.4 to eliminate the option for performing the post-
test nitrogen purge using the meter box and vacuum pump. We also
propose to make accompanying revisions in sections <IP_ADDRESS>, <IP_ADDRESS>,
<IP_ADDRESS> and <IP_ADDRESS>.

O. Data Record Requirements

    In this action, we propose the following amendments to Method 202
sections to record and report test information that were either absent
or undefined in the current promulgated method:
     Record the pre- and post-test weights of the impingers, as
well as the color of the indicating silica gel, at the completion of
sampling (sections 8.4.5 and 8.5.3).
     Record the results of the pre- and post-test leak checks
of the sampling train (sections 8.4.6 and 8.5.2).
     Record the time (hh:mm), nitrogen flowrate, CPM filter
temperature, and moisture trap temperature (if applicable) during the
post-test nitrogen purge (section <IP_ADDRESS>).
     Record the results of the field and laboratory analytical
balance calibration checks (sections 9.4 and 9.6.4).
     Record the temperature and relative humidity conditions of
the laboratory analytical balance (section 9.6.3).

P. Method Detection Limits

    In this action, we propose to revise section 13.0 regarding method
performance. We updated method detection limit values based on a formal
study submitted to the EPA by NCASI that evaluated the zero bias of
Method 202 when Method 202 Best Practices were implemented. A copy of
this study titled, ``Method 202 Zero Bias Study When Incorporating
Draft Best Practices Developed by the US EPA,'' (NCASI 2017) is
available in the docket (EPA-HQ-OAR-2016-0456-005).

Q. Alternative Blank Procedure and Correction Value

    While the EPA believes that field train proof blank results of 2.0
mg or less are achievable, we recognize there may be certain instances
when the environment surrounding the sampling location may
significantly contribute to the systematic bias of the method results
as measured by the field train proof blank. This proposed alternative
procedure would account for the uncontrollable environmental bias
associated with measurements collected in problematic sampling
locations.

    In this action, we are proposing to amend section 16.1 of Method
202 to allow the combined results from multiple field train proof
blanks to be used as the basis for blank correction up to 3.9 mg when
approved by the regulatory authority. The 3.9 mg value is based on the
Upper Prediction Limit (UPL) of the NCASI field study used to update
the method detection limit (NCASI 2017). In this procedure, we have
included conditions and criteria that a facility must satisfy in order
to demonstrate need for the alternative procedure.

IV. Request for Comments

    The EPA is requesting public comments on all of the proposed
editorial and technical amendments to Method 202. For the convenience
of the reader, we include in this notice the entire text of Method 202,
including proposed revisions, but the scope of this rulemaking is
limited to the proposed revisions and does not include any unchanged
provisions.

V. Statutory and Executive Order Reviews

    Additional information about these statutes and Executive Orders
can be found at http://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 not expected to be an Executive Order 13771
regulatory action because this action is not significant under
Executive Order 12866.

C. Paperwork Reduction Act (PRA)

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

D. Regulatory Flexibility Act (RFA)

    I certify that this 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 202 neither impose any requirements on regulated
entities beyond those specified in the current regulations, nor do they
change any emission standard.

E. Unfunded Mandates Reform Act (UMRA)

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

F. Executive Order 13132: Federalism

    This 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 action does not have tribal implications, as specified in
Executive Order 13175. This action proposes corrections and updates to
the existing procedures specified in Method 202. Thus, Executive Order
13175 does not apply to this action.

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 action is not subject to
Executive Order 13045 because it does not concern an environmental
health risk or safety risk.

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

    This 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 rulemaking does not involve technical standards.

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

    The EPA believes that this action is not subject to Executive Order
12898 (59 FR 7629, February 16, 1994) because it does not establish an
environmental health or safety standard. This action makes corrections
and updates to existing testing methodology and does not have any
impact on human health or the environment.

List of Subjects in 40 CFR Part 51

    Administrative practice and procedure, Air pollution control, EPA
Method 202, Incorporation by reference, Particulate matter, Reporting
and recordkeeping requirements, Sulfur dioxide.

     Dated: August 23, 2017.
E. Scott Pruitt,
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 51--REQUIREMENTS FOR PREPARATION, ADOPTION, AND SUBMITTAL OF
IMPLEMENTATION PLANS

0
1. The authority citation for part 51 continues to read as follows:

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

Subpart BB--Data Requirements for Characterizing Air Quality for
the Primary SO2 NAAQS

0
2. In appendix M to part 51-- Recommended Test Methods for State
Implementation Plans, revise Method 202 to read as follows:

Method 202--Dry Impinger Method for Determining Condensable Particulate
Emissions From Stationary Sources

1.0 Scope and Applicability

    1.1 Scope. The U.S. Environmental Protection Agency (U.S. EPA or
``we'') developed this method to describe the procedures that the stack
tester (``you'') must follow to measure condensable particulate matter
(CPM) emissions from stationary sources. This method includes
procedures for measuring both organic and inorganic CPM.
    1.2 Applicability. This method addresses the equipment,
preparation, and analysis necessary to measure only CPM. You can use
this method only for stationary source emission measurements. You can
use this method to measure CPM from stationary source

emissions after filterable particulate matter (PM) has been removed.
Condensable PM is measured in the emissions after removal from the
stack and after passing through a filter.
    (a) If you are required to measure total primary (direct)
PM2.5 and/or PM10, then you must combine the
procedures in this method with the procedures in Method 201A of
appendix M to this part. If you are required to measure both the
filterable and condensable components of total primary (direct) PM
emissions to the atmosphere, then you may use Method 5 of appendix A-3
to part 60, or Method 17 of appendix A-6 to part 60.

    Note:  If Method 17 of appendix A-6 to part 60 is attempted in
conjunction with Method 202 to measure total primary PM, and the
constant weight requirements for the filterable fractions cannot be
met, it may be necessary to conduct additional test runs using an
applicable filterable PM method that requires a heated filter
temperature.

    (b) If the gas filtration temperature of the filterable PM method
used does not exceed 30 [deg]C (85[emsp14][deg]F), then use of this
method is not necessary to measure primary PM, as the CPM is collected
as filterable PM.

    Note:  For those methods that require in-stack filtration (i.e.,
Method 17 and 201A), the measured stack temperature is considered
the filtration temperature.

    1.3 Responsibility. You are responsible for obtaining the equipment
and supplies you will need to use for this method. You should also
develop your own procedures for following this method and any
additional procedures to ensure accurate sampling and analytical
measurements.
    1.4 Additional Methods. To obtain reliable results, you should have
a thorough knowledge of the following test methods that are found in
appendices A-1 through A-3 and A-6 to part 60, and in appendix M to
this part:
    (a) Method 1--Sample and velocity traverses for stationary sources.
    (b) Method 2--Determination of stack gas velocity and volumetric
flow rate (Type S pitot tube).
    (c) Method 3--Gas analysis for the determination of dry molecular
weight.
    (d) Method 4--Determination of moisture content in stack gases.
    (e) Method 5--Determination of particulate matter emissions from
stationary sources.
    (f) Method 17--Determination of particulate matter emissions from
stationary sources (in-stack filtration method).
    (g) Method 201A--Determination of PM10 and
PM2.5 emissions from stationary sources (constant sampling
rate procedure).
    (h) In addition to Method 5, it is also acceptable to use Method
5A, 5D or 5I to collect filterable PM from stationary sources.

    Note: You must maintain the gas filtration temperature of the
filterable PM method as specified in the method, unless otherwise
specified by an applicable subpart.

    1.5 Limitations. You can use this method to measure emissions in
stacks that have entrained droplets only when this method is combined
with a filterable PM test method that operates at high enough
temperatures to cause water droplets sampled through the probe to
become vaporous.

    Note: The EPA recommends that under these conditions or any
other conditions, when moisture collection is expected to be in
excess of 2 percent, the testing periods be limited to no greater
than 2 hours.

    1.6 Conditions. You must maintain isokinetic sampling conditions to
meet the requirements of the filterable PM test method used in
conjunction with this method. You must sample at the required number of
sampling points specified in the filterable PM test method used in
conjunction with this method. Also, if you are using this method as an
alternative to a required performance test method, you must receive
approval from the regulatory authority that established the requirement
to use this test method prior to conducting the test.

2.0 Summary of Method

    2.1 Summary. The CPM is collected in dry impingers after filterable
PM has been collected on a filter maintained as specified in either
Method 5 of appendix A-3 to part 60, Method 17 of appendix A-6 to part
60, or Method 201A of appendix M to this part. The organic and aqueous
sample fractions from the impingers and an out-of-stack CPM filter are
then taken to dryness and weighed. The total mass collected from the
impinger fractions and the CPM filter represents the CPM. Compared to
the version of Method 202 that was promulgated on December 17, 1991,
this method eliminates the use of water as the collection media in
impingers and includes the addition of a condenser followed by a water
dropout impinger after the final in-stack or heated filter. This method
also includes the addition of one modified Greenburg-Smith impinger
(backup impinger) and a CPM filter following the water dropout
impinger. Figure 1 of section 18 presents the schematic of the sampling
train configured with these changes.
    2.1.1 Condensable PM. Condensable PM is collected in the water
dropout impinger, the modified Greenburg-Smith impinger, and the CPM
filter of the sampling train as described in this method. The impinger
contents are purged with nitrogen as soon as possible after the post-
test leak check to remove dissolved sulfur dioxide (SO2)
gases from the impingers. The impinger solutions are collected and the
glassware is rinsed with water, acetone, and hexane. The CPM filter is
extracted with water and hexane; the extracted liquid is then combined
with the hexane and water fractions from the impingers. The aqueous
impinger solution is then extracted with hexane. The organic and
aqueous fractions are evaporated to dryness and the residues are
weighed. The total of the aqueous and organic fractions represents the
CPM.
    2.1.2 Dry Impinger and Additional Filter. The potential artifacts
from SO2 are reduced using a vertical condenser and water
dropout impinger to separate CPM from reactive gases. No water is added
to the water dropout and backup impingers prior to the start of
sampling. To improve the collection efficiency of CPM, an additional
filter (the ``CPM filter'') is placed between the second and third
impingers.

3.0 Definitions

    3.1 Condensable PM (CPM) means material that is vapor phase at
stack conditions, but condenses and/or reacts upon cooling and dilution
in the ambient air to form solid or liquid PM immediately after
discharge from the stack. Note that all condensable PM is assumed to be
in the PM2.5 size fraction.
    3.2 Constant weight means a difference of no more than 0.5 mg or 1
percent of total weight less tare weight, whichever is greater, between
two consecutive weighings, with no less than 6 hours of desiccation
time between weighings.
    3.3 Field Train Proof Blank. A field train proof blank for each
source category tested is recovered on-site from a clean, fully-
assembled sampling train.
    3.4 Filterable PM means particles that are emitted directly by a
source as a solid or liquid at stack or release conditions and captured
on the filter of a stack test train.
    3.5 Primary PM (also known as direct PM) means particles that enter
the atmosphere as a direct emission from a stack or an open source.
Primary PM comprises two components: Filterable PM and condensable PM.
These two PM components have no upper particle size limit.
    3.6 Primary PM2.5 (also known as direct PM2.5, total
PM2.5, PM2.5, or

combined filterable PM2.5 and condensable PM) means PM with
an aerodynamic diameter less than or equal to 2.5 micrometers. These
solid particles are emitted directly from an air emissions source or
activity, or are the gaseous emissions or liquid droplets from an air
emissions source or activity that condense to form PM at ambient
temperatures. Direct PM2.5 emissions include elemental
carbon, directly emitted organic carbon, directly emitted sulfate,
directly emitted nitrate, and other inorganic particles (including but
not limited to crustal material, metals and sea salt).
    3.7 Primary PM10 (also known as direct PM10, total
PM10, PM10, or the combination of filterable
PM10 and condensable PM) means PM with an aerodynamic
diameter equal to or less than 10 micrometers.
    3.8 ASTM E617-13. ASTM E617-13 ``Standard Specification for
Laboratory Weights and Precisions Mass Standards,'' approved May 1,
2013, was developed and adopted by the American Society for Testing and
Materials (ASTM). The standards cover weights and mass standards used
in laboratories for specific classes. The ASTM E617-13 standard has
been approved for incorporation by reference by the Director of the
Office of the Federal Register in accordance with 5 U.S.C. 552(a) and 1
CFR part 51. The standard may be obtained from http://www.astm.org or
from the ASTM at 100 Barr Harbor Drive, P.O. Box C700, West
Conshohocken, PA 19428-2959. All approved material is available for
inspection at the EPA Docket Office, EPA WJC West Building, Room 3334,
1301 Constitution Avenue NW., Washington, DC 20460, telephone number
(202) 566-1744. It is also available for inspection at the National
Archives and Records Administration (NARA). For information on the
availability of this material at NARA, call<PHONE_NUMBER> or go to
http://www.archives.gov/federal_register/code_of_federal_regulattions/ibr_locations.html.

4.0 Interferences

    [Reserved]

5.0 Safety

    Disclaimer. Because the performance of this method may require the
use of hazardous materials, operations, and equipment, you should
develop a health and safety plan to ensure the safety of your employees
who are on site conducting the particulate emission test. Your plan
should conform with all applicable Occupational Safety and Health
Administration, Mine Safety and Health Administration, and Department
of Transportation regulatory requirements. Because of the unique
situations at some facilities and because some facilities may have more
stringent requirements than is required by state or federal laws, you
may have to develop procedures to conform to the plant health and
safety requirements.

6.0 Equipment and Supplies

    The equipment used in the filterable particulate portion of the
sampling train is described in Methods 5 and 17 of appendix A-1 through
A-3 and A-6 to part 60 and Method 201A of appendix M to this part. The
equipment used in the CPM portion of the train is described in this
section.
    6.1 Condensable Particulate Sampling Train Components. The sampling
train for this method is used in addition to filterable particulate
collection using Method 5 of appendix A-3 to part 60, Method 17 of
appendix A-6 to part 60, or Method 201A of appendix M to this part.
This method includes the following exceptions or additions:
    6.1.1 Probe Extension and Liner. The probe extension between the
filterable particulate filter and the condenser must be glass- or
fluoropolymer-lined. Follow the specifications for the probe liner
specified in section <IP_ADDRESS> of Method 5 of appendix A-3 to part 60.
    6.1.2 Condenser and Impingers. You must add the following
components to the filterable particulate sampling train: A vertical
condenser, followed by a water dropout impinger or flask, followed by a
modified Greenburg-Smith impinger (backup impinger) with an open tube
tip as described in section <IP_ADDRESS> of Method 5 of appendix A-3 to part
60.
    6.1.3 Dropout Impinger Insert for Nitrogen Purge. You must use a
leak-free ground glass fitting with a long glass or PTFE stem (e.g.,
modified Greenburg-Smith impinger insert or purge stem, etc.) for the
water dropout impinger to perform the nitrogen purge of the sampling
train. The glass stem must be designed so that the tip of the stem is
\1/2\'' from the bottom of the impinger.
    6.1.4 CPM Filter Holder. The modified Greenburg-Smith impinger is
followed by a filter holder that is either glass, stainless steel (316
or equivalent), or fluoropolymer-coated stainless steel. Commercial
size filter holders are available depending on project requirements.
Use a commercial filter holder capable of supporting 47 mm or greater
diameter filter. Commercial size filter holders contain a fluoropolymer
O-ring, stainless steel, ceramic or fluoropolymer filter support and a
final fluoropolymer O-ring. At the exit of the CPM filter, install a
fluoropolymer-coated or stainless steel encased thermocouple that is in
direct contact with the gas stream.

6.2 Sample Recovery Equipment

    6.2.1 Condensable PM Recovery. Use the following equipment to
quantitatively determine the amount of CPM recovered from the sampling
train.
    (a) Nitrogen purge line. You must use inert tubing and fittings
capable of delivering at least 14 liters/min of nitrogen gas to the
impinger train from a standard gas cylinder (see Figures 2 and 3 of
section 18). You may use standard 0.6 centimeters (\1/4\ inch) tubing
and compression fittings in conjunction with an adjustable pressure
regulator and needle valve.
    (b) Rotameter. You must use a rotameter capable of measuring gas
flow up to 20 liters/min. The rotameter must be accurate to five
percent of full scale.
    (c) Nitrogen gas purging system. Compressed ultra-pure nitrogen,
regulator, and filter must be capable of providing at least 14 liters/
min purge gas for one hour through the sampling train.
    (d) Sample bottles (500 ml). You must use amber glass bottles or
other non-reactive bottles (e.g., High Density Linear Polyethylene
(HDLPE), or PTFE) pre-cleaned sample bottles for inorganic samples.
Amber glass bottles are required for organic samples and must be
prepared according to section 8.4 of this method.
    6.2.2 Analysis Equipment. The following equipment is necessary for
CPM sample analysis:
    (a) Separatory Funnel. Glass, 1 liter.
    (b) Weighing Containers. Fluoropolymer beaker liners or other low-
mass vessels which are unreactive to the sample or atmosphere.

    Note: The use of an anti-static device(s) during gravimetric
analysis to prevent static from interfering with the analysis is
recommended when using Fluoropolymer or similar beaker liners.

    (c) Glass Beakers. 300 to 500 ml.
    (d) Drying Equipment. A desiccator containing anhydrous calcium
sulfate that is maintained below 10 percent relative humidity, and a
hot plate or oven equipped with temperature control.
    (e) Glass Pipets. 5 ml.
    (f) Burette. Glass, 0 to 100 ml in 0.1 ml graduations.
    (g) Analytical Balance. Analytical balance capable of weighing at
least 0.0001 g (0.1 mg).
    (h) pH Meter. The pH meter must be capable of determining the
acidity of liquid within 0.1 pH units.

    (i) Sonication Device. The device must have a minimum sonication
frequency of 20 kHz and be approximately four to six inches deep to
accommodate the sample extractor tube.
    (j) Leak-Proof Sample Containers. Containers used for sample and
blank recovery must not contribute more than 0.05 mg of residual mass
to the CPM measurements.
    (k) Wash bottles. Any container material is acceptable, but wash
bottles used for sample and blank recovery must not contribute more
than 0.1 mg of residual mass to the CPM measurements.

7.0 Reagents and Standards

    7.1 Sample Collection. To collect a sample, you will need a CPM
filter, crushed ice, and silica gel. You must also have water and
nitrogen gas to purge the sampling train. You will find additional
information on each of these items in the following summaries.
    7.1.1 CPM Filter. You must use a nonreactive, non-disintegrating
polymer filter that does not have an organic binder and does not
contribute more than 0.5 mg of residual mass to the CPM measurements.
The CPM filter must also have an efficiency of at least 99.95 percent
(less than 0.05 percent penetration) on 0.3 micrometer dioctyl
phthalate particles. You may use test data from the supplier's quality
control program to document the CPM filter efficiency.
    7.1.2 Silica Gel. Use an indicating-type silica gel of 6 to 16
mesh. You must obtain approval of the Administrator for other types of
desiccants (equivalent or better) before you use them. Allow the silica
gel to dry for 2 hours at 175 [deg]C (350 [deg]F) if it is being
reused. You do not have to dry new silica gel if the indicator shows
the silica gel is active for moisture collection.
    7.1.3 Water. Use deionized, ultra-filtered water that contains 1.0
parts per million by weight (ppmw) (1 mg/L) residual mass or less to
recover and extract samples.
    7.1.4 Crushed Ice. Obtain from the best readily available source.
    7.1.5 Nitrogen Gas. Use Ultra-High Purity compressed nitrogen or
equivalent to purge the sampling train. The compressed nitrogen you use
to purge the sampling train must contain no more than 1 parts per
million by volume (ppmv) oxygen, 1 ppmv total hydrocarbons as carbon,
and 2 ppmv moisture. The compressed nitrogen must not contribute more
than 0.1 mg of residual mass per purge.
    7.2 Sample Recovery and Analytical Reagents. You will need acetone,
hexane, anhydrous calcium sulfate, ammonia hydroxide, and deionized
water for the sample recovery and analysis. Unless otherwise indicated,
all reagents must conform to the specifications established by the
Committee on Analytical Reagents of the American Chemical Society. If
such specifications are not available, then use the best available
grade. Additional information on each of these items is in the
following paragraphs:
    7.2.1 Acetone. Use acetone that is stored in a glass bottle. Do not
use acetone from a metal container because it normally produces a high
residual mass in the laboratory and field reagent blanks. You must use
acetone that has a blank value less than 1.0 ppmw (0.1 mg/100 g)
residue.
    7.2.2 Hexane, American Chemical Society Grade or Equivalent. You
must use hexane that has a blank residual mass value less than 1.0 ppmw
(0.1 mg/100 g) residue.
    7.2.3 Water. Use deionized, ultra-filtered water that contains 1.0
ppmw (1.0 mg/L) residual mass or less to recover material caught in the
impinger.
    7.2.4 Condensable Particulate Sample Desiccant. Use indicating-type
anhydrous calcium sulfate to desiccate water and organic extract
residue samples prior to weighing.
    7.2.5 Ammonium Hydroxide. Use National Institute of Standards and
Technology (NIST)-traceable or equivalent (0.1 N) ammonium hydroxide
(NH4OH).
    7.2.6 Standard Buffer Solutions. Use one buffer solution with a
neutral pH and a second buffer solution with an acid pH of no less than
4.

8.0 Sample Collection, Preservation, Storage, and Transport

    8.1 Qualifications. This is a complex test method. To obtain
reliable results, you should be trained and experienced with in-stack
filtration systems (such as, cyclones, impactors, and thimbles) and
impinger and moisture train systems.
    8.2 Preparations. Clean all glassware used to collect and analyze
samples prior to field tests as described in Section 8.4 prior to use.
Cleaned glassware must be used at the start of each new source category
tested at a single facility. You must analyze laboratory reagent blanks
(water, acetone, and hexane) before field tests to verify low blank
concentrations for the reagent lot(s) used. Follow the pretest
preparation instructions in Section 8.1 of Method 5.
    8.3 Site Setup. You must follow the procedures required in Methods
5, 17, or 201A, whichever is applicable to your test requirements
including:
    (a) Determining the sampling site location and traverse points.
    (b) Calculating probe/cyclone blockage (as appropriate).
    (c) Verifying the absence of cyclonic flow.
    (d) Completing a preliminary velocity profile, and selecting a
nozzle(s) and sampling rate.
    8.3.1 Sampling Site Location. Follow the standard procedures in
Method 1 of appendix A-1 to part 60 to select the appropriate sampling
site. Choose a location that maximizes the distance from upstream and
downstream flow disturbances.
    8.3.2 Traverse Points. Use the required number of traverse points
at any location, as found in in the method used to collect the
filterable particulate. You must prevent the disturbance and capture of
any solids accumulated on the inner wall surfaces by maintaining a 1
inch distance from the stack wall (0.5 inch for sampling locations less
than 24 inches in diameter).
    8.4 Sampling Train Preparation. A schematic of the sampling train
used in this method is shown in Figure 1 of section 18. All glassware
that is used to collect and analyze samples should be cleaned
sufficiently to meet the maximum field train proof blank contribution
to be subtracted from the test results in section 9.9 (0.002g or 2.0
mg). Cleaning glassware prior to the test with soap and water, then
rinsing with tap water, followed by deionized water, acetone, and
finally, hexane is recommended. After cleaning, you should bake
glassware at 300 [deg]C for 6 hours prior to beginning tests at each
source category sampled at a facility. Prior to each sampling run, the
train glassware used to collect condensable PM must be rinsed
thoroughly with acetone, hexane, and then deionized, ultra-filtered
water that contains 1 ppmw (1 mg/L) residual mass or less.

    Note: Due the length of most probes, it is not practical to heat
them in an oven. After cleaning the probe liners, it is recommended
to heat the probe to the maximum temperature practical for the probe
sheath for a period of at least 3 hours. Then rinse thoroughly with
acetone, hexane, and deionized, ultra-filtered water.

    8.4.1 Condenser and Water Dropout Impinger. Add a vertical
condenser and a water dropout impinger without bubbler tube after the
final probe extension that connects the in-stack or out-of-stack hot
filter assembly with the CPM sampling train. This vertical condenser
must be constructed in a manner that prevents the pooling of the
condensate liquid within the condenser and be capable of cooling the
stack gas to less than or equal to 30 [deg]C (85 [deg]F).

At the start of the tests, the condenser and water dropout impingers
must be clean, without any water or reagent added.
    8.4.2 Backup Impinger. The water dropout impinger is followed by a
modified Greenburg-Smith impinger (backup impinger) with no taper (see
Figure 1 of section 18). Place the water dropout and backup impingers
in an insulated box with water at less than or equal to 30 [deg]C (less
than or equal to 85 [deg]F). At the start of the tests, the backup
impinger must be free of any residual solvents from the recovery or
glassware preparation.
    8.4.3 CPM Filter. Place a filter holder with a filter meeting the
requirements in section 7.1.1 after the backup impinger. The connection
between the CPM filter and the moisture trap impinger must include a
thermocouple fitting that provides a leak-free seal between the
thermocouple and the stack gas.
    8.4.4 Moisture Traps. You must use a modified Greenburg-Smith
impinger containing 100 ml of water, or the alternative described in
Method 5 of appendix A-3 to part 60, followed by an impinger containing
200 to 300 g of indicating-type silica gel to collect moisture that
passes through the CPM filter. You must maintain the gas temperature
below 20 [deg]C (68 [deg]F) at the exit of the moisture traps.
    8.4.5 Weighing of Impingers (Pretest). Weigh each impinger to 0.1
g, including the silica gel impinger prior to train assembly using the
field balance. Record the weights of each impinger on the CPM Impinger
Data Sheet (Figure 4).
    8.4.6 Leak-Check (Pretest). Use the procedures outlined in Method 5
of appendix A-3 to part 60, Method 17 of appendix A-6 to part 60, or
Method 201A of appendix M to this part as appropriate to leak check the
entire sampling system. Specifically, perform the following procedures:
    <IP_ADDRESS> Sampling train. You must pretest the entire sampling train
for leaks. The pretest leak-check must have a leak rate of not more
than 0.02 actual cubic feet per minute or 4 percent of the average
sample flow during the test run, whichever is less. Additionally, you
must conduct the leak-check at a vacuum equal to or greater than the
vacuum anticipated during the test run. Record the leak-check results
on the field test data sheet (see Figure 5). (Note: Conduct leak-checks
during port changes only as allowed by the filterable particulate
method used with this method.)
    <IP_ADDRESS> Pitot tube assembly. After you leak-check the sample train,
perform a leak-check of the pitot tube assembly. Follow the procedures
outlined in section 8.4.1 of Method 5.
    8.5 Sampling Train Operation. Operate the sampling train as
described in the filterable particulate sampling method (i.e., Method 5
of appendix A-3 to part 60, Method 17 of appendix A-6 to part 60, or
Method 201A of appendix M to this part) with the following additions or
exceptions:
8.5.1 Impinger and CPM Filter Assembly
    <IP_ADDRESS> During sampling, monitor the moisture condensation in the
water dropout impinger and backup impinger. If the accumulated water
from moisture condensation overwhelms (i.e., the water level is more
than approximately one-half the capacity of the water dropout impinger)
the water dropout impinger, or if water accumulates in the backup
impinger sufficient to cover the impinger insert tip, then you must
interrupt the sampling run, leak check the Method 202 portion of the
sampling train, replace the water dropout and/or backup impingers with
new pre-weighed impinger(s), reassemble, leak check the sampling train,
and then resume the sampling run. Weigh the impingers removed from the
sampling train and purge the water collected as soon as practical
following the procedures in section 8.5.3.
    <IP_ADDRESS> You must include the weight of the moisture in your
moisture calculation and you must combine the recovered water with the
appropriate sample fraction for subsequent CPM analysis.
    <IP_ADDRESS> Use the field data sheet to record the CPM filter
temperature readings at the beginning of each sample time increment and
when sampling is halted. Maintain the CPM filter greater than 20 [deg]C
(greater than 65 [deg]F) but less than or equal to 30 [deg]C (less than
or equal to 85 [deg]F) during sample collection.
    8.5.2 Leak-Check (Post-Test). Conduct the leak rate check according
to the filterable particulate sampling method used during sampling.
Conduct the leak-check at a vacuum equal to or greater than the maximum
vacuum achieved during the test run. Record the leak-check results on
the field test data sheet. If the leak rate of the sampling train
exceeds 0.02 actual cubic feet per minute or 4 percent of the average
sampling rate during the test run (whichever is less), then the run is
invalid and you must repeat it.
    8.5.3 Weighing of Impingers (Post-test). You must weigh each
impinger to 0.1 g after the completion of the testing and prior to the
post-test nitrogen purge and record these weights on the CPM Impinger
data sheet. Alternatively, you may choose to weigh each impinger after
completion of the post-test nitrogen purge. If this option is chosen,
you must do the following in addition to the procedures of section
8.5.4. Purge the sampling train from the water dropout impinger to the
exhaust of the moisture traps (see Figure 2). You must maintain the
temperature of the moisture traps following the CPM filter to prevent
removal of moisture during the purge. If necessary, add more ice during
the purge to maintain the gas temperature measured at the exit of the
silica gel impinger below 20 [deg]C (68 [deg]F).

    Note: You should also note the color of the indicating silica
gel to determine whether it has been completely spent, and record
its condition on the CPM Impinger Data Sheet.

    8.5.4 Post-Test Nitrogen Purge. As soon as possible after the post-
test leak-check, conduct the nitrogen purge. If no water was collected
before the CPM filter, then you may skip the remaining purge steps and
proceed with sample recovery (see section 8.5.5). If any water was
collected before the CPM filter, you must purge the CPM sampling train.
    <IP_ADDRESS> You may purge the entire CPM sample collection train from
the water dropout impinger through the CPM filter holder outlet or you
may quantitatively transfer the water collected in the water dropout
impinger to the backup impinger and purge only the backup impinger and
the CPM filter and holder (see Figure 3).
    <IP_ADDRESS> If you choose to conduct a purge of the entire CPM sampling
train, you must place the dropout impinger insert into the water
dropout impinger, and the impinger tip must extend at least 1
centimeter below the water level of the impinger catch.
    <IP_ADDRESS> If the tip of the impinger insert does not extend below the
water level (including the water transferred from the water dropout
impinger if this option was chosen), you must add a measured amount of
degassed, deionized ultra-filtered water that contains 1 ppmw (1 mg/L)
residual mass or less until the impinger tip is at least 1 centimeter
below the surface of the water. You must record the amount of water
added to the water dropout impinger (Vp) (see Figure 4 of section 18)
to correct the moisture content of the effluent gas. (Note: Prior to
use, water must be degassed using a nitrogen purge bubbled through the
water for at least 15 minutes to remove dissolved oxygen.)
    <IP_ADDRESS> To perform the nitrogen purge, you must start with no flow
of gas running through the clean purge line and fittings. Connect the
purge nitrogen in-line filter outlet to the input of the

impinger train to be purged. Increase the nitrogen flow gradually to
avoid over-pressurizing the impinger array. You must purge the CPM
train at a minimum of 14 liters per minute. Record the time (hh:mm),
nitrogen flowrate, and the temperature(s) of the CPM filter and
moisture trap (if applicable) at the start of the nitrogen purge on the
CPM Impinger Data Sheet.
    <IP_ADDRESS> During the purge procedure, maintain the gas temperature
measured at the exit of the CPM filter greater than 20 [deg]C (65
[deg]F), but less than or equal to 30 [deg]C (85 [deg]F). Continue the
purge under these conditions for at least 1 hour, recording the CPM
temperature and nitrogen rotameter value every 10 minutes. At the
conclusion of the purge, turn off the nitrogen delivery system. Record
the time (hh:mm) of the purge and the temperature of the CPM filter at
the start of the nitrogen purge on the CPM Impinger Data Sheet.
8.5.5 Sample Recovery
    <IP_ADDRESS> Filterable PM samples. Recovery of the filterable PM
samples involves the quantitative transfer of PM according to the
filterable particulate sampling method used (i.e., Method 5 of appendix
A-3 to part 60, Method 17 of appendix A-6 to part 60, or Method 201A of
appendix M to this part).
    <IP_ADDRESS> CPM Container #1, Aqueous liquid impinger contents.
Quantitatively transfer liquid from the dropout and the backup
impingers prior to the CPM filter into a clean, leak-proof container
labeled with test identification and ``CPM Container #1, Aqueous Liquid
Impinger Contents.'' Rinse all sampling train components including the
back half of the filterable PM filter holder, the probe extension (if
applicable), condenser, each impinger and the connecting glassware, and
the front half of the CPM filter housing twice with water. Recover the
rinse water, and add it to CPM Container #1. Mark the liquid level on
the container.
    <IP_ADDRESS> CPM Container #2, Organic rinses. Follow the water rinses
of the back half of the filterable PM filter holder, probe extension
(if applicable), condenser, each impinger, and all of the connecting
glassware and front half of the CPM filter with an acetone rinse.
Recover the acetone rinse into a clean, leak-proof amber glass
container labeled with test identification and ``CPM Container #2,
Organic Rinses.'' Then repeat the entire rinse procedure with two
rinses of hexane, and save the hexane rinses in the same container as
the acetone rinse (CPM Container #2). Mark the liquid level on the
container.
    <IP_ADDRESS> CPM Container #3, CPM filter sample. Use tweezers and/or
clean disposable surgical gloves to remove the filter from the CPM
filter holder. Place the filter in the Petri dish labeled with test
identification and ``CPM Container #3, Filter Sample.''
    <IP_ADDRESS> CPM Container #4, Acetone field reagent blank. Take a
minimum of 200 ml of the acetone directly from the wash bottle you used
for sample recovery and place it in a clean, leak-proof amber glass
container labeled with test identification and ``CPM Container #4,
Acetone Field Reagent Blank'' (see section 11.2.6 for analysis). Mark
the liquid level on the container. Collect one acetone field reagent
blank from each lot of acetone used for the test.
    <IP_ADDRESS> CPM Container #5, Water field reagent blank. Take a minimum
of 200 ml of the water directly from the wash bottle you used for
sample recovery and place it in a clean, leak-proof container labeled
with test identification and ``CPM Container #5, Water Field Reagent
Blank'' (see section 11.2.7 for analysis). Mark the liquid level on the
container. Collect one water field reagent blank from each lot of water
used for the test.
    <IP_ADDRESS> CPM Container #6, Hexane field reagent blank. Take a
minimum of 200 ml of the hexane directly from the wash bottle you used
for sample recovery and place it in a clean, leak-proof amber glass
container labeled with test identification and ``CPM Container #6,
Hexane Field Reagent Blank'' (see section 11.2.8 for analysis). Mark
the liquid level on the container. Collect one hexane field reagent
blank from each lot of hexane used for the test.
    <IP_ADDRESS> Field train proof blank. To demonstrate the cleanliness of
sampling train glassware, you must prepare a full sampling train to
serve as a field train proof blank just as it would be prepared for
sampling, including the filterable PM method front half, probe
extension (if applicable), condenser, impingers, CPM filter, and
transfer line. Transport and assemble the field train proof blank
sample train to the sampling location and perform a pre-test leak check
as if it were an actual sample train. Hold this train at the sampling
location for the same amount of time as a test run unless otherwise
specified by the Administrator, and perform a post-test leak check on
this train at the end of the actual test sampling time. After the post-
test leak check, you must conduct a nitrogen purge of the field train
proof blank sample as specified in section 8.5.4. For the nitrogen
purge, you must add 100 ml of deionized ultra-filtered water and
replicate the nitrogen purge procedures that you will use for the test
runs. After conducting the nitrogen purge, recover the field train
proof blank as described in sections <IP_ADDRESS>.1 through <IP_ADDRESS>.3.
    <IP_ADDRESS>.1 CPM Container #7, Field train proof blank, inorganic
rinses. Rinse the probe extension, condenser, each impinger and the
connecting glassware, and the front half of the CPM filter housing
twice with water. Recover the rinse water and place it in a clean,
leak-proof container labeled with test identification and ``CPM
Container #7, Field Train Proof Blank, Inorganic Rinses.'' Mark the
liquid level on the container.
    <IP_ADDRESS>.2 CPM Container #8, Field train proof blank, organic
rinses. Follow the water rinse of the probe extension, condenser, each
impinger and the connecting glassware, and the front half of the CPM
filter housing with an acetone rinse. Recover the acetone rinse into a
clean, leak-proof container labeled with test identification and ``CPM
Container #8, Field Train Proof Blank, Organic Rinses.'' Then repeat
the entire rinse procedure with two rinses of hexane and recover the
hexane rinses into the same container as the acetone rinse (CPM
Container #10). Mark the liquid level on the container.
    <IP_ADDRESS>.3 CPM Container #9, Field train proof blank, filter sample.
Use tweezers and/or clean disposable surgical gloves to remove the
filter from the CPM filter holder. Place the filter in the Petri dish
labeled with test identification and ``CPM Container #9, Field Train
Proof Blank, Filter Sample.''
    8.5.6 Sample Transport procedures. Containers must remain in an
upright position at all times during shipping. You do not have to ship
the containers under dry or blue ice. However, samples should be
maintained at or below 30 [deg]C (85 [deg]F) during shipping.

9.0 Quality Control

    9.1 Daily Quality Checks. You must perform daily quality checks of
field log notebooks and data entries and calculations using data
quality indicators from this method and your site-specific test plan.
You must review and evaluate recorded and transferred raw data,
calculations, and documentation of testing procedures. You must initial
or sign log notebook pages and data entry forms that were reviewed.
    9.2 Calculation Verification. Verify the calculations by
independent, manual checks. You must flag any suspect data and identify
the nature of the problem and potential effect on data quality. After
you complete the test, prepare a data summary and compile all the
calculations and raw data sheets.
    9.3 Conditions. You must document data and information on the
process

unit tested, the particulate control system used to control emissions,
any non-particulate control system that may affect particulate
emissions, the sampling train conditions, and weather conditions.
Discontinue the test if the operating conditions may cause non-
representative particulate emissions.
    9.4 Field Balance Calibration Check. Record the results of the
calibration check procedures on field balances each day that they are
used as required in section 10.3.
    9.5 Glassware. Use class A volumetric glassware for titrations, or
calibrate your equipment against NIST-traceable glassware.

9.6 Laboratory Analytical Balance

    9.6.1 Maintain the location of the analytical balance (i.e.,
weighing room) at 20 [deg]C  3 [deg]C (68[emsp14][deg]F
 5[emsp14][deg]F).
    9.6.2 Maintain the location the analytical balance (i.e., weighing
room) at 35 to 50 percent relative humidity. Alternatively, it is
acceptable for the percent relative humidity to be less than 35
percent. In either case, you should maintain the relative humidity
within 10 percent relative humidity for sampling weighings.
    9.6.3  Record and report the temperature and relative humidity of
the analytical balance location for each measurement performed.
    9.6.4 Calibration Check. Record the calibration check of your
laboratory analytical balance at least once each day that you weigh CPM
samples. Audit the balance using at least one ASTM E617-13 Class 2
tolerance (or better) calibration weight, within 1 g to 5 g of the
weight of the sample plus container you will be weighing.
    9.7 Laboratory Reagent Blanks. You should analyze blanks of water,
acetone, and hexane used for field recovery and sample analysis.
Analyze and report at least one sample (500 ml minimum) of each lot of
reagents that you plan to use for sample recovery and analysis. These
blanks are not required by the test method, but analyzing reagent
blanks before field use is recommended to verify low reagent blank
concentrations.
    9.8 Field Reagent Blanks. You must analyze and report the results
of each lot of reagent used for the field test.
    9.9 Field Train Proof Blank. You must recover a minimum of one
field train proof blank for each new source category at a single
facility using glassware prepped according to section 8.4. You must
assemble the sampling train as it will be used for testing, including
the filterable PM method front half, CPM filter, and transfer line. You
must prepare and recover the field train proof blank as described in
section <IP_ADDRESS>. From each field sample weight, you will subtract the
condensable particulate mass you determine with this field train proof
blank or 0.002 g (2.0 mg), whichever is less, unless otherwise
specified by the regulatory authority.

10.0 Calibration and Standardization

    Maintain a field log notebook of all condensable particulate
sampling and analysis calibrations. Include copies of the relevant
portions of the calibration and field logs in the final test report.
    10.1 Thermocouple Calibration. You must calibrate the thermocouples
using the procedures described in section 10.3.1 of Method 2 of
appendix A-1 to part 60 or Alternative Method 2, Thermocouple
Calibration (ALT-011) (https://www.epa.gov/emc). Calibrate each
temperature sensor at a minimum of three points over the anticipated
range of use against a NIST-traceable thermometer. Alternatively, a
reference thermocouple and potentiometer calibrated against NIST
standards can be used.
    10.2 Ammonium Hydroxide. The 0.1 N NH4OH used for
titrations in this method is made as follows: Add 7 ml of concentrated
(14.8 M) NH4OH to 1 liter of water. Standardize against
certified standard of 0.1 N H2SO4, and calculate
the exact normality using a procedure parallel to that described in
section 10.5 of Method 6 of appendix A-4 to 40 CFR part 60.
Alternatively, purchase 0.1 N NH4OH that has been
standardized against a NIST reference material. Record the normality on
the CPM Work Table (see Figure 6 of section 18).
    10.3 Field Balance Calibration Check. Check the calibration of the
balance used to weigh impingers with a weight that is at least 500 g or
within 50 g of a loaded impinger. The weight must be ASTM E617-13
``Standard Specification for Laboratory Weights and Precision Mass
Standards'' Class 6 (or better). Daily, before use, the field balance
must measure the weight within  0.5 g of the certified mass
and record the results. If the balance calibration check fails, perform
corrective measures and repeat the check before using balance.
    10.4 Analytical Balance Calibration. Perform a multipoint
calibration (at least five points spanning the operational range) of
the analytical balance before the first use, and semiannually
thereafter. The calibration of the analytical balance must be conducted
using ASTM E617-13 ``Standard Specification for Laboratory Weights and
Precision Mass Standards'' Class 2 (or better) tolerance weights. Audit
the balance each day it is used for gravimetric measurements by
weighing at least one ASTM E617-13 Class 2 tolerance (or better)
calibration weight that corresponds to 50 to 150 percent of the weight
of one filter or between 1 g and 5 g and record the results. If the
scale cannot reproduce the value of the calibration weight to within
0.5 mg of the certified mass, perform corrective measures and conduct
the multipoint calibration before use.

11.0 Analytical Procedures

11.1 Analytical Data Sheets

    (a) Record the filterable particulate field data on the appropriate
(i.e., Method 5, 17, or 201A) analytical data sheets. Record the
condensable particulate data on the CPM Work Table (see Figure 7 of
section 18).
    (b) Visually inspect the liquid level mark on each sample container
and record on the CPM Work Table whether leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the
Administrator, to correct the final results.
    11.2 Condensable PM Analysis. See the flow chart in Figure 8 of
section 18 for the steps to process and combine fractions from the CPM
train.
    11.2.1 Container #3, CPM Filter Sample. Extract the CPM filter as
described in this section.
    <IP_ADDRESS> Extract the water soluble (aqueous or inorganic) CPM from
the CPM filter by placing it into a clean extraction container or
flask. Add sufficient deionized, ultra-filtered water to cover the
filter (e.g., 10 ml of water). Place the extractor container into a
sonication bath and extract the water-soluble material for a minimum of
2 minutes. Combine the aqueous extract with the contents of Container
#1. Repeat this extraction step twice for a total of three extractions.
    <IP_ADDRESS> Extract the organic soluble CPM from the CPM filter by
adding sufficient hexane to cover the filter (e.g., 10 ml of hexane).
Place the extractor tube into a sonication bath and extract the organic
soluble material for a minimum of two minutes. Combine the organic
extract with the contents of Container #2. Repeat this extraction step
twice for a total of three extractions.
    11.2.2 CPM Container #1, Aqueous Liquid Impinger Contents. Analyze
the water-soluble CPM in Container #1 as described in this section.
Place the contents of Container #1 into a separatory funnel. Add
approximately 30 ml of hexane to the funnel, mix well, and pour off the
upper organic phase. Repeat this procedure twice with 30 ml

of hexane each time combining the organic phase from each extraction.
Each time, leave a small amount of the organic/hexane phase in the
separatory funnel, ensuring that no water is collected in the organic
phase. This extraction should yield about 90 ml of organic extract.
Combine the organic extract from Container #1 with the organic train
rinse in Container #2.
    <IP_ADDRESS> Determine the inorganic fraction weight. Transfer the
aqueous fraction from the extraction to a clean 500 ml or smaller
beaker. Evaporate to no less than 10 ml liquid on a hot plate or in the
oven at 105 [deg]C and allow to dry at room temperature (not to exceed
30 [deg]C (85[emsp14][deg]F)). Following evaporation, desiccate the
residue for 24 hours in a desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least 6 hours to a constant weight.
(See section 3.0 for a definition of constant weight.) Report results
to the nearest 0.1 mg on the CPM Work Table (see Figure 6 of section
18) and proceed directly to section 11.2.3. If the residue cannot be
weighed to constant weight, re-dissolve the residue in 100 ml of
deionized distilled ultra-filtered water that contains 1 ppmw (1 mg/L)
residual mass or less and continue to section <IP_ADDRESS>.
    <IP_ADDRESS> You must ensure that water and volatile acids have
completely evaporated before neutralizing nonvolatile acids in the
sample. Only after failure to reach constant weight and rehydration,
per section <IP_ADDRESS>, use titration to neutralize acid in the sample
and remove water of hydration. Calibrate the pH meter with the neutral
and acid buffer solutions immediately prior to the titration of the
samples. Then titrate the sample with 0.1 N NH4OH to a pH of
7.0, as indicated by the pH meter. Record the volume of titrant used on
the CPM Work Table (see Figure 6 of section 18).
    <IP_ADDRESS> Using a hot plate or an oven at 105 [deg]C, evaporate the
aqueous phase to approximately 10 ml. Quantitatively transfer the
beaker contents to a clean, 50 ml pre-tared weighing container and
evaporate to dryness at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least 6
hours to a constant weight. (See section 3.0 for a definition of
constant weight.) Report results to the nearest 0.1 mg on the CPM Work
Table (see Figure 6 of section 18).
    <IP_ADDRESS> Calculate the correction factor to subtract the
NH4\+\ retained in the sample using Equation 1 in section
12.
    11.2.3 CPM Container #2, Organic Fraction Weight Determination.
Analyze the organic soluble CPM in Container #2 as described in this
section. Place the organic phase in a clean glass beaker. Evaporate the
organic extract at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood to not less than
10 ml. Quantitatively transfer the beaker contents to a clean 50 ml
pre-tared weighing container and evaporate to dryness at room
temperature (not to exceed 30 [deg]C (85[emsp14][deg]F)) and pressure
in a laboratory hood. Following evaporation, desiccate the organic
fraction for 24 hours in a desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least 6 hours to a constant weight
(i.e., less than or equal to 0.5 mg change from previous weighing), and
report results to the nearest 0.1 mg on the CPM Work Table (see Figure
6 of section 18).
    11.2.4 Container #4, Acetone Field Reagent Blank. Use 200 ml of
acetone from the blank container used for this analysis. Transfer 200
ml of the acetone field reagent blank to a clean 250 ml beaker.
Evaporate the acetone at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood to approximately
10 ml. Quantitatively transfer the beaker contents to a clean pre-tared
weighing container, and evaporate to dryness at room temperature (not
to exceed 30 [deg]C (85[emsp14][deg]F)) and pressure in a laboratory
hood. Following evaporation, desiccate the residue for 24 hours in a
desiccator containing anhydrous calcium sulfate. Weigh at intervals of
at least 6 hours to a constant weight (i.e., less than or equal to 0.5
mg change from previous weighing), and report results to the nearest
0.1 mg on Figure 5 of section 19.
    11.2.5 Container #5, Water Field Reagent Blank. Use 200 ml of the
water from the blank container for this analysis. Transfer the water to
a clean 250 ml beaker, and evaporate to approximately 10 ml liquid in
the oven at 105 [deg]C. Quantitatively transfer the beaker contents to
a clean 50 ml pre-tared weighing container and evaporate to dryness at
room temperature (not to exceed 30 [deg]C (85[emsp14][deg]F)) and
pressure in a laboratory hood. Following evaporation, desiccate the
residue for 24 hours in a desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least 6 hours to a constant weight
(i.e., less than or equal to 0.5 mg change from previous weighing) and
report results to the nearest 0.1 mg on Figure 5 of section 18.
    11.2.6 Container #6, Hexane Field Reagent Blank. Use 200 ml of
hexane from the blank container for this analysis. Transfer 150 ml of
the hexane to a clean 250 ml beaker. Evaporate the hexane at room
temperature (not to exceed 30 [deg]C (85[emsp14][deg]F)) and pressure
in a laboratory hood to approximately 10 ml. Quantitatively transfer
the beaker contents to a clean 50 ml pre-tared weighing container and
evaporate to dryness at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least 6
hours to a constant weight (i.e., less than or equal to 0.5 mg change
from previous weighing), and report results to the nearest 0.1 mg on
Figure 5 of section 18.

12.0 Calculations and Data Analysis

    12.1 Nomenclature. Report results in International System of Units
(SI units) unless the regulatory authority for testing specifies
English units. The following nomenclature is used.

[Delta]H@ = Pressure drop across orifice at flow rate of
0.75 SCFM at standard conditions, inches of water column (Note
Specific to each orifice and meter box).
17.03 = mg/milliequivalents for ammonium ion.
ACFM = Actual cubic feet per minute.
Ccpm = Concentration of the condensable PM in the stack
gas, dry basis, corrected to standard conditions, milligrams/dry
standard cubic foot.
mc = Mass of the NH4\+\ added to sample to
form ammonium sulfate, mg.
mcpm = Mass of the total condensable PM, mg.
mfb = Mass of total CPM in field train proof blank, mg.
mg = Milligrams.
mg/dscf = Milligrams per dry standard cubic foot.
mg/L = Milligrams per liter.
mi = Mass of inorganic CPM, mg.
mib = Mass of inorganic CPM in field train proof blank,
mg.
mo = Mass of organic CPM, mg.
mob = Mass of organic CPM in field train blank, mg.
mr = Mass of dried sample from inorganic fraction, mg.
N = Normality of ammonium hydroxide titrant.
ppmv = Parts per million by volume.
ppmw = Parts per million by weight.
Vm(std) = Volume of gas sample measured by the dry gas
meter, corrected to standard conditions, dry standard cubic meter
(dscm) or dry standard cubic foot (dscf) as defined in Equation 5-1
of Method 5.
Vt = Volume of NH4OH titrant, ml.
Vp = Volume of water added during train purge.

    12.2 Calculations. Use the following equations to complete the
calculations required in this test method. Enter the appropriate
results from these calculations on the CPM Work Table (see Figure 7 of
section 18).

    12.2.1 Mass of ammonia correction. Correction for ammonia added
during titration of 100 ml aqueous CPM sample. This calculation assumes
no waters of hydration.
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    (Eq. 1)12.2.2 Mass of the Field Train Proof Blank (mg). Per section
9.9, the mass of the field train proof blank, mfb, shall not
exceed 2.0 mg.
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    (Eq. 2)12.2.3 Mass of Inorganic CPM (mg).
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    (Eq. 3)12.2.4 Total Mass of CPM (mg).
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    (Eq. 4)12.2.5 Concentration of CPM (mg/dscf).
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    12.3 Emissions Test Report. You must prepare a test report
following the guidance in EPA Guideline Document 043.

13.0 Method Performance

    A field evaluation (NCASI 2017) of Method 202 incorporating Best
Practices showed that the detection limit was 1.6 for total CPM;
consisting of approximately 1.0 mg for organic CPM and approximately
0.6 mg for inorganic CPM. This field evaluation also demonstrated that
the expected blank value of the field train proof blank was less than
1.8 mg.

14.0 Pollution Prevention

    [Reserved]

15.0 Waste Management

    Solvent and water are evaporated in a laboratory hood during
analysis. No liquid waste is generated in the performance of this
method. Organic solvents used to clean sampling equipment should be
managed as Resource Conservation and Recovery Act organic waste.

16.0 Alternative Procedures

    16.1 Alternative Field Train Proof Blank Procedure. The following
procedure may be utilized with approval by the regulatory authority at
stationary sources with environments with significant ambient PM
concentrations that could positively bias the results of the Method 202
samples collected. This procedure would permit you to subtract up to
0.0039 g (3.9 mg) from the measured condensable particulate mass.
    16.1.1 The facility must request this alternative prior to the test
program, and the request must be approved by the regulatory authority
prior to the testing. The request may include the following elements:
    (1) Documented adherence to the Best Practices for Method 202 by
the tester. This documentation may include:
    (a) Tester's Method 202 standard operating procedure (SOP);
    (b) Residual mass of the laboratory reagent blanks (Reagent ID,
Manufacturer, Lot Number);
    (c) Tester-specific Method Detection Limit;
    (d) Training records.
    (2) Justification by the facility that the environment around the
sampling location is likely to bias the CPM results. This justification
may include:
    (a) Schematic of the facility identifying locations that may
contribute to environmental bias;
    (b) Ambient PM concentration (mg/m\3\);
    (c) Previous test results (i.e., field train proof blank results).
    16.1.2 Upon the regularity authority approval, you will recover a
minimum of two field train proof blanks for each source category tested
at the subject facility using glassware prepped according to section
8.4 of this method. You must perform the field train proof blank
evaluations as described in section 9.9 of this method.
    16.1.3 From each field sample weight, you will subtract the average
condensable particulate mass you determine with all of the duplicate
field train proof blank trains or 0.0039 g (3.9 mg), whichever is less
unless the difference between highest and lowest values of the field
train proof blanks is >1.0 mg. If the agreement is >1.0 mg, then you
must subtract the lowest

condensable particulate mass values you determine with the field train
proof blank trains or 0.002 g (2.0 mg), whichever is less, unless
otherwise specified by the regulatory authority.
    16.2 Alternative Method 2. Thermocouple Calibration (ALT-011) for
the thermocouple calibration can be found at http://www3.epa.gov/ttn/emc/approalt/alt-011.pdf.

17.0 References

(1) Commonwealth of Pennsylvania, Department of Environmental
Resources. 1960. Chapter 139, Sampling and Testing (Title 25, Rules
and Regulations, part I, Department of Environmental Resources,
Subpart C, Protection of Natural Resources, Article III, Air
Resources). January 8, 1960.
(2) DeWees, W.D. and K.C. Steinsberger. 1989. ``Method Development
and Evaluation of Draft Protocol for Measurement of Condensable
Particulate Emissions.'' Draft Report. November 17, 1989.
(3) DeWees, W.D., K.C. Steinsberger, G.M. Plummer, L.T. Lay, G.D.
McAlister, and R.T. Shigehara. 1989. ``Laboratory and Field
Evaluation of EPA Method 5 Impinger Catch for Measuring Condensable
Matter from Stationary Sources.'' Paper presented at the 1989 EPA/
AWMA International Symposium on Measurement of Toxic and Related Air
Pollutants. Raleigh, North Carolina. May 1-5, 1989.
(4) Electric Power Research Institute (EPRI). 2008. ``Laboratory
Comparison of Methods to Sample and Analyze Condensable PM.'' EPRI
Agreement EP-P24373/C11811 Condensable Particulate Methods: EPRI
Collaboration with EPA, October 2008.
(5) Nothstein, Greg. Masters Thesis. University of Washington.
Department of Environmental Health. Seattle, Washington.
(6) Richards, J., T. Holder, and D. Goshaw. 2005. ``Optimized Method
202 Sampling Train to Minimize the Biases Associated with Method 202
Measurement of Condensable PM Emissions.'' Paper presented at Air &
Waste Management Association Hazardous Waste Combustion Specialty
Conference. St. Louis, Missouri. November 2-3, 2005.
(7) Texas Air Control Board, Laboratory Division. 1976.
``Determination of Particulate in Stack Gases Containing Sulfuric
Acid and/or Sulfur Dioxide.'' Laboratory Methods for Determination
of Air Pollutants. Modified December 3, 1976.
(8) Puget Sound Air Pollution Control Agency, Engineering Division.
1983. ``Particulate Source Test Procedures Adopted by Puget Sound
Air Pollution Control Agency Board of Directors.'' Seattle,
Washington. August 11, 1983.
(9) U.S. Environmental Protection Agency, Federal Reference Methods
1 through 5 and Method 17, 40 CFR 60, appendix A-1 through A-3 and
A-6.
(10) U.S. Environmental Protection Agency. 2008. ``Evaluation and
Improvement of Condensable PM Measurement,'' EPA Contract No. EP-D-
07-097, Work Assignment 2-03, October 2008.
(11) U.S. Environmental Protection Agency. 2005. ``Laboratory
Evaluation of Method 202 to Determine Fate of SO2 in
Impinger Water,'' EPA Contract No. 68-D-02-061, Work Assignment 3-
14, September 30, 2005.
(12) U.S. Environmental Protection Agency. 2010. ``Field Valuation
of an Improved Method for Sampling and Analysis of Filterable and
Condensable Particulate Matter.'' Office of Air Quality Planning and
Standards, Sector Policy and Program Division Monitoring Policy
Group. Research Triangle Park, NC 27711.
(13) Wisconsin Department of Natural Resources. 1988. Air Management
Operations Handbook, Revision 3. January 11, 1988.
(14) U.S. Environmental Protection Agency. 2016. ``EPA Method 202
Best Practices Handbook.'' Office of Air Quality Planning and
Standards, Air Quality Assessment Division, Measurements Technology
Group. Research Triangle Park, NC 27711.
(15) National Council for Air and Stream Improvement. Research Brief
submitted to the US EPA. May 25, 2017. ``Method 202 Zero Bias Study
When Incorporating Draft Best Practices Developed by the US EPA.''
NCASI Southern Research Center. Newberry, Florida 32669.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

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[FR Doc. 2017-18425 Filed 9-7-17; 8:45 am]
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