82_FR_42681 82 FR 42508 - Method 202-Dry Impinger Method for Determining Condensable Particulate Emissions From Stationary Sources

82 FR 42508 - Method 202-Dry Impinger Method for Determining Condensable Particulate Emissions From Stationary Sources

ENVIRONMENTAL PROTECTION AGENCY

Federal Register Volume 82, Issue 173 (September 8, 2017)

Page Range42508-42530
FR Document2017-18425

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.

Federal Register, Volume 82 Issue 173 (Friday, September 8, 2017)
[Federal Register Volume 82, Number 173 (Friday, September 8, 2017)]
[Proposed Rules]
[Pages 42508-42530]
From the Federal Register Online  [www.thefederalregister.org]
[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 Once submitted, comments cannot be edited or withdrawn.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).

[[Page 42522]]

    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.
[GRAPHIC] [TIFF OMITTED] TP08SE17.000

    (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.
[GRAPHIC] [TIFF OMITTED] TP08SE17.001

    (Eq. 2)12.2.3 Mass of Inorganic CPM (mg).
    [GRAPHIC] [TIFF OMITTED] TP08SE17.002
    
    (Eq. 3)12.2.4 Total Mass of CPM (mg).
    [GRAPHIC] [TIFF OMITTED] TP08SE17.003
    
    (Eq. 4)12.2.5 Concentration of CPM (mg/dscf).
    [GRAPHIC] [TIFF OMITTED] TP08SE17.004
    
    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

BILLING CODE 6560-50-P

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[[Page 42525]]


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[[Page 42526]]


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[[Page 42527]]


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[[Page 42528]]


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[[Page 42529]]


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[[Page 42530]]


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[FR Doc. 2017-18425 Filed 9-7-17; 8:45 am]
BILLING CODE 6560-50-C



                                                  42508                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                                                                                 TABLE 1—FORMAT FOR SUBMITTING COMMENTS
                                                                                       Name of regulation

                                                  Type of product or FDA Center regulating the product.
                                                  Citation to Code of Federal Regulations and statutory citation (as appli-
                                                    cable).
                                                  Approved information collection and OMB Control Number (as applica-
                                                    ble).
                                                  Brief description of concern ......................................................................       (For example, what innovation makes the regulation outdated? Why?)
                                                  Available data on cost or economic impact .............................................                   (Quantified costs and/or cost savings. Qualitative description, if need-
                                                                                                                                                               ed.)
                                                  Proposed solution .....................................................................................   (Include your solution. For example, how would you modify the regula-
                                                                                                                                                               tion? Provide specific text if you are recommending a modification.)



                                                  III. References                                                       Condensable Particulate Emissions from                       hearing on our Web site at: https://
                                                     The following references are on                                    Stationary Sources to improve the                            www.epa.gov/emc/emc-proposed-test-
                                                  display in the Dockets Management                                     consistency in results achieved across                       methods. The EPA does not intend to
                                                  Staff office (see ADDRESSES) and are                                  the testing community.                                       publish another document in the
                                                  available for viewing by interested                                   DATES:                                                       Federal Register announcing any
                                                  persons between 9 a.m. and 4 p.m.,                                      Comments. Comments must be                                 updates on the request for a public
                                                  Monday through Friday; they are also                                  received on or before November 7, 2017.                      hearing. Please contact Mr. Ned
                                                  available electronically at https://                                    Public Hearing. If a public hearing is                     Shappley at (919) 541–7903 or by email
                                                  www.regulations.gov. FDA has verified                                 requested by September 18, 2017, then                        at shappley.ned@epa.gov to request a
                                                  the Web site addresses, as of the date                                we will hold a public hearing on                             public hearing, to register to speak at the
                                                  this document publishes in the Federal                                October 10, 2017 at the location                             public hearing, or to inquire as to
                                                  Register, but Web sites are subject to                                described in the ADDRESSES section. The                      whether a public hearing will be held.
                                                  change over time.                                                     last day to pre-register in advance to                          Docket: All documents in the docket
                                                                                                                        speak at the public hearing will be                          are listed in the http://
                                                  1. Executive Order 13771 (January 30, 2017);                          October 6, 2017.
                                                       available at https://
                                                                                                                                                                                     www.regulations.gov index. Although
                                                       www.federalregister.gov/documents/                               ADDRESSES: Submit your comments,                             listed in the index, some information is
                                                       2017/02/03/2017-02451/reducing-                                  identified by Docket ID No. EPA–HQ–                          not publicly available, e.g., CBI or other
                                                       regulation-and-controlling-regulatory-                           OAR–2016–0456, to the Federal                                information whose disclosure is
                                                       costs.                                                           eRulemaking Portal at http://                                restricted by statute. Certain other
                                                  2. Executive Order 13777 (February 24,                                www.regulations.gov. Follow the online                       material, such as copyrighted material,
                                                       2017); available at https://                                     instructions for submitting comments.                        will be publicly available only in hard
                                                       www.federalregister.gov/documents/                               Once submitted, comments cannot be                           copy. Publicly available docket
                                                       2017/03/01/2017-04107/enforcing-the-                             edited or withdrawn. The EPA may                             materials are available either
                                                       regulatory-reform-agenda.
                                                                                                                        publish any comment received to its                          electronically in http://
                                                    Dated: August 30, 2017.                                             public docket. Do not submit                                 www.regulations.gov or in hard copy at
                                                  Anna K. Abram,                                                        electronically any information you                           the EPA Docket Center, EPA/DC, EPA
                                                  Deputy Commissioner for Policy, Planning,                             consider to be Confidential Business                         WJC West Building, Room 3334, 1301
                                                  Legislation, and Analysis.                                            Information (CBI) or other information                       Constitution Avenue NW., Washington,
                                                  [FR Doc. 2017–19047 Filed 9–7–17; 8:45 am]                            whose disclosure is restricted by statute.                   DC. This Docket Facility is open from
                                                  BILLING CODE 4164–01–P                                                Multimedia submissions (audio, video,                        8:30 a.m. to 4:30 p.m., Monday through
                                                                                                                        etc.) must be accompanied by a written                       Friday, excluding legal holidays. The
                                                                                                                        comment. The written comment is                              telephone number for the Public
                                                  ENVIRONMENTAL PROTECTION                                              considered the official comment and                          Reading Room is (202) 566–1744, and
                                                  AGENCY                                                                should include discussion of all points                      the telephone number for the Air Docket
                                                                                                                        you wish to make. The EPA will                               is (202) 566–1742.
                                                  40 CFR Part 51                                                        generally not consider comments or                           FOR FURTHER INFORMATION CONTACT: Mr.
                                                  [EPA–HQ–OAR–2016–0456; FRL–9966–75–
                                                                                                                        comment contents located outside of the                      Ned Shappley, Office of Air Quality
                                                  OAR]                                                                  primary submission (i.e., on the Web,                        Planning and Standards, Air Quality
                                                                                                                        Cloud, or other file sharing system). For                    Assessment Division, Measurement
                                                  RIN 2060–AS91                                                         additional submission methods, the full                      Technology Group (E143–02),
                                                                                                                        EPA public comment policy,                                   Environmental Protection Agency,
                                                  Method 202—Dry Impinger Method for                                    information about CBI or multimedia
                                                  Determining Condensable Particulate                                                                                                Research Triangle Park, NC 27711;
                                                                                                                        submissions, and general guidance on                         telephone number: (919) 541–5225; fax
                                                  Emissions From Stationary Sources                                     making effective comments, please visit                      number: (919) 541–0516; email address:
                                                                                                                        http://www2.epa.gov/dockets/
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                                                  AGENCY:  Environmental Protection                                                                                                  shappley.ned@epa.gov.
                                                  Agency (EPA).                                                         commenting-epa-dockets.
                                                                                                                                                                                     SUPPLEMENTARY INFORMATION: The
                                                  ACTION: Proposed rule.                                                  Public Hearing. If a public hearing is
                                                                                                                        requested, it will be held at EPA                            following topics are discussed in this
                                                  SUMMARY:   In this action, the                                        Headquarters, William Jefferson Clinton                      preamble.
                                                  Environmental Protection Agency (EPA)                                 East Building, 1201 Constitution                             I. General Information
                                                  proposes editorial and technical                                      Avenue NW., Washington, DC 20004. If                            A. Does this action apply to me?
                                                  revisions to the EPA’s Method 202—Dry                                 a public hearing is requested, then we                          B. What should I consider as I prepare my
                                                  Impinger Method for Determining                                       will provide details about the public                             comments?



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                                                                                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                                           42509

                                                     C. Where can I get a copy of this document                                 C. Paperwork Reduction Act (PRA)                     action applies to sources through
                                                       and other related information?                                           D. Regulatory Flexibility Act (RFA)                  actions by state and local agencies that
                                                                                                                                E. Unfunded Mandates Reform Act
                                                  II. Background                                                                                                                     implement CPM control measures to
                                                                                                                                   (UMRA)
                                                                                                                                F. Executive Order 13132: Federalism                 attain the National Ambient Air Quality
                                                  III. Summary of Proposed Revisions
                                                                                                                                G. Executive Order 13175: Consultation               Standards (NAAQS) for particles less
                                                     A. Blank Correction
                                                                                                                                   and Coordination With Indian Tribal               than 2.5 micrometers in diameter
                                                     B. Procedures for the Field Train Proof
                                                                                                                                   Governments                                       (PM2.5) and specify the use of EPA
                                                        Blank
                                                                                                                                H. Executive Order 13045: Protection of              Method 202 to demonstrate compliance
                                                     C. Configuration of the Vertical Condenser
                                                                                                                                   Children From Environmental Health                with the control measures. State, tribal,
                                                     D. Use of Graduated Cylinders
                                                                                                                                   Risks and Safety Risks
                                                     E. Limitations of Method 202
                                                                                                                                I. Executive Order 13211: Actions That               and local agencies that specify the use
                                                     F. Required Use of Method 202                                                                                                   of EPA Method 202 would have to
                                                                                                                                   Significantly Affect Energy Supply,
                                                     G. Sample Container Material                                                  Distribution, or Use                              implement the following requirements:
                                                     H. Weighing Containers
                                                     I. Laboratory Analytical Balance
                                                                                                                                J. National Technology Transfer and                  (1) Adopt this method in rules or
                                                                                                                                   Advancement Act (NTTAA)                           permits (either by incorporation by
                                                        Requirements                                                            K. Executive Order 12898: Federal Actions
                                                     J. Field Balance Requirements                                                                                                   reference or by duplicating the method
                                                                                                                                   To Address Environmental Justice in
                                                     K. pH Measurement                                                             Minority Populations and Low-Income
                                                                                                                                                                                     in its entirety) and (2) promulgate an
                                                     L. Glassware Cleaning Procedures                                              Populations                                       emissions limit requiring the use of EPA
                                                     M. Reagent Blanks                                                                                                               Method 202 (or a method that
                                                     N. Nitrogen Purge Requirements                                         I. General Information                                   incorporates EPA Method 202). This
                                                     O. Data Record Requirements
                                                     P. Method Detection Limits                                             A. Does this action apply to me?                         action also applies to stationary sources
                                                     Q. Alternative Blank Procedure and                                                                                              that are required to meet applicable
                                                                                                                              This action applies to you if you
                                                        Correction Value                                                                                                             CPM requirements established through
                                                                                                                            operate a stationary source that is
                                                                                                                                                                                     federal, state, or tribal rules or
                                                  IV. Request for Comments                                                  subject to applicable requirements to
                                                                                                                            control or measure condensable                           permitting programs such as New
                                                  V. Statutory and Executive Order Reviews                                                                                           Source Performance Standards and New
                                                                                                                            particulate matter (CPM) emissions
                                                    A. Executive Order 12866: Regulatory                                    where EPA Method 202 is incorporated                     Source Review (NSR), which specify the
                                                      Planning and Review and Executive
                                                                                                                            as a component of the applicable test                    use of EPA Method 202 to demonstrate
                                                      Order 13563: Improving Regulation and                                                                                          compliance with the control measures.
                                                      Regulatory Review                                                     method. In addition, this action applies
                                                    B. Executive Order 13771: Reducing                                      to you if federal, state, tribal, or local                 The source categories and entities
                                                      Regulations and Controlling Regulatory                                agencies take certain additional                         potentially affected include, but are not
                                                      Costs                                                                 independent actions. For example, this                   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                                     ROM that you mail to the EPA, mark the                   disclosed except in accordance with
                                                  the applicability of the proposed                                         outside of the disk or CD–ROM as CBI                     procedures set forth in 40 Code of
                                                  changes to Method 202, contact the                                        and then identify electronically within                  Federal Regulations (CFR) part 2.
                                                  person listed in the preceding FOR                                        the disk or CD–ROM the specific                            Do not submit information that you
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                  FURTHER INFORMATION CONTACT section.                                      information that is claimed as CBI. In                   consider to be CBI or otherwise
                                                  B. What should I consider as I prepare                                    addition to one complete version of the                  protected through http://
                                                  my comments?                                                              comment that includes information                        www.regulations.gov or email. Send or
                                                                                                                            claimed as CBI, a copy of the comment                    deliver information identified as CBI to
                                                  1. Submitting CBI                                                         that does not contain the information                    only the following address: OAQPS
                                                     Clearly mark the part or all of the                                    claimed as CBI must be submitted for                     Document Control Officer (Room C404–
                                                  information that you claim to be CBI.                                     inclusion in the public docket.                          02), U.S. EPA, Research Triangle Park,
                                                  For CBI information in a disk or CD–                                      Information marked as CBI will not be


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                                                  42510                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                  NC 27711, Attention Docket ID No.        EPA previously developed and                                         of the earlier EPA work and addressed
                                                  EPA–HQ–OAR–2016–0456.                    promulgated Method 202                                               some additional issues. The report of
                                                    If you have any questions about CBI    (Determination of Condensable                                        that work is available in the docket as
                                                  or the procedures for claiming CBI,      Particulate Emissions from Stationary                                EPA–HQ–OAR–2016–0456–0002. In
                                                  please consult the person identified in  Sources) in 40 CFR part 51, appendix M                               2009, an EPA contractor conducted a
                                                  the FOR FURTHER INFORMATION CONTACT      (Recommended Test Methods for State                                  third study, ‘‘Evaluation and
                                                  section.                                 Implementation Plans).                                               Improvement of Condensable
                                                                                              Specifically, on December 17, 1991                                Particulate Matter Measurement,’’ that
                                                  2. Docket
                                                                                           (56 FR 65433), the EPA first                                         presents the results of a laboratory
                                                     The docket number for the Method      promulgated Method 202 to provide a                                  evaluation of a dry impinger
                                                  202 revisions is Docket ID No. EPA–      test method for measuring CPM from                                   modification to Method 202. The report
                                                  HQ–OAR–2016–0456.                        stationary sources. Method 202, as                                   of that work is available in the docket
                                                  C. Where can I get a copy of this        promulgated in 1991, used water-filled                               as EPA–HQ–OAR–2016–0456–0003.
                                                  document and other related               impingers to cool, condense, and collect                                In 2010, the EPA promulgated
                                                  information?                             materials that are vaporous at stack                                 amendments to Method 202 (75 FR
                                                                                           conditions and become solid or liquid                                80118) to improve the measurement of
                                                     World Wide Web (WWW). In addition     PM at ambient air temperatures. Method                               fine PM emissions. The final
                                                  to being available in the docket, an     202, as promulgated in 1991, contains                                amendments revised the sample
                                                  electronic copy of the proposed method several optional procedures that were                                  collection and recovery procedures of
                                                  revisions is available on the Air        intended to accommodate the various                                  the method to: (1) Reduce the potential
                                                  Emission Measurement Center (EMC)        test methods in use by state and local                               for CPM formation due to oxidation of
                                                  Web site at https://www.epa.gov/emc/     regulatory entities at the time Method                               dissolved SO2 when using Method 202
                                                  emc-proposed-test-methods.               202 was being developed.                                             (as promulgated in 1991) and (2)
                                                  II. Background                              When conducted consistently and                                   promote consistent application of the
                                                                                           carefully, this version of the method                                method by eliminating most of the
                                                     Section 110 of the Clean Air Act, as  provided improved precision for most                                 hardware and analytical options in the
                                                  amended (42 U.S.C. 7410), requires state emission sources, and has been                                       existing method. The most significant
                                                  and local air pollution control agencies successfully implemented in regulatory                               procedural changes were the addition of
                                                  to develop, and submit for EPA           programs where the emission limits and                               a condenser prior to the first impinger,
                                                  approval, State Implementation Plans     compliance demonstrations are                                        the removal of water from the two
                                                  (SIPs) that provide for the attainment,  established based on a consistent                                    impingers between the condenser and
                                                  maintenance, and enforcement of the      application of Method 202 and its                                    the CPM filter, and the addition of the
                                                  NAAQS in each air quality control        associated options. However, when the                                requirement for a post-test nitrogen
                                                  region (or portion thereof) within each  same emission source is tested using                                 purge. These revisions increased the
                                                  state. The emissions inventory and       different combinations of the optional                               precision of Method 202 and reduced
                                                  analyses used in the state’s attainment  procedures within the method, there                                  potential positive and negative biases by
                                                  demonstrations must consider PM2.5 and were variations in the measured CPM                                    removal of the myriad of options and
                                                  particles less than 10 micrometers in    emissions. Additionally, during                                      elimination of water in the two
                                                  diameter (PM10) emissions from           validation of the method, we                                         impingers, which significantly
                                                  stationary sources that are significant  determined that sulfur dioxide (SO2) gas                             improved the consistency in the
                                                  contributors of primary PM10 and PM2.5   (a typical component of emissions from                               measurements obtained between source
                                                  emissions. Primary or direct PM          several types of stationary sources) can                             tests performed under different
                                                  emissions are the solid particles or     be absorbed partially in the impinger                                regulatory authorities.
                                                  liquid droplets emitted directly from an solutions and can react chemically to                                   On April 8, 2014, the EPA issued
                                                  air emissions source or activity and the form sulfuric acid. This sulfuric acid                               interim guidance on the treatment of
                                                  gaseous emissions or liquid droplets     ‘‘artifact’’ is not related to the primary                           CPM results in the Prevention of
                                                  from an air emissions source or activity emission of CPM from the source, but                                 Significant Deterioration (PSD) and
                                                  that condense to form PM or liquid       may be counted erroneously as CPM                                    Nonattainment NSR Permitting
                                                  droplets at ambient temperatures.        when using Method 202. The EPA                                       Programs. The purpose of this guidance
                                                     Subpart A of 40 CFR part 51           conducted additional studies to further                              was to address concerns that CPM test
                                                  (Requirements for Preparation,           examine the mechanism and the effects                                results obtained with the method could
                                                  Adoption, and Submittal of               of sulfuric acid formation. The results of                           include a positive bias that results in the
                                                  Implementation Plans) defines primary    our 1989 laboratory study and field                                  overestimation of emissions due to the
                                                  PM2.5 and PM10 as including both the     evaluation commissioned to evaluate                                  potential for blank contamination
                                                  filterable and condensable fractions of  the impinger approach can be found in                                associated with the implementation of
                                                  PM. Filterable PM consists of those      ‘‘Laboratory and Field Evaluation of the                             Method 202. In this interim guidance,
                                                  particles that are directly emitted by a EPA Method 5 Impinger Catch for                                      we recommend to air agencies and
                                                  source as a solid or liquid at the stack Measuring Condensible Matter from                                    permit applicants that it is appropriate
                                                  (or similar release conditions) and      Stationary Sources.’’ The report of that                             on an interim basis to allow major
                                                  captured on the filter of a stack test   work is available in the docket as EPA–                              source permit applicants to depart from
                                                  sampling train. Condensable PM is the    HQ–OAR–2016–0456–0001. Essentially,                                  one aspect of Method 202, specifically
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                                                  material that is in vapor phase at stack the 1989 study verified the need for a                               the current upper limit of 2.0 milligrams
                                                  conditions but condenses and/or reacts   nitrogen purge when SO2 is present in                                (mg) for the field train recovery blank.
                                                  upon cooling and dilution in the         stack gas and also provided guidance for                             Consistent with this guidance, during
                                                  ambient air to form solid or liquid PM   analyzing the collected samples. In                                  the prescribed interim period, air
                                                  immediately after discharge from the     2005, an EPA contractor conducted a                                  agencies may allow permit applicants to
                                                  stack. In response to the need to        second study, ‘‘Laboratory Evaluation of                             use field train proof blanks, in lieu of
                                                  quantify primary PM10 and PM2.5          Method 202 to Determine Fate of SO2 in                               the field train recovery blanks, and
                                                  emissions from stationary sources, the   Impinger Water,’’ that replicated some                               blank values as high as 5.1 mg can then


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                           42511

                                                  be used in the calculation of CPM                       requirement and the associated text in                sources of possible contamination
                                                  emissions. As part of this guidance, the                section 9.10 from the method.                         experienced by the field samples.
                                                  EPA announced plans to issue guidance                      The EPA received technical
                                                                                                                                                                C. Configuration of the Vertical
                                                  on best practices for Method 202                        information and recommendations from
                                                                                                                                                                Condenser
                                                  implementation and to revise Method                     the National Council on Air and Stream
                                                  202 as necessary. In addition, this                     Improvement (NCASI) supporting the                      Currently, Method 202 does not
                                                  guidance stated that the interim                        use of a field train proof blank to                   specify the orientation of the moisture
                                                  guidance period will end on the                         evaluate method blank correction. The                 condenser located before the first
                                                  effective date of any revision that the                 EPA believes the updated field train                  impinger of the sampling train.
                                                  EPA may make for Method 202                             proof blank is a better indicator of the              Although the sampling trains depicted
                                                  regarding the use of blanks in the field                total systematic blank error for Method               in Figures 1 through 3 show the
                                                  train on individual test results. We                    202 sample runs. Under the proposed                   placement of the condenser, the incline
                                                  intend that the interim guidance will no                amendments, a clean and prepared                      of the condenser in the figures is not
                                                  longer apply as of the effective date of                sampling train is transported and fully               specified.
                                                  the final rule resulting from this                      assembled at the sampling location, leak                When the condenser is installed
                                                  proposal. A copy of the interim                         checked, left in place without collecting             horizontally or at an angle, condensed
                                                  guidance is available in the docket                     a sample, purged with nitrogen, and                   moisture may pool in the condenser
                                                  (EPA–HQ–OAR–2016–0456–003) and                          recovered in the same manner as a                     coils, increasing the potential for SO2 to
                                                  on the EMC Web site at https://                         sample collection train. All components               dissolve into that water and slowly
                                                  www3.epa.gov/ttn/emc/methods/                           of the Method 202 sampling train must                 oxidize to form CPM that is not related
                                                  psdnsrinterimcmpmemo4814.pdf.                           be included in the field train proof                  to the primary emission of CPM from
                                                     On March 10, 2016, the EPA released                  blank to properly quantify the blank                  the source. We believe that requiring the
                                                  the EPA Method 202 Best Practices                       value. The field train proof blank                    condenser to be installed vertically will
                                                  Handbook. This handbook provides                        represents the systematic bias associated             minimize pooling of condensed
                                                  quality control procedures for                          with all of the uncertainty from the                  moisture in the condenser coils, thereby
                                                  evaluating the cause of blank                           reagents, sampling media, glassware                   reducing the potential for this bias and
                                                  contamination and practices to reduce                   preparation, recovery and analysis                    promoting consistency in CPM
                                                  contamination, so that testers may                      procedures, environmental                             measurement.
                                                  achieve the expected results when using                                                                         In this action, we propose revisions to
                                                                                                          contamination, leak checks, and test
                                                  Method 202. A copy of this handbook is                                                                        sections 2.1.2, 6.1.2, and 8.4.1 to require
                                                                                                          crew sample handling.
                                                  available in the docket as EPA–HQ–                                                                            that the moisture condenser be installed
                                                  OAR–2016–0456–004 and on the EMC                        B. Procedures for the Field Train Proof               in a vertical orientation. We propose to
                                                  Web site at https://www3.epa.gov/ttn/                   Blank                                                 revise Figures 1 through 3 to depict the
                                                  emc/methods/m202-best-practices-                           In the current version of Method 202,              condenser in the vertical position
                                                  handbook.pdf.                                           the setup and recovery procedures for                 consistent with the changes to the
                                                                                                          the field train proof blank are                       method text. We also propose to revise
                                                  III. Summary of Proposed Revisions                                                                            section 6.1.4 (and renumber as section
                                                                                                          incomplete. We are proposing the
                                                     In this action, we are proposing                     following revisions for the field train               6.1.3) to allow other equipment options
                                                  technical revisions and editorial                       proof blank setup and recovery                        to purge the water in the dropout
                                                  changes to clarify and update the                       procedures specified in sections 8.5.5.8,             impinger.
                                                  requirements and procedures specified                   8.5.5.8.1, 8.5.5.8.2, and 9.9:                        D. Use of Graduated Cylinders
                                                  in Method 202. Proposed editorial                          • Adding a full sampling train setup
                                                  changes include correcting inconsistent                                                                         Currently, Method 202 allows the use
                                                                                                          including the front half of the train for
                                                  terminology, improving readability, and                                                                       of a graduated cylinder to measure the
                                                                                                          collecting filterable PM, probe extension
                                                  simplifying text to aid in consistent                                                                         volume of moisture collected in the
                                                                                                          and/or transfer line, condenser,
                                                  implementation of the method.                                                                                 impingers and the silica gel trap for the
                                                                                                          impingers, and filter used to collect the
                                                  Proposed technical revisions are                                                                              purpose of calculating the moisture
                                                                                                          CPM.
                                                  discussed below.                                           • Requiring that the entire filterable             content of the effluent gas. We believe
                                                                                                          PM and CPM sampling train is                          that using a graduated cylinder to
                                                  A. Blank Correction                                                                                           measure the accumulated water is not
                                                                                                          transported to and assembled at the
                                                     In this action, we propose to replace                sampling location.                                    sensitive enough to measure the
                                                  the field train recovery blank                             • Adding pre- and post-test leak                   moisture and potentially adds an
                                                  requirement used to determine the                       checks.                                               unnecessary additional source for
                                                  blank correction (up to 2.0 mg) with a                     • Exposing the assembled field train               potential loss of condensable particulate
                                                  field train proof blank requirement. In                 proof blank sampling train to the                     residual mass in samples measured by
                                                  the current version of Method 202, the                  sampling environment for the same                     Method 202. Therefore, we propose to
                                                  result of the field train recovery blank                duration as the test runs to be                       revise section 8.5.3.4 (and renumber as
                                                  is used as the basis for the blank                      conducted.                                            section 8.5.3) to remove the option to
                                                  correction (up to 2.0 mg). Specifically,                   • Performing a post-test nitrogen                  use graduated cylinders and to require
                                                  we propose to revise section 8.5.4.10                   purge of the field train proof blank.                 use of a balance to determine the mass
                                                  (and renumber as section 8.5.5.8) to                       • Requiring recovery of the sampling               of each impinger for the purpose of
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                                                  require conducting a field train proof                  train components identical to how field               measuring the moisture collected during
                                                  blank to demonstrate the cleanliness of                 samples are recovered.                                sampling. Instructions to weigh each
                                                  the sampling train. We propose to revise                   In this action, we are also proposing              impinger before testing, which is a
                                                  sections 9.9, 12.1, and 12.2.2, and                     to add section 8.5.5.8.3 to include                   necessary step for determining the
                                                  Figures 4, 5, and 6 to replace the field                procedures for handling the CPM filter                amount of moisture collected when
                                                  train recovery blank with the field train               from the field train proof blank. We                  using a balance, are proposed for
                                                  proof blank. We also propose to remove                  believe that the proposed revisions will              relocation to section 8.4.5. We also
                                                  the field train recovery blank                          generate blank samples that duplicate                 propose to make accompanying


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                                                  42512                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                  revisions in sections 8.5.1.1, 8.5.1.2, and             otherwise specified by an applicable                  aluminum weighing tins can be used for
                                                  11.1(b) to clarify the procedures for                   subpart.                                              final sample evaporation and weighing.
                                                  weighing the impingers and captured                                                                           In this action, we propose to include a
                                                                                                          F. Required Use of Method 202
                                                  moisture. Sections related to                                                                                 list of acceptable weighing containers
                                                  transferring the moisture-trap impinger                    Condensable PM is formed from                      that includes fluoropolymer beaker
                                                  and silica gel impinger contents in                     gaseous materials that condense and/or                liners and other vessels that have low
                                                  sample containers for measurement                       react upon cooling and dilution in the                mass and are unreactive to the sample
                                                  using graduated cylinders are proposed                  ambient air. Method 202 requires the                  and the atmosphere. Laboratories have
                                                  to be removed.                                          use of a particulate sampling method                  reported that aluminum weighing tins
                                                                                                          (e.g., Method 5, 17, or 201A) to                      may oxidize in contact with some
                                                  E. Limitations of Method 202                            separately collect the filterable PM from             sample matrices. The heavier weight of
                                                     High moisture in the sampled gas                     CPM.                                                  some glass beakers or containers may
                                                  stream can result in the accumulation of                   Filterable PM methods that collect                 cause difficulty with measurement of
                                                  SO2 in the collected moisture resulting                 particulate out-of-stack have specified               trace amounts of residual mass. We
                                                  in a positive bias for CPM                              filter temperature requirements and                   propose to revise sections 6.2.2(b),
                                                  measurements. As the moisture                           require the addition of a Method 202                  11.2.2.3, 11.2.3, 11.2.4, 11.2.5, and
                                                  accumulates in the sample impingers,                    sampling train to collect CPM. Filterable             11.2.6 to remove the connotation of
                                                  the method performs similarly to the                    PM methods that employ in-stack filters               sampling ‘‘tin’’ as an implicit approval
                                                  original version of Method 202 where                    collect particulate material at the source            of aluminum tins.
                                                  SO2 in the effluent could react in the                  gas temperature.
                                                  condensed moisture and form sulfuric                       If the temperature of the filterable PM            I. Laboratory Analytical Balance
                                                  acid that may be counted erroneously as                 sampling equipment, including the                     Requirements
                                                  CPM. In addition, longer sampling times                 filter, meets Method 202 temperature                     We propose additional quality control
                                                  coupled with high moisture can (in the                  requirements (i.e., ≤30 °C (85 °F)), both             requirements for analytical balance use.
                                                  water-contained impingers) allow more                   filterable and CPM are collected                      Currently, section 9.6 of Method 202
                                                  SO2 conversion to CPM since the                         together on the filter and CPM is not                 requires calibration of the analytical
                                                  conversion of SO2 to CPM has a                          quantified independently but rather as                balance on each day that samples are
                                                  relatively slow reaction rate.                          total particulate, total PM10, or total               weighed, and section 10.3 of the Method
                                                     Section 8.5.1.1 of Method 202                        PM2.5 depending on the filterable                     202 Best Practices Handbook provides
                                                  recommends removing moisture from                       collection method.                                    additional steps that stack testers can
                                                  the sampling train during the test run                     In this action, we propose to revise               use to improve consistency in analytical
                                                  when the amount of moisture collected                   section 1.2 to clearly state that, if the             balance measurements. In this action,
                                                  is greater than half the capacity of the                sample gas filtration temperature never               we propose to amend section 9.6 to
                                                  water dropout impinger or the moisture                  exceeds 30 °C (85 °F), then Method 202                specify the correct mass standard to use
                                                  level of the back-up impinger is above                  is not required to measure total primary              for the Analytical Calibration Check,
                                                  the impinger tip.                                       PM because the CPM would be collected
                                                     Longer sampling run times also delay                                                                       specifications for the temperature and
                                                                                                          with the filterable PM.                               humidity control in weighing areas and
                                                  the start of the post-test nitrogen purge.
                                                  The post-test nitrogen purge is designed                G. Sample Container Material                          requirements for balance calibration
                                                  to remove dissolved gasses from the                                                                           checks that approximately match the
                                                                                                             Currently, section 6.2.1(d) of Method
                                                  accumulated moisture and thus reduce                                                                          sample measurements to include the
                                                                                                          202 specifies the use of amber glass
                                                  the potential chemical reactions. In this                                                                     following requirements:
                                                                                                          sample bottles for sample recovery. In
                                                  action, we propose to amend Method                      this action, we propose to revise section                • The laboratory analytical balance
                                                  202 by adding a recommendation in                       6.2.1(d) to allow the use of sample                   must be maintained at a constant
                                                  section 1.5 to limit the sampling time to               containers made from other non-reactive               temperature of 20 °C ± 3 °C (68 °F ±
                                                  2 hours for Method 202 testing when                     materials (e.g., high density                         5 °F).
                                                  excessive moisture collection is                        polyethylene (HDPE),                                     • The relative humidity at the
                                                  expected. We also propose revisions to                  polytetrafluoroethylene (PTFE)) as an                 location of the laboratory analytical
                                                  section 8.5.1.1 to specify that if                      alternative to amber glass bottles for                balance must be maintained at 35 to 50
                                                  accumulated water exceeds half of the                   inorganic (aqueous) samples. We also                  percent, with the exception that if the
                                                  capacity of the water dropout impinger,                 propose to revise sections 6.2.1(d),                  relative humidity is lower than 35
                                                  or if water accumulates in the back-up                  8.5.5.3, 8.5.5.5, and 8.5.5.7 to require              percent, the relative humidity must be
                                                  impinger sufficient to cover the                        cleaning of all sample containers                     maintained within ±10 percent during
                                                  impinger tip, the impinger(s) must be                   according to the procedures in section                sample weighing.
                                                  removed and replaced with new pre-                      8.4 prior to use.                                        • The results of the calibration check
                                                  weighed impingers and all resulting                        Although we are proposing to revise                of the laboratory analytical balance must
                                                  impingers must be weighed, purged and                   the method to allow use of polymer or                 be within 0.05 percent of the applicable
                                                  recovered following the procedures of                   glass sample containers for inorganic                 certified weight.
                                                  the method.                                             samples, we continue to require glass                    • The laboratory analytical balance
                                                     The current version of Method 202                    containers for organic samples. The                   must be checked each day it is used for
                                                  also prohibits the use of certain                                                                             gravimetric measurements by weighing
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                                                                                                          proposed revisions would provide
                                                  filterable particulate test methods in                  testers with an alternative for storing               at least one ASTM E617–13 Class 2
                                                  conjunction with Method 202. In this                    inorganic samples to avoid this                       tolerance (or better) calibration weight
                                                  action, we propose revisions to section                 potential source of contamination.                    that corresponds to 50 to 150 percent of
                                                  1.4 to state only the acceptable filterable                                                                   the weight of one filter or between 1
                                                  particulate test methods and to include                 H. Weighing Containers                                gram (g) and 5 g. If the scale cannot
                                                  a note that you must maintain the gas                     Currently, section 6.2.2(b) of Method               reproduce the value of the calibration
                                                  filtration temperature as specified in the              202 specifies that glass evaporation                  weight to within 0.5 mg of the certified
                                                  filterable PM test method unless                        vials, fluoropolymer beaker liners, or                mass, perform corrective measures and


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                          42513

                                                  conduct the multipoint calibration                      highly recommended baking of                          could potentially contaminate samples
                                                  before use.                                             glassware as discussed in the EPA                     and outweigh the advantages of train
                                                                                                          Method 202 Best Practices Handbook).                  purges done immediately following the
                                                  J. Field Balance Requirements                              • Removing the option to use the                   sampling. In this action, we propose to
                                                     In this action, we propose to correct                field train proof blank as an alternative             revise section 8.5.4 to eliminate the
                                                  section 9.4 to specify the mass standard                to baking since the field train proof                 option for performing the post-test
                                                  with which to conduct the field balance                 blank is being proposed as a                          nitrogen purge using the meter box and
                                                  calibration check. We believe that this                 requirement of Method 202.                            vacuum pump. We also propose to make
                                                  additional requirement is necessary to                     • Adding a recommended procedure                   accompanying revisions in sections
                                                  increase consistency of Method 202                      for cleaning the probe liners by heating              8.5.4.1, 8.5.4.2, 8.5.4.4 and 8.5.4.5.
                                                  moisture sample measurements. We                        for a period of at least 3 hours at the
                                                  propose the requirement that the field                  maximum practical temperature.                        O. Data Record Requirements
                                                  balance calibration check be performed                     These proposed revisions make the                     In this action, we propose the
                                                  daily with an ASTM E617–13 Class 6 (or                  glassware cleaning procedures                         following amendments to Method 202
                                                  better) weight.                                         performance-based, clarify the                        sections to record and report test
                                                                                                          requirements, and provide testers with                information that were either absent or
                                                  K. pH Measurement                                       an additional method for ensuring                     undefined in the current promulgated
                                                     In sections 6.2.2(h) and 11.2.2.2 of the             cleanliness of the probe liners.                      method:
                                                  current method, pH measurement by pH                                                                             • Record the pre- and post-test
                                                  meter or colorimetric pH indicator is                   M. Reagent Blanks
                                                                                                                                                                weights of the impingers, as well as the
                                                  allowable for the titration procedure.                     Currently, Method 202 specifies a
                                                                                                                                                                color of the indicating silica gel, at the
                                                  While the use of a colorimetric (e.g.,                  volume of 150 milliliters (mL) for
                                                                                                                                                                completion of sampling (sections 8.4.5
                                                  Phenolphthalein) indicator is an                        performing reagent blank analyses and
                                                                                                                                                                and 8.5.3).
                                                  acceptable technique for accurately                     specifies that field reagent blanks are
                                                                                                                                                                   • Record the results of the pre- and
                                                  determining the end-point of an acid-                   optional. In this action, we propose to
                                                                                                                                                                post-test leak checks of the sampling
                                                  base titration, we are concerned that                   revise section 9.7 to specify a minimum
                                                                                                                                                                train (sections 8.4.6 and 8.5.2).
                                                  determining the pH using colorimetric                   volume of 200 mL for these field reagent
                                                                                                          blank volumes and to revise section 9.8                  • Record the time (hh:mm), nitrogen
                                                  pH indicators may introduce additional
                                                                                                          to require analysis of field reagent                  flowrate, CPM filter temperature, and
                                                  error in the measurement of CPM due to
                                                                                                          blanks in the performance of Method                   moisture trap temperature (if applicable)
                                                  over-titration.
                                                                                                          202. We also propose to make                          during the post-test nitrogen purge
                                                     In this action, we propose to amend
                                                                                                          accompanying revisions to sections                    (section 8.5.4.4).
                                                  sections 6.2.2(h) and 11.2.2.2 to remove
                                                  the option of using a colorimetric pH                   8.5.5.5, 8.5.5.6, 8.5.5.7, 11.2.4, 11.2.5,               • Record the results of the field and
                                                  indicator and require the use of a pH                   and 11.2.6.                                           laboratory analytical balance calibration
                                                  meter whose calibration has been                           The original solvent blank volume                  checks (sections 9.4 and 9.6.4).
                                                  checked immediately prior to the                        was intended to represent amounts                        • Record the temperature and relative
                                                  titration step. We also propose to correct              typically used during sample recovery.                humidity conditions of the laboratory
                                                  the CPM Sample Processing Flow Chart                    A larger reagent blank volume is                      analytical balance (section 9.6.3).
                                                  for sample analysis (Figure 8). We                      necessary to quantify residual mass                   P. Method Detection Limits
                                                  believe these revisions will increase the               using the analytical balance specified in
                                                  consistency and comparability of                        Method 202 with a sensitivity of 0.0001                  In this action, we propose to revise
                                                  Method 202 results between source                       g (0.1 mg). These proposed revisions are              section 13.0 regarding method
                                                  tests.                                                  based on recommendations received                     performance. We updated method
                                                                                                          from state agencies. This change to the               detection limit values based on a formal
                                                  L. Glassware Cleaning Procedures                        method quality control quantifies any                 study submitted to the EPA by NCASI
                                                     To obtain reliable CPM data using                    addition to the sample mass from gross                that evaluated the zero bias of Method
                                                  Method 202 for PSD and NSR permits,                     contamination originating from the use                202 when Method 202 Best Practices
                                                  residual mass from sampling and                         of reagents in the field.                             were implemented. A copy of this study
                                                  analysis equipment must be minimized.                                                                         titled, ‘‘Method 202 Zero Bias Study
                                                     In this action, we propose the                       N. Nitrogen Purge Requirements                        When Incorporating Draft Best Practices
                                                  following amendments to clarify                            Method 202, as promulgated in 2010,                Developed by the US EPA,’’ (NCASI
                                                  equipment and glassware cleaning in                     includes two approaches for performing                2017) is available in the docket (EPA–
                                                  section 8.4 of Method 202, including:                   the post-test nitrogen purge: (1) A                   HQ–OAR–2016–0456–005).
                                                     • Adding a specification that all                    negative pressure purge using the pump
                                                                                                                                                                Q. Alternative Blank Procedure and
                                                  glassware used in the implementation of                 and meter box from the sampling train
                                                                                                                                                                Correction Value
                                                  Method 202, including the impinger                      or (2) a positive pressure purge using
                                                  train and sample containers, should be                  the gas cylinder pressure to propel the                 While the EPA believes that field train
                                                  cleaned sufficiently to meet the blank                  nitrogen gas through the CPM collection               proof blank results of 2.0 mg or less are
                                                  correction maximum limit of 2.0 mg in                   components.                                           achievable, we recognize there may be
                                                  section 9.9.                                               The intent of the multiple purge                   certain instances when the environment
                                                     • Removing the statement referencing                 options was to allow the testing                      surrounding the sampling location may
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                                                  cleaning silicone grease so that it is not              contractors to either purge the sampling              significantly contribute to the
                                                  mistakenly viewed as acceptable to use                  train on or near the sampling location or             systematic bias of the method results as
                                                  such grease in Method 202 sampling                      to transport the train components to a                measured by the field train proof blank.
                                                  trains.                                                 controlled environment less susceptible               This proposed alternative procedure
                                                     • Removing the requirement that                      to sources of contamination. We now                   would account for the uncontrollable
                                                  glassware must be baked after cleaning                  believe that a post-test nitrogen purge of            environmental bias associated with
                                                  (although the EPA is proposing to                       the sampling train using the meter box                measurements collected in problematic
                                                  remove the baking requirement, we                       and a vacuum pump adds steps that                     sampling locations.


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                                                  42514                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                     In this action, we are proposing to                  requirements on regulated entities                    K. Executive Order 12898: Federal
                                                  amend section 16.1 of Method 202 to                     beyond those specified in the current                 Actions To Address Environmental
                                                  allow the combined results from                         regulations, nor do they change any                   Justice in Minority Populations and
                                                  multiple field train proof blanks to be                 emission standard.                                    Low-Income Populations
                                                  used as the basis for blank correction up                                                                       The EPA believes that this action is
                                                  to 3.9 mg when approved by the                          E. Unfunded Mandates Reform Act
                                                                                                          (UMRA)                                                not subject to Executive Order 12898 (59
                                                  regulatory authority. The 3.9 mg value                                                                        FR 7629, February 16, 1994) because it
                                                  is based on the Upper Prediction Limit                    This action does not contain any                    does not establish an environmental
                                                  (UPL) of the NCASI field study used to                                                                        health or safety standard. This action
                                                                                                          unfunded mandate of $100 million or
                                                  update the method detection limit                                                                             makes corrections and updates to
                                                                                                          more as described in UMRA, 2 U.S.C.
                                                  (NCASI 2017). In this procedure, we                                                                           existing testing methodology and does
                                                                                                          1531–1538, and does not significantly or
                                                  have included conditions and criteria                                                                         not have any impact on human health
                                                  that a facility must satisfy in order to                uniquely affect small governments. The
                                                                                                          action imposes no enforceable duty on                 or the environment.
                                                  demonstrate need for the alternative
                                                  procedure.                                              any state, local or tribal governments or             List of Subjects in 40 CFR Part 51
                                                                                                          the private sector.
                                                  IV. Request for Comments                                                                                        Administrative practice and
                                                                                                          F. Executive Order 13132: Federalism                  procedure, Air pollution control, EPA
                                                    The EPA is requesting public                                                                                Method 202, Incorporation by reference,
                                                  comments on all of the proposed                           This action does not have federalism                Particulate matter, Reporting and
                                                  editorial and technical amendments to                   implications. It will not have substantial            recordkeeping requirements, Sulfur
                                                  Method 202. For the convenience of the                  direct effects on the states, on the                  dioxide.
                                                  reader, we include in this notice the                   relationship between the national                       Dated: August 23, 2017.
                                                  entire text of Method 202, including                    government and the states, or on the
                                                  proposed revisions, but the scope of this                                                                     E. Scott Pruitt,
                                                                                                          distribution of power and
                                                  rulemaking is limited to the proposed                                                                         Administrator.
                                                                                                          responsibilities among the various
                                                  revisions and does not include any                      levels of government.                                   For the reasons stated in the
                                                  unchanged provisions.                                                                                         preamble, the Environmental Protection
                                                                                                          G. Executive Order 13175: Consultation                Agency proposes to amend title 40,
                                                  V. Statutory and Executive Order                        and Coordination With Indian Tribal                   chapter I of the Code of Federal
                                                  Reviews                                                 Governments                                           Regulations as follows:
                                                    Additional information about these
                                                  statutes and Executive Orders can be                      This action does not have tribal                    PART 51—REQUIREMENTS FOR
                                                  found at http://www2.epa.gov/laws-                      implications, as specified in Executive               PREPARATION, ADOPTION, AND
                                                  regulations/laws-and-executive-orders.                  Order 13175. This action proposes                     SUBMITTAL OF IMPLEMENTATION
                                                                                                          corrections and updates to the existing               PLANS
                                                  A. Executive Order 12866: Regulatory                    procedures specified in Method 202.
                                                  Planning and Review and Executive                       Thus, Executive Order 13175 does not                  ■ 1. The authority citation for part 51
                                                  Order 13563: Improving Regulation and                                                                         continues to read as follows:
                                                                                                          apply to this action.
                                                  Regulatory Review
                                                                                                                                                                    Authority: 42 U.S.C. 7401, et seq.
                                                    This action is not a significant                      H. Executive Order 13045: Protection of
                                                  regulatory action and was, therefore, not               Children From Environmental Health                    Subpart BB—Data Requirements for
                                                  submitted to the Office of Management                   Risks and Safety Risks                                Characterizing Air Quality for the
                                                  and Budget (OMB) for review.                                                                                  Primary SO2 NAAQS
                                                                                                            The EPA interprets Executive Order
                                                  B. Executive Order 13771: Reducing                      13045 as applying only to those                       ■ 2. In appendix M to part 51—
                                                  Regulations and Controlling Regulatory                  regulatory actions that concern                       Recommended Test Methods for State
                                                  Costs                                                   environmental health or safety risks that             Implementation Plans, revise Method
                                                    This action is not expected to be an                  the EPA has reason to believe may                     202 to read as follows:
                                                  Executive Order 13771 regulatory action                 disproportionately affect children, per               Method 202—Dry Impinger Method for
                                                  because this action is not significant                  the definition of ‘‘covered regulatory                Determining Condensable Particulate
                                                  under Executive Order 12866.                            action’’ in section 2–202 of the                      Emissions From Stationary Sources
                                                                                                          Executive Order. This action is not
                                                  C. Paperwork Reduction Act (PRA)                        subject to Executive Order 13045                      1.0 Scope and Applicability
                                                    This action does not impose an                        because it does not concern an                          1.1 Scope. The U.S. Environmental
                                                  information collection burden under the                 environmental health risk or safety risk.             Protection Agency (U.S. EPA or ‘‘we’’)
                                                  PRA. The revisions being proposed in                                                                          developed this method to describe the
                                                  this action do not add information                      I. Executive Order 13211: Actions That                procedures that the stack tester (‘‘you’’)
                                                  collection requirements, but make                       Significantly Affect Energy Supply,                   must follow to measure condensable
                                                  corrections and updates to existing                     Distribution, or Use                                  particulate matter (CPM) emissions from
                                                  testing methodology.                                                                                          stationary sources. This method
                                                                                                            This action is not subject to Executive
                                                                                                                                                                includes procedures for measuring both
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                                                  D. Regulatory Flexibility Act (RFA)                     Order 13211, because it is not a
                                                                                                                                                                organic and inorganic CPM.
                                                     I certify that this action will not have             significant regulatory action under                     1.2 Applicability. This method
                                                  a significant economic impact on a                      Executive Order 12866.                                addresses the equipment, preparation,
                                                  substantial number of small entities                    J. National Technology Transfer and                   and analysis necessary to measure only
                                                  under the RFA. This action will not                     Advancement Act (NTTAA)                               CPM. You can use this method only for
                                                  impose any requirements on small                                                                              stationary source emission
                                                  entities. The proposed revisions to                       This rulemaking does not involve                    measurements. You can use this method
                                                  Method 202 neither impose any                           technical standards.                                  to measure CPM from stationary source


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                         42515

                                                  emissions after filterable particulate                  stationary sources (constant sampling                    2.1.1 Condensable PM. Condensable
                                                  matter (PM) has been removed.                           rate procedure).                                      PM is collected in the water dropout
                                                  Condensable PM is measured in the                         (h) In addition to Method 5, it is also             impinger, the modified Greenburg-
                                                  emissions after removal from the stack                  acceptable to use Method 5A, 5D or 5I                 Smith impinger, and the CPM filter of
                                                  and after passing through a filter.                     to collect filterable PM from stationary              the sampling train as described in this
                                                    (a) If you are required to measure total              sources.                                              method. The impinger contents are
                                                  primary (direct) PM2.5 and/or PM10, then                                                                      purged with nitrogen as soon as possible
                                                                                                            Note: You must maintain the gas filtration
                                                  you must combine the procedures in                      temperature of the filterable PM method as
                                                                                                                                                                after the post-test leak check to remove
                                                  this method with the procedures in                      specified in the method, unless otherwise             dissolved sulfur dioxide (SO2) gases
                                                  Method 201A of appendix M to this                       specified by an applicable subpart.                   from the impingers. The impinger
                                                  part. If you are required to measure both                                                                     solutions are collected and the
                                                  the filterable and condensable                             1.5 Limitations. You can use this                  glassware is rinsed with water, acetone,
                                                  components of total primary (direct) PM                 method to measure emissions in stacks                 and hexane. The CPM filter is extracted
                                                  emissions to the atmosphere, then you                   that have entrained droplets only when                with water and hexane; the extracted
                                                  may use Method 5 of appendix A–3 to                     this method is combined with a                        liquid is then combined with the hexane
                                                  part 60, or Method 17 of appendix                       filterable PM test method that operates               and water fractions from the impingers.
                                                  A–6 to part 60.                                         at high enough temperatures to cause                  The aqueous impinger solution is then
                                                                                                          water droplets sampled through the                    extracted with hexane. The organic and
                                                     Note: If Method 17 of appendix A–6 to part
                                                                                                          probe to become vaporous.                             aqueous fractions are evaporated to
                                                  60 is attempted in conjunction with Method
                                                  202 to measure total primary PM, and the                  Note: The EPA recommends that under                 dryness and the residues are weighed.
                                                  constant weight requirements for the                    these conditions or any other conditions,             The total of the aqueous and organic
                                                  filterable fractions cannot be met, it may be           when moisture collection is expected to be in         fractions represents the CPM.
                                                  necessary to conduct additional test runs               excess of 2 percent, the testing periods be              2.1.2 Dry Impinger and Additional
                                                  using an applicable filterable PM method that           limited to no greater than 2 hours.                   Filter. The potential artifacts from SO2
                                                  requires a heated filter temperature.                                                                         are reduced using a vertical condenser
                                                                                                            1.6 Conditions. You must maintain
                                                     (b) If the gas filtration temperature of             isokinetic sampling conditions to meet                and water dropout impinger to separate
                                                  the filterable PM method used does not                  the requirements of the filterable PM                 CPM from reactive gases. No water is
                                                  exceed 30 °C (85 °F), then use of this                  test method used in conjunction with                  added to the water dropout and backup
                                                  method is not necessary to measure                      this method. You must sample at the                   impingers prior to the start of sampling.
                                                  primary PM, as the CPM is collected as                  required number of sampling points                    To improve the collection efficiency of
                                                  filterable PM.                                          specified in the filterable PM test                   CPM, an additional filter (the ‘‘CPM
                                                                                                          method used in conjunction with this                  filter’’) is placed between the second
                                                    Note: For those methods that require in-
                                                  stack filtration (i.e., Method 17 and 201A),            method. Also, if you are using this                   and third impingers.
                                                  the measured stack temperature is considered            method as an alternative to a required                3.0 Definitions
                                                  the filtration temperature.                             performance test method, you must
                                                                                                                                                                   3.1 Condensable PM (CPM) means
                                                     1.3 Responsibility. You are                          receive approval from the regulatory
                                                                                                                                                                material that is vapor phase at stack
                                                  responsible for obtaining the equipment                 authority that established the
                                                                                                                                                                conditions, but condenses and/or reacts
                                                  and supplies you will need to use for                   requirement to use this test method
                                                                                                                                                                upon cooling and dilution in the
                                                  this method. You should also develop                    prior to conducting the test.
                                                                                                                                                                ambient air to form solid or liquid PM
                                                  your own procedures for following this                  2.0    Summary of Method                              immediately after discharge from the
                                                  method and any additional procedures                                                                          stack. Note that all condensable PM is
                                                  to ensure accurate sampling and                            2.1 Summary. The CPM is collected                  assumed to be in the PM2.5 size fraction.
                                                  analytical measurements.                                in dry impingers after filterable PM has                 3.2 Constant weight means a
                                                     1.4 Additional Methods. To obtain                    been collected on a filter maintained as              difference of no more than 0.5 mg or 1
                                                  reliable results, you should have a                     specified in either Method 5 of                       percent of total weight less tare weight,
                                                  thorough knowledge of the following                     appendix A–3 to part 60, Method 17 of                 whichever is greater, between two
                                                  test methods that are found in                          appendix A–6 to part 60, or Method                    consecutive weighings, with no less
                                                  appendices A–1 through A–3 and A–6                      201A of appendix M to this part. The                  than 6 hours of desiccation time
                                                  to part 60, and in appendix M to this                   organic and aqueous sample fractions                  between weighings.
                                                  part:                                                   from the impingers and an out-of-stack                   3.3 Field Train Proof Blank. A field
                                                     (a) Method 1—Sample and velocity                     CPM filter are then taken to dryness and              train proof blank for each source
                                                  traverses for stationary sources.                       weighed. The total mass collected from                category tested is recovered on-site from
                                                     (b) Method 2—Determination of stack                  the impinger fractions and the CPM                    a clean, fully-assembled sampling train.
                                                  gas velocity and volumetric flow rate                   filter represents the CPM. Compared to                   3.4 Filterable PM means particles
                                                  (Type S pitot tube).                                    the version of Method 202 that was                    that are emitted directly by a source as
                                                     (c) Method 3—Gas analysis for the                    promulgated on December 17, 1991, this                a solid or liquid at stack or release
                                                  determination of dry molecular weight.                  method eliminates the use of water as                 conditions and captured on the filter of
                                                     (d) Method 4—Determination of                        the collection media in impingers and                 a stack test train.
                                                  moisture content in stack gases.                        includes the addition of a condenser                     3.5 Primary PM (also known as
                                                     (e) Method 5—Determination of                        followed by a water dropout impinger                  direct PM) means particles that enter the
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                                                  particulate matter emissions from                       after the final in-stack or heated filter.            atmosphere as a direct emission from a
                                                  stationary sources.                                     This method also includes the addition                stack or an open source. Primary PM
                                                     (f) Method 17—Determination of                       of one modified Greenburg-Smith                       comprises two components: Filterable
                                                  particulate matter emissions from                       impinger (backup impinger) and a CPM                  PM and condensable PM. These two PM
                                                  stationary sources (in-stack filtration                 filter following the water dropout                    components have no upper particle size
                                                  method).                                                impinger. Figure 1 of section 18                      limit.
                                                     (g) Method 201A—Determination of                     presents the schematic of the sampling                   3.6 Primary PM2.5 (also known as
                                                  PM10 and PM2.5 emissions from                           train configured with these changes.                  direct PM2.5, total PM2.5, PM2.5, or


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                                                  42516                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                  combined filterable PM2.5 and                           Health Administration, and Department                 fluoropolymer O-ring. At the exit of the
                                                  condensable PM) means PM with an                        of Transportation regulatory                          CPM filter, install a fluoropolymer-
                                                  aerodynamic diameter less than or equal                 requirements. Because of the unique                   coated or stainless steel encased
                                                  to 2.5 micrometers. These solid particles               situations at some facilities and because             thermocouple that is in direct contact
                                                  are emitted directly from an air                        some facilities may have more stringent               with the gas stream.
                                                  emissions source or activity, or are the                requirements than is required by state or
                                                  gaseous emissions or liquid droplets                    federal laws, you may have to develop       6.2 Sample Recovery Equipment
                                                  from an air emissions source or activity                procedures to conform to the plant             6.2.1 Condensable PM Recovery. Use
                                                  that condense to form PM at ambient                     health and safety requirements.             the following equipment to
                                                  temperatures. Direct PM2.5 emissions                                                                quantitatively determine the amount of
                                                                                                          6.0 Equipment and Supplies                  CPM recovered from the sampling train.
                                                  include elemental carbon, directly
                                                  emitted organic carbon, directly emitted                   The equipment used in the filterable        (a) Nitrogen purge line. You must use
                                                  sulfate, directly emitted nitrate, and                  particulate portion of the sampling train inert tubing and fittings capable of
                                                  other inorganic particles (including but                is described in Methods 5 and 17 of         delivering at least 14 liters/min of
                                                  not limited to crustal material, metals                 appendix A–1 through A–3 and A–6 to         nitrogen gas to the impinger train from
                                                  and sea salt).                                          part 60 and Method 201A of appendix         a standard gas cylinder (see Figures 2
                                                     3.7 Primary PM10 (also known as                      M to this part. The equipment used in       and 3 of section 18). You may use
                                                  direct PM10, total PM10, PM10, or the                   the CPM portion of the train is             standard 0.6 centimeters (1⁄4 inch)
                                                  combination of filterable PM10 and                      described in this section.                  tubing and compression fittings in
                                                  condensable PM) means PM with an                           6.1 Condensable Particulate              conjunction with an adjustable pressure
                                                  aerodynamic diameter equal to or less                   Sampling Train Components. The              regulator and needle valve.
                                                  than 10 micrometers.                                    sampling train for this method is used         (b) Rotameter. You must use a
                                                     3.8 ASTM E617–13. ASTM E617–13                       in addition to filterable particulate       rotameter capable of measuring gas flow
                                                  ‘‘Standard Specification for Laboratory                 collection using Method 5 of appendix       up to 20 liters/min. The rotameter must
                                                  Weights and Precisions Mass                             A–3 to part 60, Method 17 of appendix       be accurate to five percent of full scale.
                                                  Standards,’’ approved May 1, 2013, was                  A–6 to part 60, or Method 201A of              (c) Nitrogen gas purging system.
                                                  developed and adopted by the American                   appendix M to this part. This method        Compressed ultra-pure nitrogen,
                                                  Society for Testing and Materials                       includes the following exceptions or        regulator, and filter must be capable of
                                                  (ASTM). The standards cover weights                     additions:                                  providing at least 14 liters/min purge
                                                  and mass standards used in laboratories                    6.1.1 Probe Extension and Liner. The gas for one hour through the sampling
                                                  for specific classes. The ASTM E617–13                  probe extension between the filterable      train.
                                                  standard has been approved for                          particulate filter and the condenser           (d) Sample bottles (500 ml). You must
                                                  incorporation by reference by the                       must be glass- or fluoropolymer-lined.      use amber glass bottles or other non-
                                                  Director of the Office of the Federal                   Follow the specifications for the probe     reactive bottles (e.g., High Density
                                                  Register in accordance with 5 U.S.C.                    liner specified in section 6.1.1.2 of       Linear Polyethylene (HDLPE), or PTFE)
                                                  552(a) and 1 CFR part 51. The standard                  Method 5 of appendix A–3 to part 60.        pre-cleaned sample bottles for inorganic
                                                  may be obtained from http://                               6.1.2 Condenser and Impingers. You samples. Amber glass bottles are
                                                  www.astm.org or from the ASTM at 100                    must add the following components to        required for organic samples and must
                                                  Barr Harbor Drive, P.O. Box C700, West                  the filterable particulate sampling train: be prepared according to section 8.4 of
                                                  Conshohocken, PA 19428–2959. All                        A vertical condenser, followed by a         this method.
                                                  approved material is available for                      water dropout impinger or flask,               6.2.2 Analysis Equipment. The
                                                  inspection at the EPA Docket Office,                    followed by a modified Greenburg-           following equipment is necessary for
                                                  EPA WJC West Building, Room 3334,                       Smith impinger (backup impinger) with CPM sample analysis:
                                                  1301 Constitution Avenue NW.,                           an open tube tip as described in section       (a) Separatory Funnel. Glass, 1 liter.
                                                  Washington, DC 20460, telephone                         6.1.1.8 of Method 5 of appendix A–3 to         (b) Weighing Containers.
                                                  number (202) 566–1744. It is also                       part 60.                                    Fluoropolymer beaker liners or other
                                                  available for inspection at the National                   6.1.3 Dropout Impinger Insert for        low-mass vessels which are unreactive
                                                  Archives and Records Administration                     Nitrogen Purge. You must use a leak-free to the sample or atmosphere.
                                                  (NARA). For information on the                          ground glass fitting with a long glass or      Note: The use of an anti-static device(s)
                                                  availability of this material at NARA,                  PTFE stem (e.g., modified Greenburg-        during gravimetric analysis to prevent static
                                                  call 202–741–6030 or go to http://                      Smith impinger insert or purge stem,        from interfering with the analysis is
                                                  www.archives.gov/federal_register/                      etc.) for the water dropout impinger to     recommended when using Fluoropolymer or
                                                  code_of_federal_regulattions/ibr_                       perform the nitrogen purge of the           similar beaker liners.
                                                  locations.html.                                         sampling train. The glass stem must be         (c) Glass Beakers. 300 to 500 ml.
                                                                                                          designed so that the tip of the stem is        (d) Drying Equipment. A desiccator
                                                  4.0 Interferences                                       1⁄2″ from the bottom of the impinger.
                                                                                                                                                      containing anhydrous calcium sulfate
                                                    [Reserved]                                               6.1.4 CPM Filter Holder. The             that is maintained below 10 percent
                                                                                                          modified Greenburg-Smith impinger is        relative humidity, and a hot plate or
                                                  5.0 Safety                                              followed by a filter holder that is either  oven equipped with temperature
                                                    Disclaimer. Because the performance                   glass, stainless steel (316 or equivalent), control.
                                                  of this method may require the use of                   or fluoropolymer-coated stainless steel.
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                                                                                                                                                         (e) Glass Pipets. 5 ml.
                                                  hazardous materials, operations, and                    Commercial size filter holders are             (f) Burette. Glass, 0 to 100 ml in 0.1
                                                  equipment, you should develop a health                  available depending on project              ml graduations.
                                                  and safety plan to ensure the safety of                 requirements. Use a commercial filter          (g) Analytical Balance. Analytical
                                                  your employees who are on site                          holder capable of supporting 47 mm or       balance capable of weighing at least
                                                  conducting the particulate emission test.               greater diameter filter. Commercial size    0.0001 g (0.1 mg).
                                                  Your plan should conform with all                       filter holders contain a fluoropolymer         (h) pH Meter. The pH meter must be
                                                  applicable Occupational Safety and                      O-ring, stainless steel, ceramic or         capable of determining the acidity of
                                                  Health Administration, Mine Safety and                  fluoropolymer filter support and a final    liquid within 0.1 pH units.


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                             42517

                                                     (i) Sonication Device. The device                    ammonia hydroxide, and deionized                         (a) Determining the sampling site
                                                  must have a minimum sonication                          water for the sample recovery and                     location and traverse points.
                                                  frequency of 20 kHz and be                              analysis. Unless otherwise indicated, all                (b) Calculating probe/cyclone
                                                  approximately four to six inches deep to                reagents must conform to the                          blockage (as appropriate).
                                                  accommodate the sample extractor tube.                  specifications established by the                        (c) Verifying the absence of cyclonic
                                                     (j) Leak-Proof Sample Containers.                    Committee on Analytical Reagents of                   flow.
                                                  Containers used for sample and blank                    the American Chemical Society. If such                   (d) Completing a preliminary velocity
                                                  recovery must not contribute more than                  specifications are not available, then use            profile, and selecting a nozzle(s) and
                                                  0.05 mg of residual mass to the CPM                     the best available grade. Additional                  sampling rate.
                                                  measurements.                                           information on each of these items is in                 8.3.1 Sampling Site Location.
                                                     (k) Wash bottles. Any container                      the following paragraphs:                             Follow the standard procedures in
                                                  material is acceptable, but wash bottles                   7.2.1 Acetone. Use acetone that is                 Method 1 of appendix A–1 to part 60 to
                                                  used for sample and blank recovery                      stored in a glass bottle. Do not use                  select the appropriate sampling site.
                                                  must not contribute more than 0.1 mg of                 acetone from a metal container because                Choose a location that maximizes the
                                                  residual mass to the CPM                                it normally produces a high residual                  distance from upstream and
                                                  measurements.                                           mass in the laboratory and field reagent              downstream flow disturbances.
                                                                                                                                                                   8.3.2 Traverse Points. Use the
                                                  7.0 Reagents and Standards                              blanks. You must use acetone that has
                                                                                                                                                                required number of traverse points at
                                                                                                          a blank value less than 1.0 ppmw (0.1
                                                     7.1 Sample Collection. To collect a                                                                        any location, as found in in the method
                                                                                                          mg/100 g) residue.
                                                  sample, you will need a CPM filter,                                                                           used to collect the filterable particulate.
                                                                                                             7.2.2 Hexane, American Chemical                    You must prevent the disturbance and
                                                  crushed ice, and silica gel. You must                   Society Grade or Equivalent. You must
                                                  also have water and nitrogen gas to                                                                           capture of any solids accumulated on
                                                                                                          use hexane that has a blank residual                  the inner wall surfaces by maintaining
                                                  purge the sampling train. You will find                 mass value less than 1.0 ppmw (0.1 mg/
                                                  additional information on each of these                                                                       a 1 inch distance from the stack wall
                                                                                                          100 g) residue.                                       (0.5 inch for sampling locations less
                                                  items in the following summaries.
                                                                                                             7.2.3 Water. Use deionized, ultra-                 than 24 inches in diameter).
                                                     7.1.1 CPM Filter. You must use a
                                                                                                          filtered water that contains 1.0 ppmw                    8.4 Sampling Train Preparation. A
                                                  nonreactive, non-disintegrating polymer
                                                                                                          (1.0 mg/L) residual mass or less to                   schematic of the sampling train used in
                                                  filter that does not have an organic
                                                                                                          recover material caught in the impinger.              this method is shown in Figure 1 of
                                                  binder and does not contribute more
                                                  than 0.5 mg of residual mass to the CPM                    7.2.4 Condensable Particulate                      section 18. All glassware that is used to
                                                  measurements. The CPM filter must also                  Sample Desiccant. Use indicating-type                 collect and analyze samples should be
                                                  have an efficiency of at least 99.95                    anhydrous calcium sulfate to desiccate                cleaned sufficiently to meet the
                                                  percent (less than 0.05 percent                         water and organic extract residue                     maximum field train proof blank
                                                  penetration) on 0.3 micrometer dioctyl                  samples prior to weighing.                            contribution to be subtracted from the
                                                  phthalate particles. You may use test                      7.2.5 Ammonium Hydroxide. Use                      test results in section 9.9 (0.002g or 2.0
                                                  data from the supplier’s quality control                National Institute of Standards and                   mg). Cleaning glassware prior to the test
                                                  program to document the CPM filter                      Technology (NIST)-traceable or                        with soap and water, then rinsing with
                                                  efficiency.                                             equivalent (0.1 N) ammonium                           tap water, followed by deionized water,
                                                     7.1.2 Silica Gel. Use an indicating-                 hydroxide (NH4OH).                                    acetone, and finally, hexane is
                                                  type silica gel of 6 to 16 mesh. You must                  7.2.6 Standard Buffer Solutions. Use               recommended. After cleaning, you
                                                  obtain approval of the Administrator for                one buffer solution with a neutral pH                 should bake glassware at 300 °C for 6
                                                  other types of desiccants (equivalent or                and a second buffer solution with an                  hours prior to beginning tests at each
                                                  better) before you use them. Allow the                  acid pH of no less than 4.                            source category sampled at a facility.
                                                  silica gel to dry for 2 hours at 175 °C                 8.0 Sample Collection, Preservation,                  Prior to each sampling run, the train
                                                  (350 °F) if it is being reused. You do not              Storage, and Transport                                glassware used to collect condensable
                                                  have to dry new silica gel if the                                                                             PM must be rinsed thoroughly with
                                                  indicator shows the silica gel is active                  8.1 Qualifications. This is a complex               acetone, hexane, and then deionized,
                                                  for moisture collection.                                test method. To obtain reliable results,              ultra-filtered water that contains 1
                                                     7.1.3 Water. Use deionized, ultra-                   you should be trained and experienced                 ppmw (1 mg/L) residual mass or less.
                                                  filtered water that contains 1.0 parts per              with in-stack filtration systems (such as,
                                                                                                                                                                  Note: Due the length of most probes, it is
                                                  million by weight (ppmw) (1 mg/L)                       cyclones, impactors, and thimbles) and
                                                                                                                                                                not practical to heat them in an oven. After
                                                  residual mass or less to recover and                    impinger and moisture train systems.                  cleaning the probe liners, it is recommended
                                                  extract samples.                                          8.2 Preparations. Clean all glassware               to heat the probe to the maximum
                                                     7.1.4 Crushed Ice. Obtain from the                   used to collect and analyze samples                   temperature practical for the probe sheath for
                                                  best readily available source.                          prior to field tests as described in                  a period of at least 3 hours. Then rinse
                                                     7.1.5 Nitrogen Gas. Use Ultra-High                   Section 8.4 prior to use. Cleaned                     thoroughly with acetone, hexane, and
                                                  Purity compressed nitrogen or                           glassware must be used at the start of                deionized, ultra-filtered water.
                                                  equivalent to purge the sampling train.                 each new source category tested at a                    8.4.1 Condenser and Water Dropout
                                                  The compressed nitrogen you use to                      single facility. You must analyze                     Impinger. Add a vertical condenser and
                                                  purge the sampling train must contain                   laboratory reagent blanks (water,                     a water dropout impinger without
                                                  no more than 1 parts per million by                     acetone, and hexane) before field tests to            bubbler tube after the final probe
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                  volume (ppmv) oxygen, 1 ppmv total                      verify low blank concentrations for the               extension that connects the in-stack or
                                                  hydrocarbons as carbon, and 2 ppmv                      reagent lot(s) used. Follow the pretest               out-of-stack hot filter assembly with the
                                                  moisture. The compressed nitrogen                       preparation instructions in Section 8.1               CPM sampling train. This vertical
                                                  must not contribute more than 0.1 mg of                 of Method 5.                                          condenser must be constructed in a
                                                  residual mass per purge.                                  8.3 Site Setup. You must follow the                 manner that prevents the pooling of the
                                                     7.2 Sample Recovery and Analytical                   procedures required in Methods 5, 17,                 condensate liquid within the condenser
                                                  Reagents. You will need acetone,                        or 201A, whichever is applicable to                   and be capable of cooling the stack gas
                                                  hexane, anhydrous calcium sulfate,                      your test requirements including:                     to less than or equal to 30 °C (85 °F).


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                                                  42518                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                  At the start of the tests, the condenser                assembly. Follow the procedures                       may choose to weigh each impinger
                                                  and water dropout impingers must be                     outlined in section 8.4.1 of Method 5.                after completion of the post-test
                                                  clean, without any water or reagent                        8.5 Sampling Train Operation.                      nitrogen purge. If this option is chosen,
                                                  added.                                                  Operate the sampling train as described               you must do the following in addition
                                                     8.4.2 Backup Impinger. The water                     in the filterable particulate sampling                to the procedures of section 8.5.4. Purge
                                                  dropout impinger is followed by a                       method (i.e., Method 5 of appendix A–                 the sampling train from the water
                                                  modified Greenburg-Smith impinger                       3 to part 60, Method 17 of appendix A–                dropout impinger to the exhaust of the
                                                  (backup impinger) with no taper (see                    6 to part 60, or Method 201A of                       moisture traps (see Figure 2). You must
                                                  Figure 1 of section 18). Place the water                appendix M to this part) with the                     maintain the temperature of the
                                                  dropout and backup impingers in an                      following additions or exceptions:                    moisture traps following the CPM filter
                                                  insulated box with water at less than or                8.5.1 Impinger and CPM Filter                         to prevent removal of moisture during
                                                  equal to 30 °C (less than or equal to 85                Assembly                                              the purge. If necessary, add more ice
                                                  °F). At the start of the tests, the backup                                                                    during the purge to maintain the gas
                                                  impinger must be free of any residual                      8.5.1.1 During sampling, monitor the               temperature measured at the exit of the
                                                  solvents from the recovery or glassware                 moisture condensation in the water                    silica gel impinger below 20 °C (68 °F).
                                                  preparation.                                            dropout impinger and backup impinger.
                                                                                                          If the accumulated water from moisture                  Note: You should also note the color of the
                                                     8.4.3 CPM Filter. Place a filter holder                                                                    indicating silica gel to determine whether it
                                                                                                          condensation overwhelms (i.e., the
                                                  with a filter meeting the requirements in                                                                     has been completely spent, and record its
                                                                                                          water level is more than approximately
                                                  section 7.1.1 after the backup impinger.                                                                      condition on the CPM Impinger Data Sheet.
                                                                                                          one-half the capacity of the water
                                                  The connection between the CPM filter                                                                            8.5.4 Post-Test Nitrogen Purge. As
                                                                                                          dropout impinger) the water dropout
                                                  and the moisture trap impinger must                                                                           soon as possible after the post-test leak-
                                                                                                          impinger, or if water accumulates in the
                                                  include a thermocouple fitting that                                                                           check, conduct the nitrogen purge. If no
                                                                                                          backup impinger sufficient to cover the
                                                  provides a leak-free seal between the                                                                         water was collected before the CPM
                                                                                                          impinger insert tip, then you must
                                                  thermocouple and the stack gas.                                                                               filter, then you may skip the remaining
                                                                                                          interrupt the sampling run, leak check
                                                     8.4.4 Moisture Traps. You must use                   the Method 202 portion of the sampling                purge steps and proceed with sample
                                                  a modified Greenburg-Smith impinger                     train, replace the water dropout and/or               recovery (see section 8.5.5). If any water
                                                  containing 100 ml of water, or the                      backup impingers with new pre-                        was collected before the CPM filter, you
                                                  alternative described in Method 5 of                    weighed impinger(s), reassemble, leak                 must purge the CPM sampling train.
                                                  appendix A–3 to part 60, followed by an                 check the sampling train, and then                       8.5.4.1 You may purge the entire
                                                  impinger containing 200 to 300 g of                     resume the sampling run. Weigh the                    CPM sample collection train from the
                                                  indicating-type silica gel to collect                   impingers removed from the sampling                   water dropout impinger through the
                                                  moisture that passes through the CPM                    train and purge the water collected as                CPM filter holder outlet or you may
                                                  filter. You must maintain the gas                       soon as practical following the                       quantitatively transfer the water
                                                  temperature below 20 °C (68 °F) at the                  procedures in section 8.5.3.                          collected in the water dropout impinger
                                                  exit of the moisture traps.                                8.5.1.2 You must include the weight                to the backup impinger and purge only
                                                     8.4.5 Weighing of Impingers                          of the moisture in your moisture                      the backup impinger and the CPM filter
                                                  (Pretest). Weigh each impinger to 0.1 g,                calculation and you must combine the                  and holder (see Figure 3).
                                                  including the silica gel impinger prior to              recovered water with the appropriate                     8.5.4.2 If you choose to conduct a
                                                  train assembly using the field balance.                 sample fraction for subsequent CPM                    purge of the entire CPM sampling train,
                                                  Record the weights of each impinger on                  analysis.                                             you must place the dropout impinger
                                                  the CPM Impinger Data Sheet (Figure 4).                    8.5.1.3 Use the field data sheet to                insert into the water dropout impinger,
                                                     8.4.6 Leak-Check (Pretest). Use the                  record the CPM filter temperature                     and the impinger tip must extend at
                                                  procedures outlined in Method 5 of                      readings at the beginning of each sample              least 1 centimeter below the water level
                                                  appendix A–3 to part 60, Method 17 of                   time increment and when sampling is                   of the impinger catch.
                                                  appendix A–6 to part 60, or Method                      halted. Maintain the CPM filter greater                  8.5.4.3 If the tip of the impinger
                                                  201A of appendix M to this part as                      than 20 °C (greater than 65 °F) but less              insert does not extend below the water
                                                  appropriate to leak check the entire                    than or equal to 30 °C (less than or equal            level (including the water transferred
                                                  sampling system. Specifically, perform                  to 85 °F) during sample collection.                   from the water dropout impinger if this
                                                  the following procedures:                                  8.5.2 Leak-Check (Post-Test).                      option was chosen), you must add a
                                                     8.4.6.1 Sampling train. You must                     Conduct the leak rate check according to              measured amount of degassed,
                                                  pretest the entire sampling train for                   the filterable particulate sampling                   deionized ultra-filtered water that
                                                  leaks. The pretest leak-check must have                 method used during sampling. Conduct                  contains 1 ppmw (1 mg/L) residual mass
                                                  a leak rate of not more than 0.02 actual                the leak-check at a vacuum equal to or                or less until the impinger tip is at least
                                                  cubic feet per minute or 4 percent of the               greater than the maximum vacuum                       1 centimeter below the surface of the
                                                  average sample flow during the test run,                achieved during the test run. Record the              water. You must record the amount of
                                                  whichever is less. Additionally, you                    leak-check results on the field test data             water added to the water dropout
                                                  must conduct the leak-check at a                        sheet. If the leak rate of the sampling               impinger (Vp) (see Figure 4 of section
                                                  vacuum equal to or greater than the                     train exceeds 0.02 actual cubic feet per              18) to correct the moisture content of
                                                  vacuum anticipated during the test run.                 minute or 4 percent of the average                    the effluent gas. (Note: Prior to use,
                                                  Record the leak-check results on the                    sampling rate during the test run                     water must be degassed using a nitrogen
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                  field test data sheet (see Figure 5). (Note:            (whichever is less), then the run is                  purge bubbled through the water for at
                                                  Conduct leak-checks during port                         invalid and you must repeat it.                       least 15 minutes to remove dissolved
                                                  changes only as allowed by the filterable                  8.5.3 Weighing of Impingers (Post-                 oxygen.)
                                                  particulate method used with this                       test). You must weigh each impinger to                   8.5.4.4 To perform the nitrogen
                                                  method.)                                                0.1 g after the completion of the testing             purge, you must start with no flow of
                                                     8.4.6.2 Pitot tube assembly. After                   and prior to the post-test nitrogen purge             gas running through the clean purge line
                                                  you leak-check the sample train,                        and record these weights on the CPM                   and fittings. Connect the purge nitrogen
                                                  perform a leak-check of the pitot tube                  Impinger data sheet. Alternatively, you               in-line filter outlet to the input of the


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                          42519

                                                  impinger train to be purged. Increase the               disposable surgical gloves to remove the              as described in sections 8.5.5.8.1
                                                  nitrogen flow gradually to avoid over-                  filter from the CPM filter holder. Place              through 8.5.5.8.3.
                                                  pressurizing the impinger array. You                    the filter in the Petri dish labeled with                8.5.5.8.1 CPM Container #7, Field
                                                  must purge the CPM train at a minimum                   test identification and ‘‘CPM Container               train proof blank, inorganic rinses.
                                                  of 14 liters per minute. Record the time                #3, Filter Sample.’’                                  Rinse the probe extension, condenser,
                                                  (hh:mm), nitrogen flowrate, and the                        8.5.5.5 CPM Container #4, Acetone                  each impinger and the connecting
                                                  temperature(s) of the CPM filter and                    field reagent blank. Take a minimum of                glassware, and the front half of the CPM
                                                  moisture trap (if applicable) at the start              200 ml of the acetone directly from the               filter housing twice with water. Recover
                                                  of the nitrogen purge on the CPM                        wash bottle you used for sample                       the rinse water and place it in a clean,
                                                  Impinger Data Sheet.                                    recovery and place it in a clean, leak-               leak-proof container labeled with test
                                                     8.5.4.5 During the purge procedure,                  proof amber glass container labeled with              identification and ‘‘CPM Container #7,
                                                  maintain the gas temperature measured                   test identification and ‘‘CPM Container               Field Train Proof Blank, Inorganic
                                                  at the exit of the CPM filter greater than              #4, Acetone Field Reagent Blank’’ (see                Rinses.’’ Mark the liquid level on the
                                                  20 °C (65 °F), but less than or equal to                section 11.2.6 for analysis). Mark the                container.
                                                  30 °C (85 °F). Continue the purge under                 liquid level on the container. Collect                   8.5.5.8.2 CPM Container #8, Field
                                                  these conditions for at least 1 hour,                   one acetone field reagent blank from                  train proof blank, organic rinses. Follow
                                                  recording the CPM temperature and                       each lot of acetone used for the test.                the water rinse of the probe extension,
                                                  nitrogen rotameter value every 10                          8.5.5.6 CPM Container #5, Water                    condenser, each impinger and the
                                                  minutes. At the conclusion of the purge,                field reagent blank. Take a minimum of                connecting glassware, and the front half
                                                  turn off the nitrogen delivery system.                  200 ml of the water directly from the                 of the CPM filter housing with an
                                                  Record the time (hh:mm) of the purge                    wash bottle you used for sample                       acetone rinse. Recover the acetone rinse
                                                  and the temperature of the CPM filter at                recovery and place it in a clean, leak-               into a clean, leak-proof container
                                                  the start of the nitrogen purge on the                  proof container labeled with test                     labeled with test identification and
                                                  CPM Impinger Data Sheet.                                identification and ‘‘CPM Container #5,                ‘‘CPM Container #8, Field Train Proof
                                                                                                          Water Field Reagent Blank’’ (see section              Blank, Organic Rinses.’’ Then repeat the
                                                  8.5.5 Sample Recovery                                   11.2.7 for analysis). Mark the liquid                 entire rinse procedure with two rinses
                                                     8.5.5.1 Filterable PM samples.                       level on the container. Collect one water             of hexane and recover the hexane rinses
                                                  Recovery of the filterable PM samples                   field reagent blank from each lot of                  into the same container as the acetone
                                                  involves the quantitative transfer of PM                water used for the test.                              rinse (CPM Container #10). Mark the
                                                  according to the filterable particulate                    8.5.5.7 CPM Container #6, Hexane                   liquid level on the container.
                                                  sampling method used (i.e., Method 5 of                 field reagent blank. Take a minimum of                   8.5.5.8.3 CPM Container #9, Field
                                                  appendix A–3 to part 60, Method 17 of                   200 ml of the hexane directly from the                train proof blank, filter sample. Use
                                                  appendix A–6 to part 60, or Method                      wash bottle you used for sample                       tweezers and/or clean disposable
                                                  201A of appendix M to this part).                       recovery and place it in a clean, leak-               surgical gloves to remove the filter from
                                                     8.5.5.2 CPM Container #1, Aqueous                    proof amber glass container labeled with              the CPM filter holder. Place the filter in
                                                  liquid impinger contents. Quantitatively                test identification and ‘‘CPM Container               the Petri dish labeled with test
                                                  transfer liquid from the dropout and the                #6, Hexane Field Reagent Blank’’ (see                 identification and ‘‘CPM Container #9,
                                                  backup impingers prior to the CPM filter                section 11.2.8 for analysis). Mark the                Field Train Proof Blank, Filter Sample.’’
                                                  into a clean, leak-proof container                      liquid level on the container. Collect                   8.5.6 Sample Transport procedures.
                                                  labeled with test identification and                    one hexane field reagent blank from                   Containers must remain in an upright
                                                  ‘‘CPM Container #1, Aqueous Liquid                      each lot of hexane used for the test.                 position at all times during shipping.
                                                  Impinger Contents.’’ Rinse all sampling                    8.5.5.8 Field train proof blank. To                You do not have to ship the containers
                                                  train components including the back                     demonstrate the cleanliness of sampling               under dry or blue ice. However, samples
                                                  half of the filterable PM filter holder, the            train glassware, you must prepare a full              should be maintained at or below 30 °C
                                                  probe extension (if applicable),                        sampling train to serve as a field train              (85 °F) during shipping.
                                                  condenser, each impinger and the                        proof blank just as it would be prepared
                                                  connecting glassware, and the front half                for sampling, including the filterable                9.0 Quality Control
                                                  of the CPM filter housing twice with                    PM method front half, probe extension                    9.1 Daily Quality Checks. You must
                                                  water. Recover the rinse water, and add                 (if applicable), condenser, impingers,                perform daily quality checks of field log
                                                  it to CPM Container #1. Mark the liquid                 CPM filter, and transfer line. Transport              notebooks and data entries and
                                                  level on the container.                                 and assemble the field train proof blank              calculations using data quality
                                                     8.5.5.3 CPM Container #2, Organic                    sample train to the sampling location                 indicators from this method and your
                                                  rinses. Follow the water rinses of the                  and perform a pre-test leak check as if               site-specific test plan. You must review
                                                  back half of the filterable PM filter                   it were an actual sample train. Hold this             and evaluate recorded and transferred
                                                  holder, probe extension (if applicable),                train at the sampling location for the                raw data, calculations, and
                                                  condenser, each impinger, and all of the                same amount of time as a test run unless              documentation of testing procedures.
                                                  connecting glassware and front half of                  otherwise specified by the                            You must initial or sign log notebook
                                                  the CPM filter with an acetone rinse.                   Administrator, and perform a post-test                pages and data entry forms that were
                                                  Recover the acetone rinse into a clean,                 leak check on this train at the end of the            reviewed.
                                                  leak-proof amber glass container labeled                actual test sampling time. After the post-               9.2 Calculation Verification. Verify
                                                  with test identification and ‘‘CPM                      test leak check, you must conduct a                   the calculations by independent,
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                  Container #2, Organic Rinses.’’ Then                    nitrogen purge of the field train proof               manual checks. You must flag any
                                                  repeat the entire rinse procedure with                  blank sample as specified in section                  suspect data and identify the nature of
                                                  two rinses of hexane, and save the                      8.5.4. For the nitrogen purge, you must               the problem and potential effect on data
                                                  hexane rinses in the same container as                  add 100 ml of deionized ultra-filtered                quality. After you complete the test,
                                                  the acetone rinse (CPM Container #2).                   water and replicate the nitrogen purge                prepare a data summary and compile all
                                                  Mark the liquid level on the container.                 procedures that you will use for the test             the calculations and raw data sheets.
                                                     8.5.5.4 CPM Container #3, CPM                        runs. After conducting the nitrogen                      9.3 Conditions. You must document
                                                  filter sample. Use tweezers and/or clean                purge, recover the field train proof blank            data and information on the process


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                                                  42520                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                  unit tested, the particulate control                    8.5.5.8. From each field sample weight,               gravimetric measurements by weighing
                                                  system used to control emissions, any                   you will subtract the condensable                     at least one ASTM E617–13 Class 2
                                                  non-particulate control system that may                 particulate mass you determine with                   tolerance (or better) calibration weight
                                                  affect particulate emissions, the                       this field train proof blank or 0.002 g               that corresponds to 50 to 150 percent of
                                                  sampling train conditions, and weather                  (2.0 mg), whichever is less, unless                   the weight of one filter or between 1 g
                                                  conditions. Discontinue the test if the                 otherwise specified by the regulatory                 and 5 g and record the results. If the
                                                  operating conditions may cause non-                     authority.                                            scale cannot reproduce the value of the
                                                  representative particulate emissions.                   10.0 Calibration and Standardization                  calibration weight to within 0.5 mg of
                                                     9.4 Field Balance Calibration                                                                              the certified mass, perform corrective
                                                  Check. Record the results of the                           Maintain a field log notebook of all               measures and conduct the multipoint
                                                  calibration check procedures on field                   condensable particulate sampling and                  calibration before use.
                                                  balances each day that they are used as                 analysis calibrations. Include copies of
                                                  required in section 10.3.                               the relevant portions of the calibration              11.0     Analytical Procedures
                                                     9.5 Glassware. Use class A                           and field logs in the final test report.              11.1     Analytical Data Sheets
                                                  volumetric glassware for titrations, or                    10.1 Thermocouple Calibration.
                                                                                                          You must calibrate the thermocouples                     (a) Record the filterable particulate
                                                  calibrate your equipment against NIST-
                                                                                                          using the procedures described in                     field data on the appropriate (i.e.,
                                                  traceable glassware.
                                                                                                          section 10.3.1 of Method 2 of appendix                Method 5, 17, or 201A) analytical data
                                                  9.6 Laboratory Analytical Balance                       A–1 to part 60 or Alternative Method 2,               sheets. Record the condensable
                                                     9.6.1 Maintain the location of the                   Thermocouple Calibration (ALT–011)                    particulate data on the CPM Work Table
                                                  analytical balance (i.e., weighing room)                (https://www.epa.gov/emc). Calibrate                  (see Figure 7 of section 18).
                                                  at 20 °C ± 3 °C (68 °F ± 5 °F).                         each temperature sensor at a minimum                     (b) Visually inspect the liquid level
                                                     9.6.2 Maintain the location the                      of three points over the anticipated                  mark on each sample container and
                                                  analytical balance (i.e., weighing room)                range of use against a NIST-traceable                 record on the CPM Work Table whether
                                                  at 35 to 50 percent relative humidity.                  thermometer. Alternatively, a reference               leakage occurred during transport. If a
                                                  Alternatively, it is acceptable for the                 thermocouple and potentiometer                        noticeable amount of leakage has
                                                  percent relative humidity to be less than               calibrated against NIST standards can be              occurred, either void the sample or use
                                                  35 percent. In either case, you should                  used.                                                 methods, subject to the approval of the
                                                  maintain the relative humidity within                      10.2 Ammonium Hydroxide. The                       Administrator, to correct the final
                                                  ±10 percent relative humidity for                       0.1 N NH4OH used for titrations in this               results.
                                                  sampling weighings.                                     method is made as follows: Add 7 ml of                   11.2 Condensable PM Analysis. See
                                                     9.6.3 Record and report the                          concentrated (14.8 M) NH4OH to 1 liter                the flow chart in Figure 8 of section 18
                                                  temperature and relative humidity of                    of water. Standardize against certified               for the steps to process and combine
                                                  the analytical balance location for each                standard of 0.1 N H2SO4, and calculate                fractions from the CPM train.
                                                  measurement performed.                                  the exact normality using a procedure                    11.2.1 Container #3, CPM Filter
                                                     9.6.4 Calibration Check. Record the                  parallel to that described in section 10.5            Sample. Extract the CPM filter as
                                                  calibration check of your laboratory                    of Method 6 of appendix A–4 to 40 CFR                 described in this section.
                                                  analytical balance at least once each day               part 60. Alternatively, purchase 0.1 N                   11.2.1.1 Extract the water soluble
                                                  that you weigh CPM samples. Audit the                   NH4OH that has been standardized                      (aqueous or inorganic) CPM from the
                                                  balance using at least one ASTM E617–                   against a NIST reference material.                    CPM filter by placing it into a clean
                                                  13 Class 2 tolerance (or better)                        Record the normality on the CPM Work                  extraction container or flask. Add
                                                  calibration weight, within 1 g to 5 g of                Table (see Figure 6 of section 18).                   sufficient deionized, ultra-filtered water
                                                  the weight of the sample plus container                    10.3 Field Balance Calibration                     to cover the filter (e.g., 10 ml of water).
                                                  you will be weighing.                                   Check. Check the calibration of the                   Place the extractor container into a
                                                     9.7 Laboratory Reagent Blanks. You                   balance used to weigh impingers with a                sonication bath and extract the water-
                                                  should analyze blanks of water, acetone,                weight that is at least 500 g or within               soluble material for a minimum of 2
                                                  and hexane used for field recovery and                  50 g of a loaded impinger. The weight                 minutes. Combine the aqueous extract
                                                  sample analysis. Analyze and report at                  must be ASTM E617–13 ‘‘Standard                       with the contents of Container #1.
                                                  least one sample (500 ml minimum) of                    Specification for Laboratory Weights                  Repeat this extraction step twice for a
                                                  each lot of reagents that you plan to use               and Precision Mass Standards’’ Class 6                total of three extractions.
                                                  for sample recovery and analysis. These                 (or better). Daily, before use, the field                11.2.1.2 Extract the organic soluble
                                                  blanks are not required by the test                     balance must measure the weight within                CPM from the CPM filter by adding
                                                  method, but analyzing reagent blanks                    ± 0.5 g of the certified mass and record              sufficient hexane to cover the filter (e.g.,
                                                  before field use is recommended to                      the results. If the balance calibration               10 ml of hexane). Place the extractor
                                                  verify low reagent blank concentrations.                check fails, perform corrective measures              tube into a sonication bath and extract
                                                     9.8 Field Reagent Blanks. You must                   and repeat the check before using                     the organic soluble material for a
                                                  analyze and report the results of each lot              balance.                                              minimum of two minutes. Combine the
                                                  of reagent used for the field test.                        10.4 Analytical Balance                            organic extract with the contents of
                                                     9.9 Field Train Proof Blank. You                     Calibration. Perform a multipoint                     Container #2. Repeat this extraction step
                                                  must recover a minimum of one field                     calibration (at least five points spanning            twice for a total of three extractions.
                                                  train proof blank for each new source                   the operational range) of the analytical                 11.2.2 CPM Container #1, Aqueous
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                  category at a single facility using                     balance before the first use, and                     Liquid Impinger Contents. Analyze the
                                                  glassware prepped according to section                  semiannually thereafter. The calibration              water-soluble CPM in Container #1 as
                                                  8.4. You must assemble the sampling                     of the analytical balance must be                     described in this section. Place the
                                                  train as it will be used for testing,                   conducted using ASTM E617–13                          contents of Container #1 into a
                                                  including the filterable PM method front                ‘‘Standard Specification for Laboratory               separatory funnel. Add approximately
                                                  half, CPM filter, and transfer line. You                Weights and Precision Mass Standards’’                30 ml of hexane to the funnel, mix well,
                                                  must prepare and recover the field train                Class 2 (or better) tolerance weights.                and pour off the upper organic phase.
                                                  proof blank as described in section                     Audit the balance each day it is used for             Repeat this procedure twice with 30 ml


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                             42521

                                                  of hexane each time combining the                          11.2.3 CPM Container #2, Organic                   to a clean 250 ml beaker. Evaporate the
                                                  organic phase from each extraction.                     Fraction Weight Determination. Analyze                hexane at room temperature (not to
                                                  Each time, leave a small amount of the                  the organic soluble CPM in Container #2               exceed 30 °C (85 °F)) and pressure in a
                                                  organic/hexane phase in the separatory                  as described in this section. Place the               laboratory hood to approximately 10 ml.
                                                  funnel, ensuring that no water is                       organic phase in a clean glass beaker.                Quantitatively transfer the beaker
                                                  collected in the organic phase. This                    Evaporate the organic extract at room                 contents to a clean 50 ml pre-tared
                                                  extraction should yield about 90 ml of                  temperature (not to exceed 30 °C (85 °F))             weighing container and evaporate to
                                                  organic extract. Combine the organic                    and pressure in a laboratory hood to not              dryness at room temperature (not to
                                                  extract from Container #1 with the                      less than 10 ml. Quantitatively transfer              exceed 30 °C (85 °F)) and pressure in a
                                                  organic train rinse in Container #2.                    the beaker contents to a clean 50 ml pre-             laboratory hood. Following evaporation,
                                                     11.2.2.1 Determine the inorganic                     tared weighing container and evaporate                desiccate the residue for 24 hours in a
                                                  fraction weight. Transfer the aqueous                   to dryness at room temperature (not to                desiccator containing anhydrous
                                                  fraction from the extraction to a clean                 exceed 30 °C (85 °F)) and pressure in a               calcium sulfate. Weigh at intervals of at
                                                  500 ml or smaller beaker. Evaporate to                  laboratory hood. Following evaporation,               least 6 hours to a constant weight (i.e.,
                                                  no less than 10 ml liquid on a hot plate                desiccate the organic fraction for 24                 less than or equal to 0.5 mg change from
                                                  or in the oven at 105 °C and allow to                   hours in a desiccator containing                      previous weighing), and report results to
                                                  dry at room temperature (not to exceed                  anhydrous calcium sulfate. Weigh at                   the nearest 0.1 mg on Figure 5 of section
                                                  30 °C (85 °F)). Following evaporation,                  intervals of at least 6 hours to a constant           18.
                                                  desiccate the residue for 24 hours in a                 weight (i.e., less than or equal to 0.5 mg
                                                                                                          change from previous weighing), and                   12.0     Calculations and Data Analysis
                                                  desiccator containing anhydrous
                                                  calcium sulfate. Weigh at intervals of at               report results to the nearest 0.1 mg on                 12.1 Nomenclature. Report results in
                                                  least 6 hours to a constant weight. (See                the CPM Work Table (see Figure 6 of                   International System of Units (SI units)
                                                  section 3.0 for a definition of constant                section 18).                                          unless the regulatory authority for
                                                  weight.) Report results to the nearest 0.1                 11.2.4 Container #4, Acetone Field                 testing specifies English units. The
                                                  mg on the CPM Work Table (see Figure                    Reagent Blank. Use 200 ml of acetone                  following nomenclature is used.
                                                  6 of section 18) and proceed directly to                from the blank container used for this
                                                                                                                                                                DH@ = Pressure drop across orifice at flow
                                                  section 11.2.3. If the residue cannot be                analysis. Transfer 200 ml of the acetone
                                                                                                                                                                     rate of 0.75 SCFM at standard
                                                  weighed to constant weight, re-dissolve                 field reagent blank to a clean 250 ml                      conditions, inches of water column (Note
                                                  the residue in 100 ml of deionized                      beaker. Evaporate the acetone at room                      Specific to each orifice and meter box).
                                                  distilled ultra-filtered water that                     temperature (not to exceed 30 °C (85 °F))             17.03 = mg/milliequivalents for ammonium
                                                  contains 1 ppmw (1 mg/L) residual mass                  and pressure in a laboratory hood to                       ion.
                                                  or less and continue to section 11.2.2.2.               approximately 10 ml. Quantitatively                   ACFM = Actual cubic feet per minute.
                                                                                                          transfer the beaker contents to a clean               Ccpm = Concentration of the condensable PM
                                                     11.2.2.2 You must ensure that water                                                                             in the stack gas, dry basis, corrected to
                                                                                                          pre-tared weighing container, and
                                                  and volatile acids have completely                                                                                 standard conditions, milligrams/dry
                                                                                                          evaporate to dryness at room
                                                  evaporated before neutralizing                                                                                     standard cubic foot.
                                                                                                          temperature (not to exceed 30 °C (85 °F))
                                                  nonvolatile acids in the sample. Only                                                                         mc = Mass of the NH4+ added to sample to
                                                                                                          and pressure in a laboratory hood.
                                                  after failure to reach constant weight                                                                             form ammonium sulfate, mg.
                                                                                                          Following evaporation, desiccate the                  mcpm = Mass of the total condensable PM, mg.
                                                  and rehydration, per section 11.2.2.1,
                                                                                                          residue for 24 hours in a desiccator                  mfb = Mass of total CPM in field train proof
                                                  use titration to neutralize acid in the                 containing anhydrous calcium sulfate.
                                                  sample and remove water of hydration.                                                                              blank, mg.
                                                                                                          Weigh at intervals of at least 6 hours to             mg = Milligrams.
                                                  Calibrate the pH meter with the neutral                 a constant weight (i.e., less than or equal           mg/dscf = Milligrams per dry standard cubic
                                                  and acid buffer solutions immediately                   to 0.5 mg change from previous                             foot.
                                                  prior to the titration of the samples.                  weighing), and report results to the                  mg/L = Milligrams per liter.
                                                  Then titrate the sample with 0.1 N                      nearest 0.1 mg on Figure 5 of section 19.             mi = Mass of inorganic CPM, mg.
                                                  NH4OH to a pH of 7.0, as indicated by                      11.2.5 Container #5, Water Field                   mib = Mass of inorganic CPM in field train
                                                  the pH meter. Record the volume of                      Reagent Blank. Use 200 ml of the water                     proof blank, mg.
                                                  titrant used on the CPM Work Table (see                                                                       mo = Mass of organic CPM, mg.
                                                                                                          from the blank container for this
                                                  Figure 6 of section 18).                                                                                      mob = Mass of organic CPM in field train
                                                                                                          analysis. Transfer the water to a clean                    blank, mg.
                                                     11.2.2.3 Using a hot plate or an oven                250 ml beaker, and evaporate to                       mr = Mass of dried sample from inorganic
                                                  at 105 °C, evaporate the aqueous phase                  approximately 10 ml liquid in the oven                     fraction, mg.
                                                  to approximately 10 ml. Quantitatively                  at 105 °C. Quantitatively transfer the                N = Normality of ammonium hydroxide
                                                  transfer the beaker contents to a clean,                beaker contents to a clean 50 ml pre-                      titrant.
                                                  50 ml pre-tared weighing container and                  tared weighing container and evaporate                ppmv = Parts per million by volume.
                                                  evaporate to dryness at room                            to dryness at room temperature (not to                ppmw = Parts per million by weight.
                                                  temperature (not to exceed 30 °C (85 °F))               exceed 30 °C (85 °F)) and pressure in a               Vm(std) = Volume of gas sample measured by
                                                  and pressure in a laboratory hood.                      laboratory hood. Following evaporation,                    the dry gas meter, corrected to standard
                                                  Following evaporation, desiccate the                                                                               conditions, dry standard cubic meter
                                                                                                          desiccate the residue for 24 hours in a
                                                  residue for 24 hours in a desiccator                                                                               (dscm) or dry standard cubic foot (dscf)
                                                                                                          desiccator containing anhydrous                            as defined in Equation 5–1 of Method 5.
                                                  containing anhydrous calcium sulfate.                   calcium sulfate. Weigh at intervals of at             Vt = Volume of NH4OH titrant, ml.
                                                  Weigh at intervals of at least 6 hours to               least 6 hours to a constant weight (i.e.,
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                                                                                                                                Vp = Volume of water added during train
                                                  a constant weight. (See section 3.0 for a               less than or equal to 0.5 mg change from                   purge.
                                                  definition of constant weight.) Report                  previous weighing) and report results to
                                                  results to the nearest 0.1 mg on the CPM                the nearest 0.1 mg on Figure 5 of section               12.2 Calculations. Use the following
                                                  Work Table (see Figure 6 of section 18).                18.                                                   equations to complete the calculations
                                                     11.2.2.4 Calculate the correction                       11.2.6 Container #6, Hexane Field                  required in this test method. Enter the
                                                  factor to subtract the NH4+ retained in                 Reagent Blank. Use 200 ml of hexane                   appropriate results from these
                                                  the sample using Equation 1 in section                  from the blank container for this                     calculations on the CPM Work Table
                                                  12.                                                     analysis. Transfer 150 ml of the hexane               (see Figure 7 of section 18).


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                                                  42522                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules

                                                     12.2.1 Mass of ammonia correction.                   sample. This calculation assumes no
                                                  Correction for ammonia added during                     waters of hydration.
                                                  titration of 100 ml aqueous CPM




                                                    12.2.2 Mass of the Field Train Proof                  the field train proof blank, mfb, shall not
                                                  Blank (mg). Per section 9.9, the mass of                exceed 2.0 mg.




                                                     12.2.3    Mass of Inorganic CPM (mg).




                                                     12.2.4    Total Mass of CPM (mg).




                                                    12.2.5     Concentration of CPM (mg/
                                                  dscf).




                                                    12.3 Emissions Test Report. You                       16.0 Alternative Procedures                              (2) Justification by the facility that the
                                                  must prepare a test report following the                   16.1 Alternative Field Train Proof                 environment around the sampling
                                                  guidance in EPA Guideline Document                      Blank Procedure. The following                        location is likely to bias the CPM
                                                  043.                                                    procedure may be utilized with                        results. This justification may include:
                                                                                                          approval by the regulatory authority at                  (a) Schematic of the facility
                                                  13.0    Method Performance                                                                                    identifying locations that may
                                                                                                          stationary sources with environments
                                                    A field evaluation (NCASI 2017) of                    with significant ambient PM                           contribute to environmental bias;
                                                  Method 202 incorporating Best Practices                 concentrations that could positively bias                (b) Ambient PM concentration (mg/
                                                  showed that the detection limit was 1.6                 the results of the Method 202 samples                 m3);
                                                  for total CPM; consisting of                            collected. This procedure would permit                   (c) Previous test results (i.e., field
                                                  approximately 1.0 mg for organic CPM                    you to subtract up to 0.0039 g (3.9 mg)               train proof blank results).




                                                                                                                                                                                                                EP08SE17.004</GPH>
                                                  and approximately 0.6 mg for inorganic                  from the measured condensable                            16.1.2 Upon the regularity authority
                                                  CPM. This field evaluation also                         particulate mass.                                     approval, you will recover a minimum
                                                  demonstrated that the expected blank                       16.1.1 The facility must request this              of two field train proof blanks for each
                                                  value of the field train proof blank was                alternative prior to the test program, and            source category tested at the subject
                                                                                                          the request must be approved by the                   facility using glassware prepped
                                                                                                                                                                                                                EP08SE17.003</GPH>

                                                  less than 1.8 mg.
                                                                                                          regulatory authority prior to the testing.            according to section 8.4 of this method.
                                                  14.0    Pollution Prevention                            The request may include the following                 You must perform the field train proof
                                                                                                          elements:                                             blank evaluations as described in
                                                     [Reserved]                                                                                                 section 9.9 of this method.
                                                                                                             (1) Documented adherence to the Best
                                                                                                                                                                                                                EP08SE17.002</GPH>




                                                  15.0    Waste Management                                Practices for Method 202 by the tester.                  16.1.3 From each field sample
                                                                                                          This documentation may include:                       weight, you will subtract the average
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                     Solvent and water are evaporated in a                   (a) Tester’s Method 202 standard                   condensable particulate mass you
                                                  laboratory hood during analysis. No                     operating procedure (SOP);                            determine with all of the duplicate field
                                                  liquid waste is generated in the                           (b) Residual mass of the laboratory                train proof blank trains or 0.0039 g (3.9
                                                                                                                                                                                                                EP08SE17.001</GPH>




                                                  performance of this method. Organic                     reagent blanks (Reagent ID,                           mg), whichever is less unless the
                                                  solvents used to clean sampling                         Manufacturer, Lot Number);                            difference between highest and lowest
                                                  equipment should be managed as                             (c) Tester-specific Method Detection               values of the field train proof blanks is
                                                  Resource Conservation and Recovery                      Limit;                                                >1.0 mg. If the agreement is >1.0 mg,
                                                                                                                                                                                                                EP08SE17.000</GPH>




                                                  Act organic waste.                                         (d) Training records.                              then you must subtract the lowest


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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                                            42523

                                                  condensable particulate mass values                     (4) Electric Power Research Institute (EPRI).              Contract No. EP–D–07–097, Work
                                                  you determine with the field train proof                     2008. ‘‘Laboratory Comparison of                      Assignment 2–03, October 2008.
                                                  blank trains or 0.002 g (2.0 mg),                            Methods to Sample and Analyze                    (11) U.S. Environmental Protection Agency.
                                                                                                               Condensable PM.’’ EPRI Agreement EP–                  2005. ‘‘Laboratory Evaluation of Method
                                                  whichever is less, unless otherwise                          P24373/C11811 Condensable Particulate                 202 to Determine Fate of SO2 in Impinger
                                                  specified by the regulatory authority.                       Methods: EPRI Collaboration with EPA,                 Water,’’ EPA Contract No. 68–D–02–061,
                                                    16.2 Alternative Method 2.                                 October 2008.                                         Work Assignment 3–14, September 30,
                                                  Thermocouple Calibration (ALT–011)                      (5) Nothstein, Greg. Masters Thesis.                       2005.
                                                  for the thermocouple calibration can be                      University of Washington. Department of          (12) U.S. Environmental Protection Agency.
                                                                                                               Environmental Health. Seattle,                        2010. ‘‘Field Valuation of an Improved
                                                  found at http://www3.epa.gov/ttn/emc/                        Washington.
                                                  approalt/alt-011.pdf.                                                                                              Method for Sampling and Analysis of
                                                                                                          (6) Richards, J., T. Holder, and D. Goshaw.                Filterable and Condensable Particulate
                                                  17.0    References                                           2005. ‘‘Optimized Method 202 Sampling                 Matter.’’ Office of Air Quality Planning
                                                                                                               Train to Minimize the Biases Associated               and Standards, Sector Policy and
                                                  (1) Commonwealth of Pennsylvania,                            with Method 202 Measurement of                        Program Division Monitoring Policy
                                                       Department of Environmental Resources.                  Condensable PM Emissions.’’ Paper                     Group. Research Triangle Park, NC
                                                       1960. Chapter 139, Sampling and Testing                 presented at Air & Waste Management                   27711.
                                                       (Title 25, Rules and Regulations, part I,               Association Hazardous Waste                      (13) Wisconsin Department of Natural
                                                       Department of Environmental Resources,                  Combustion Specialty Conference. St.                  Resources. 1988. Air Management
                                                       Subpart C, Protection of Natural                        Louis, Missouri. November 2–3, 2005.                  Operations Handbook, Revision 3.
                                                       Resources, Article III, Air Resources).            (7) Texas Air Control Board, Laboratory
                                                                                                                                                                     January 11, 1988.
                                                       January 8, 1960.                                        Division. 1976. ‘‘Determination of
                                                                                                                                                                (14) U.S. Environmental Protection Agency.
                                                                                                               Particulate in Stack Gases Containing
                                                  (2) DeWees, W.D. and K.C. Steinsberger.                                                                            2016. ‘‘EPA Method 202 Best Practices
                                                                                                               Sulfuric Acid and/or Sulfur Dioxide.’’
                                                       1989. ‘‘Method Development and                                                                                Handbook.’’ Office of Air Quality
                                                                                                               Laboratory Methods for Determination of
                                                       Evaluation of Draft Protocol for                                                                              Planning and Standards, Air Quality
                                                                                                               Air Pollutants. Modified December 3,
                                                       Measurement of Condensable Particulate                                                                        Assessment Division, Measurements
                                                                                                               1976.
                                                       Emissions.’’ Draft Report. November 17,                                                                       Technology Group. Research Triangle
                                                                                                          (8) Puget Sound Air Pollution Control
                                                       1989.                                                                                                         Park, NC 27711.
                                                                                                               Agency, Engineering Division. 1983.
                                                  (3) DeWees, W.D., K.C. Steinsberger, G.M.                    ‘‘Particulate Source Test Procedures             (15) National Council for Air and Stream
                                                       Plummer, L.T. Lay, G.D. McAlister, and                  Adopted by Puget Sound Air Pollution                  Improvement. Research Brief submitted
                                                       R.T. Shigehara. 1989. ‘‘Laboratory and                  Control Agency Board of Directors.’’                  to the US EPA. May 25, 2017. ‘‘Method
                                                       Field Evaluation of EPA Method 5                        Seattle, Washington. August 11, 1983.                 202 Zero Bias Study When Incorporating
                                                       Impinger Catch for Measuring                       (9) U.S. Environmental Protection Agency,                  Draft Best Practices Developed by the US
                                                       Condensable Matter from Stationary                      Federal Reference Methods 1 through 5                 EPA.’’ NCASI Southern Research Center.
                                                       Sources.’’ Paper presented at the 1989                  and Method 17, 40 CFR 60, appendix A–                 Newberry, Florida 32669.
                                                       EPA/AWMA International Symposium                        1 through A–3 and A–6.                           18.0 Tables, Diagrams, Flowcharts,
                                                       on Measurement of Toxic and Related                (10) U.S. Environmental Protection Agency.            and Validation Data
                                                       Air Pollutants. Raleigh, North Carolina.                2008. ‘‘Evaluation and Improvement of
                                                       May 1–5, 1989.                                          Condensable PM Measurement,’’ EPA                BILLING CODE 6560–50–P
sradovich on DSK3GMQ082PROD with PROPOSALS




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                                                  42524                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules




                                                                                Figure 1. Schematic of Condensable Particulate Sampling Train




                                                                                        Set nitrogen flow rate
                                                                                        to 14 lpm or M@




                                                                                           •
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                                                                                                                                                   EP08SE17.006</GPH>




                                                                                                Figure 2. Nitrogen Purge (Entire CPM Train)
                                                                                                                                                                                   EP08SE17.005</GPH>




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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                            42525


                                                                                                                                                           CPM Filter


                                                                                                Set nitrogen flow rate
                                                                                                     141pm




                                                                                    Filter



                                                                                                     I




                                                                                                                                                     Collected




                                                                                                     Set nitrogen flow rate
                                                                                                     to 14 lpm or llH@




                                                                                                                                                     Collected
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                                                           Figure 3. Nitrogen Purge (Alternative Configurations)
                                                                                                                                                                                            EP08SE17.007</GPH>




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                                                  42526                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules


                                                                                                            CPM Impinger Field Data Page
                                                          Plant
                                                          Date
                                                          Source ID
                                                          Run Number
                                                                                                                                                    Mass of Liquid Collected
                                                                                                                                 CPM Impingers                                Moisture Trap
                                                                                                                             Dropout                 Back-up
                                                                                                                            Impinger                Impinger           Impinger       Silica Gel
                                                          Final- g
                                                          Initial- g
                                                          VP - Water added to purge train - ml 1                                                                            ----         ----
                                                                                            2
                                                          Mass of water collected
                                                          Total mass of water collected
                                                          Condition of Silica Gel
                                                                                                                            Post-Test Purge

                                                                                                                                                    Nitrogen         CPM Filter       Moisture
                                                                                                                          Time                      Flowrate-          Temp.         Trap Temp. 3
                                                                                                                        (HH:MM)                        lpm                 CF)           CF)
                                                          Start




                                                          End



                                                          1
                                                            Convert volume of water to mass by multiplying volume by density of water (lg/ml)
                                                          2
                                                            Final Mass - (Initial mass - water added for purge)
                                                          3
                                                            If applicable

                                                                                                       Figure 4. CPM Impinger Data Sheet
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                                                                                                                                                                    EP08SE17.008</GPH>




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sradovich on DSK3GMQ082PROD with PROPOSALS
VerDate Sep<11>2014
16:39 Sep 07, 2017




                                                                                                                                                                             Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules
                          Plant                                                                                             Ambient Pres. - "Hg
                           ocation                                                                                          !Barometric Pres - "Hg
                          Operator                                                                                          Static Press. - "H20
                          Date                                                                                              Assumed%M
Jkt 241001




                          Run Number                                                                                        !Probe Length
                          Sample Box                                                                                                             Leak Checks
                          MeterBoxiD                                        IY - Meter Box Cal.                             Sample Train Vacuum-           Pre     Post
PO 00000




                          Pitot Tube ID                                     Cp - Pitot Cal.                                 "Hg
                          Nozzle ID                                         ion Nozzle Diameter- in                         Sample Train Rate - cfm
                                                                                                                            IPitot Tube
Frm 00041




                                                                                                                                         Exit to
                                                                    AP                                                                  Moisture                   Tm
Fmt 4702




                             Traverse                  DGM       Velocity       Llli                    Probe      Filter   CPMFilter     Trap         Tm        Outlet to
                              Point                  Gas Meter     Head        Meter        Meter     Temperatur Temperatur Temperatur Temperatur Inlet to Dry   Dry Gas
                             Number          Time     Reading    Pressure     Pressure     Vacuum         e          e          e          e       Gas Meter      Meter
Sfmt 4725




                                             (min)      (cf)      ("H2 0)      ("H2 0)      ("Hg)        CF)        CF)        CF)        CF)         CF)          CF)
E:\FR\FM\08SEP1.SGM
08SEP1




                                                                                       Figure 5. Field Data Sheet




                                                                                                                                                                             42527
EP08SE17.009</GPH>


                                                  42528                 Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules


                                                                                        Field Train Proof Blank Condensable Particulate Calculations
                                                          Plant
                                                          Date
                                                          Blank No.
                                                          Field Reagent Blank Mass
                                                          Water (Section 11.2.7)                                                                                                  mg
                                                          Acetone (Section 11.2.6)                                                                                                mg
                                                          Hexane (Section 11.2.8)                                                                                                 mg
                                                          Field Train Proof Blank Mass
                                                          Mass of Organic CPM (mob)(Section 11.2.3)                                                                               mg
                                                          Mass oflnorganic CPM (mib)(Equation 3)                                                                                  mg
                                                          Mass of the Field Train Proof Blank (not to exceed 2.0 mg) (Equation 2)                                                 mg


                                                                         Figure 6. Field Train Proof Blank Condensable Particulate Calculations
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                                                                                                                                                       EP08SE17.010</GPH>




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                                                                        Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules                           42529

                                                          Calculations for Recovery of Condensable PM (CPM)
                                                          Plant - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
                                                          Date - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
                                                          RunNo. - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
                                                          Sample Preparation- CPM Containers No.1 and 2 (Section 11.1)

                                                          Was significant volume of water lost during transport?
                                                          YesorNo
                                                          IfYes, measure the volume received.
                                                          Estimate the volume lost during transport.                                                                              ml

                                                          Was significant volume of organic rinse lost during
                                                          transport? Yes or No
                                                          IfYes, measure the volume received.
                                                          Estimate the volume lost during transport.                                                                              ml
                                                          For Titration
                                                          Normality ofNHpH (N)

                                                          (Section 10.2)                                                                                                          N
                                                          Volume oftitrant (V)t

                                                          (Section 11.2.2.2)                                                                                                      ml
                                                          Mass ofNH4 added (m)

                                                          (Equation 1)                                                                                                            mg
                                                          For CPM Blank Weights
                                                          Inorganic Field Train ProofBlank Mass(mib) (Section 9.9)                                                                mg
                                                                                                                                              -------------------------
                                                          Organic Field Train Proof Blank Mass (mob) (Section 9.9)                                                                mg
                                                          Mass of Field Train Proof Blank (Mfb) (max. 2 mg)
                                                          (Equation 2)                                                                                                            mg
                                                          For CPM Train Weights
                                                          Mass of Organic CPM (m 0 ) (Section 11.2.3)                                                                             mg
                                                          Mass oflnorganic CPM (m)1 (Equation 3)                                                                                  mg
                                                          Total CPM Mass (m cpm ) (Equation 4)                                                                                    mg


                                                                                                                Figure 7. CPM Work Table
sradovich on DSK3GMQ082PROD with PROPOSALS




                                                                                                                                                                                           EP08SE17.011</GPH>




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42530                 Federal Register/Vol. 82, No. 173 /Friday, September 8, 2017/Proposed Rules

                                                               Collect Sample
                                                               Using Filterable and
                                                               Condensable Methods

                                                                            %

                                                             Measure Sample Volumes
                                                                           8.5.3



                                                                  Extract CPM
                                                                          Filter
                                                                          11.2.1



                    Combine Filter Extract                                               Combine Filter Extract w/
                      w/Container #1 — Impinger                                         Container #2 — Organic Train
                               Aqueous Sample                                                    lf%?i?Z
                                  11.2.1.1                                                         tTt

                         l                                                               ¥
                                              Combine Organic                                            .
               Extract                          Extract w/                     Evaporate             Desiccate and
          Combined Aqueous                     Organic Train                    Organic            Weigh Organic CPM
              Inorganic    —»p|                   Rinse —             p     Fraction (Room         to Constant Weight
              Fraction                         Container #2                   Temperature          and Report Results
                11.2.2                             11.2 .3                       11.2.3                   11.2.3




               Two SFep                        Desiccate and
            Evaporation to                       R
                 Dr                            Weigh Aqueous
                      yness          —»          7
                                                   norganic
              (Heated and                         Fraction
              Room Temp.)
                11.2.2 .1                         11.2.2.1




                                              Constant Weight
                                             Requirement Met?




                                     NO
                                                                Yes
                               Reconstitute
                             sample to 100 ml           Report Results
                                 11.2.2.1                  11.2.2 .1




                                                 Two Step                           .
                Titrate                       Evaporation to                    %Zilficzteegfig        Correct Mass for
              Sample with            —t»          Dryness             >           Ig    ans            NH, added and
              0.1 N NH,OH                       (Heated and                        norganig           Report Results
                                                                                   Fraction
                11.2.2.2                        Room Temp.                        11.2.2.3               11.2.2.4
                                                 11.2.2.3                           tttt*


                                             Figure 8. CPM Sample Processing Flow Chart

[FR Doc. 2017—18425 Filed 9—7—17; 8:45 am]
BILLING CODE 6560—50—C



Document Created: 2018-10-24 14:10:12
Document Modified: 2018-10-24 14:10:12
CategoryRegulatory Information
CollectionFederal Register
sudoc ClassAE 2.7:
GS 4.107:
AE 2.106:
PublisherOffice of the Federal Register, National Archives and Records Administration
SectionProposed Rules
ActionProposed rule.
DatesComments. Comments must be received on or before November 7, 2017.
ContactMr. 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-
FR Citation82 FR 42508 
RIN Number2060-AS91
CFR AssociatedAdministrative Practice and Procedure; Air Pollution Control; Epa Method 202; Incorporation by Reference; Particulate Matter; Reporting and Recordkeeping Requirements and Sulfur Dioxide

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