[Federal Register Volume 82, Number 173 (Friday, September 8, 2017)]
[Proposed Rules]
[Pages 42508-42530]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[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 Once submitted, comments cannot be edited or withdrawn.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 (919) 541-7903 or by email at 
[email protected] 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 (202) 566-1744, and the telephone 
number for the Air Docket is (202) 566-1742.

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: (919) 541-0516; email address: [email protected].

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?

[[Page 42509]]

    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:

--------------------------------------------------------------------------------------------------------------------------------------------------------
                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,

[[Page 42510]]

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

[[Page 42511]]

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 8.5.4.10 (and renumber as section 8.5.5.8) 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 8.5.5.8, 8.5.5.8.1, 
8.5.5.8.2, 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 8.5.5.8.3 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 8.5.3.4 (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

[[Page 42512]]

revisions in sections 8.5.1.1, 8.5.1.2, 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 8.5.1.1 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 8.5.1.1 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), 8.5.5.3, 8.5.5.5, and 8.5.5.7 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), 
11.2.2.3, 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

[[Page 42513]]

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 11.2.2.2 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 11.2.2.2 
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 8.5.5.5, 8.5.5.6, 8.5.5.7, 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 8.5.4.1, 8.5.4.2, 
8.5.4.4 and 8.5.4.5.

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 8.5.4.4).
     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.

[[Page 42514]]

    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

[[Page 42515]]

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

[[Page 42516]]

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 202-741-6030 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 6.1.1.2 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 6.1.1.8 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.

[[Page 42517]]

    (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).

[[Page 42518]]

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:
    8.4.6.1 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.)
    8.4.6.2 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
    8.5.1.1 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.
    8.5.1.2 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.
    8.5.1.3 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.
    8.5.4.1 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).
    8.5.4.2 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.
    8.5.4.3 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.)
    8.5.4.4 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

[[Page 42519]]

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.
    8.5.4.5 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
    8.5.5.1 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).
    8.5.5.2 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.
    8.5.5.3 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.
    8.5.5.4 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.''
    8.5.5.5 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.
    8.5.5.6 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.
    8.5.5.7 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.
    8.5.5.8 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 8.5.5.8.1 through 8.5.5.8.3.
    8.5.5.8.1 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.
    8.5.5.8.2 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.
    8.5.5.8.3 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

[[Page 42520]]

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 8.5.5.8. 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.
    11.2.1.1 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.
    11.2.1.2 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

[[Page 42521]]

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.
    11.2.2.1 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 11.2.2.2.
    11.2.2.2 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 11.2.2.1, 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).
    11.2.2.3 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).
    11.2.2.4 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).

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    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

[[Page 42523]]

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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