Method 202-Dry Impinger Method for Determining Condensable Particulate Emissions From Stationary Sources, 42508-42530 [2017-18425]
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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 applicable).
Approved information collection and OMB Control Number (as applicable).
Brief description of concern ......................................................................
Available data on cost or economic impact .............................................
Proposed solution .....................................................................................
III. References
The following references are on
display in the Dockets Management
Staff office (see ADDRESSES) and are
available for viewing by interested
persons between 9 a.m. and 4 p.m.,
Monday through Friday; they are also
available electronically at https://
www.regulations.gov. FDA has verified
the Web site addresses, as of the date
this document publishes in the Federal
Register, but Web sites are subject to
change over time.
1. Executive Order 13771 (January 30, 2017);
available at https://
www.federalregister.gov/documents/
2017/02/03/2017-02451/reducingregulation-and-controlling-regulatorycosts.
2. Executive Order 13777 (February 24,
2017); available at https://
www.federalregister.gov/documents/
2017/03/01/2017-04107/enforcing-theregulatory-reform-agenda.
Dated: August 30, 2017.
Anna K. Abram,
Deputy Commissioner for Policy, Planning,
Legislation, and Analysis.
[FR Doc. 2017–19047 Filed 9–7–17; 8:45 am]
BILLING CODE 4164–01–P
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Part 51
[EPA–HQ–OAR–2016–0456; FRL–9966–75–
OAR]
RIN 2060–AS91
sradovich on DSK3GMQ082PROD with PROPOSALS
Method 202—Dry Impinger Method for
Determining Condensable Particulate
Emissions From Stationary Sources
Environmental Protection
Agency (EPA).
ACTION: Proposed rule.
AGENCY:
In this action, the
Environmental Protection Agency (EPA)
proposes editorial and technical
revisions to the EPA’s Method 202—Dry
Impinger Method for Determining
SUMMARY:
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(For example, what innovation makes the regulation outdated? Why?)
(Quantified costs and/or cost savings. Qualitative description, if needed.)
(Include your solution. For example, how would you modify the regulation? Provide specific text if you are recommending a modification.)
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 https://
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
https://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
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hearing on our Web site at: https://
www.epa.gov/emc/emc-proposed-testmethods. 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 shappley.ned@epa.gov 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 https://
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 https://
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:
shappley.ned@epa.gov.
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?
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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
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
NAICS a
Industry ............................................................................
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a North
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:
I. General Information
Category
332410
332410
332410
324110
562213
322110
325188
327310
327410
211111
212111
212112
212113
331312
331314
331111
331513
321219
321211
321212
42509
Examples of regulated entities
Fossil fuel steam generators.
Industrial, commercial, institutional steam generating units.
Electricity generating units.
Petroleum refineries.
Municipal waste combustors.
Pulp and paper mills.
Sulfuric acid plants.
Portland cement plants.
Lime manufacturing plants.
Coal preparation plants.
Primary and secondary aluminum plants.
Iron and steel plants.
Plywood and reconstituted products plants.
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–
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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
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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 https://
www.regulations.gov or email. Send or
deliver information identified as CBI to
only the following address: OAQPS
Document Control Officer (Room C404–
02), U.S. EPA, Research Triangle Park,
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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
2. Docket
(56 FR 65433), the EPA first
The docket number for the Method
promulgated Method 202 to provide a
202 revisions is Docket ID No. EPA–
test method for measuring CPM from
HQ–OAR–2016–0456.
stationary sources. Method 202, as
promulgated in 1991, used water-filled
C. Where can I get a copy of this
impingers to cool, condense, and collect
document and other related
materials that are vaporous at stack
information?
conditions and become solid or liquid
World Wide Web (WWW). In addition
PM at ambient air temperatures. Method
to being available in the docket, an
202, as promulgated in 1991, contains
electronic copy of the proposed method several optional procedures that were
revisions is available on the Air
intended to accommodate the various
Emission Measurement Center (EMC)
test methods in use by state and local
Web site at https://www.epa.gov/emc/
regulatory entities at the time Method
emc-proposed-test-methods.
202 was being developed.
When conducted consistently and
II. Background
carefully, this version of the method
Section 110 of the Clean Air Act, as
provided improved precision for most
amended (42 U.S.C. 7410), requires state emission sources, and has been
and local air pollution control agencies
successfully implemented in regulatory
to develop, and submit for EPA
programs where the emission limits and
approval, State Implementation Plans
compliance demonstrations are
(SIPs) that provide for the attainment,
established based on a consistent
maintenance, and enforcement of the
application of Method 202 and its
NAAQS in each air quality control
associated options. However, when the
region (or portion thereof) within each
same emission source is tested using
state. The emissions inventory and
different combinations of the optional
analyses used in the state’s attainment
procedures within the method, there
demonstrations must consider PM2.5 and were variations in the measured CPM
particles less than 10 micrometers in
emissions. Additionally, during
diameter (PM10) emissions from
validation of the method, we
stationary sources that are significant
determined that sulfur dioxide (SO2) gas
contributors of primary PM10 and PM2.5
(a typical component of emissions from
emissions. Primary or direct PM
several types of stationary sources) can
emissions are the solid particles or
be absorbed partially in the impinger
liquid droplets emitted directly from an solutions and can react chemically to
air emissions source or activity and the
form sulfuric acid. This sulfuric acid
gaseous emissions or liquid droplets
‘‘artifact’’ is not related to the primary
from an air emissions source or activity
emission of CPM from the source, but
that condense to form PM or liquid
may be counted erroneously as CPM
droplets at ambient temperatures.
when using Method 202. The EPA
Subpart A of 40 CFR part 51
conducted additional studies to further
(Requirements for Preparation,
examine the mechanism and the effects
Adoption, and Submittal of
of sulfuric acid formation. The results of
Implementation Plans) defines primary
our 1989 laboratory study and field
PM2.5 and PM10 as including both the
evaluation commissioned to evaluate
filterable and condensable fractions of
the impinger approach can be found in
PM. Filterable PM consists of those
‘‘Laboratory and Field Evaluation of the
particles that are directly emitted by a
EPA Method 5 Impinger Catch for
source as a solid or liquid at the stack
Measuring Condensible Matter from
(or similar release conditions) and
Stationary Sources.’’ The report of that
captured on the filter of a stack test
work is available in the docket as EPA–
sampling train. Condensable PM is the
HQ–OAR–2016–0456–0001. Essentially,
material that is in vapor phase at stack
the 1989 study verified the need for a
conditions but condenses and/or reacts
nitrogen purge when SO2 is present in
upon cooling and dilution in the
stack gas and also provided guidance for
ambient air to form solid or liquid PM
analyzing the collected samples. In
immediately after discharge from the
2005, an EPA contractor conducted a
stack. In response to the need to
second study, ‘‘Laboratory Evaluation of
quantify primary PM10 and PM2.5
Method 202 to Determine Fate of SO2 in
emissions from stationary sources, the
Impinger Water,’’ that replicated some
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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.
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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
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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-practiceshandbook.pdf.
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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
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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
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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
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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 preweighed 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
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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 °C (85 °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 °C (85 °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
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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 °C ± 3 °C (68 °F ±
5 °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
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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.
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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 acidbase 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
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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
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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.
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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 https://www2.epa.gov/lawsregulations/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)
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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
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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.
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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
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
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
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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.
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: You must maintain the gas filtration
temperature of the filterable PM method as
specified in the method, unless otherwise
specified by an applicable subpart.
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.
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.
(b) If the gas filtration temperature of
the filterable PM method used does not
exceed 30 °C (85 °F), then use of this
method is not necessary to measure
primary PM, as the CPM is collected as
filterable PM.
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Note: For those methods that require instack 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
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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.
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.
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2.1.1 Condensable PM. Condensable
PM is collected in the water dropout
impinger, the modified GreenburgSmith 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
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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 https://
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 https://
www.archives.gov/federal_register/
code_of_federal_regulattions/ibr_
locations.html.
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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
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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.
fluoropolymer O-ring. At the exit of the
CPM filter, install a fluoropolymercoated 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
6.0 Equipment and Supplies
CPM recovered from the sampling train.
The equipment used in the filterable
(a) Nitrogen purge line. You must use
particulate portion of the sampling train inert tubing and fittings capable of
is described in Methods 5 and 17 of
delivering at least 14 liters/min of
appendix A–1 through A–3 and A–6 to
nitrogen gas to the impinger train from
part 60 and Method 201A of appendix
a standard gas cylinder (see Figures 2
M to this part. The equipment used in
and 3 of section 18). You may use
the CPM portion of the train is
standard 0.6 centimeters (1⁄4 inch)
described in this section.
tubing and compression fittings in
6.1 Condensable Particulate
conjunction with an adjustable pressure
Sampling Train Components. The
regulator and needle valve.
sampling train for this method is used
(b) Rotameter. You must use a
in addition to filterable particulate
rotameter capable of measuring gas flow
collection using Method 5 of appendix
up to 20 liters/min. The rotameter must
A–3 to part 60, Method 17 of appendix
be accurate to five percent of full scale.
A–6 to part 60, or Method 201A of
(c) Nitrogen gas purging system.
appendix M to this part. This method
Compressed ultra-pure nitrogen,
includes the following exceptions or
regulator, and filter must be capable of
additions:
providing at least 14 liters/min purge
6.1.1 Probe Extension and Liner. The gas for one hour through the sampling
probe extension between the filterable
train.
particulate filter and the condenser
(d) Sample bottles (500 ml). You must
must be glass- or fluoropolymer-lined.
use amber glass bottles or other nonFollow the specifications for the probe
reactive bottles (e.g., High Density
liner specified in section 6.1.1.2 of
Linear Polyethylene (HDLPE), or PTFE)
Method 5 of appendix A–3 to part 60.
pre-cleaned sample bottles for inorganic
6.1.2 Condenser and Impingers. You samples. Amber glass bottles are
must add the following components to
required for organic samples and must
the filterable particulate sampling train: be prepared according to section 8.4 of
A vertical condenser, followed by a
this method.
water dropout impinger or flask,
6.2.2 Analysis Equipment. The
followed by a modified Greenburgfollowing equipment is necessary for
Smith impinger (backup impinger) with CPM sample analysis:
an open tube tip as described in section
(a) Separatory Funnel. Glass, 1 liter.
(b) Weighing Containers.
6.1.1.8 of Method 5 of appendix A–3 to
Fluoropolymer beaker liners or other
part 60.
6.1.3 Dropout Impinger Insert for
low-mass vessels which are unreactive
Nitrogen Purge. You must use a leak-free to the sample or atmosphere.
ground glass fitting with a long glass or
Note: The use of an anti-static device(s)
PTFE stem (e.g., modified Greenburgduring gravimetric analysis to prevent static
Smith impinger insert or purge stem,
from interfering with the analysis is
etc.) for the water dropout impinger to
recommended when using Fluoropolymer or
similar beaker liners.
perform the nitrogen purge of the
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
1⁄2″ from the bottom of the impinger.
containing anhydrous calcium sulfate
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
followed by a filter holder that is either
oven equipped with temperature
glass, stainless steel (316 or equivalent), control.
or fluoropolymer-coated stainless steel.
(e) Glass Pipets. 5 ml.
Commercial size filter holders are
(f) Burette. Glass, 0 to 100 ml in 0.1
available depending on project
ml graduations.
requirements. Use a commercial filter
(g) Analytical Balance. Analytical
holder capable of supporting 47 mm or
balance capable of weighing at least
greater diameter filter. Commercial size
0.0001 g (0.1 mg).
(h) pH Meter. The pH meter must be
filter holders contain a fluoropolymer
capable of determining the acidity of
O-ring, stainless steel, ceramic or
liquid within 0.1 pH units.
fluoropolymer filter support and a final
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(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 indicatingtype 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 °C
(350 °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, ultrafiltered 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,
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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, ultrafiltered 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:
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(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 °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 °C (85 °F).
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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 °C (less than or equal to 85
°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 °C (68 °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
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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 preweighed 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 °C (greater than 65 °F) but less
than or equal to 30 °C (less than or equal
to 85 °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 (Posttest). 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
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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 °C (68 °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 leakcheck, 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
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impinger train to be purged. Increase the
nitrogen flow gradually to avoid overpressurizing 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 °C (65 °F), but less than or equal to
30 °C (85 °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
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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, leakproof 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, leakproof 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, leakproof 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 posttest 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
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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 °C
(85 °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
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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 nonrepresentative 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 NISTtraceable glassware.
9.6 Laboratory Analytical Balance
9.6.1 Maintain the location of the
analytical balance (i.e., weighing room)
at 20 °C ± 3 °C (68 °F ± 5 °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
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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
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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 watersoluble 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
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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 °C and allow to
dry at room temperature (not to exceed
30 °C (85 °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 °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 °C (85 °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.
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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 °C (85 °F))
and pressure in a laboratory hood to not
less than 10 ml. Quantitatively transfer
the beaker contents to a clean 50 ml pretared weighing container and evaporate
to dryness at room temperature (not to
exceed 30 °C (85 °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 °C (85 °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 °C (85 °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 °C. Quantitatively transfer the
beaker contents to a clean 50 ml pretared weighing container and evaporate
to dryness at room temperature (not to
exceed 30 °C (85 °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
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42521
to a clean 250 ml beaker. Evaporate the
hexane at room temperature (not to
exceed 30 °C (85 °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 °C (85 °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.
DH@ = Pressure drop across orifice at flow
rate of 0.75 SCFM at standard
conditions, inches of water column (Note
Specific to each orifice and meter box).
17.03 = mg/milliequivalents for ammonium
ion.
ACFM = Actual cubic feet per minute.
Ccpm = Concentration of the condensable PM
in the stack gas, dry basis, corrected to
standard conditions, milligrams/dry
standard cubic foot.
mc = Mass of the NH4+ added to sample to
form ammonium sulfate, mg.
mcpm = Mass of the total condensable PM, mg.
mfb = Mass of total CPM in field train proof
blank, mg.
mg = Milligrams.
mg/dscf = Milligrams per dry standard cubic
foot.
mg/L = Milligrams per liter.
mi = Mass of inorganic CPM, mg.
mib = Mass of inorganic CPM in field train
proof blank, mg.
mo = Mass of organic CPM, mg.
mob = Mass of organic CPM in field train
blank, mg.
mr = Mass of dried sample from inorganic
fraction, mg.
N = Normality of ammonium hydroxide
titrant.
ppmv = Parts per million by volume.
ppmw = Parts per million by weight.
Vm(std) = Volume of gas sample measured by
the dry gas meter, corrected to standard
conditions, dry standard cubic meter
(dscm) or dry standard cubic foot (dscf)
as defined in Equation 5–1 of Method 5.
Vt = Volume of NH4OH titrant, ml.
Vp = Volume of water added during train
purge.
12.2 Calculations. Use the following
equations to complete the calculations
required in this test method. Enter the
appropriate results from these
calculations on the CPM Work Table
(see Figure 7 of section 18).
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12.2.1 Mass of ammonia correction.
Correction for ammonia added during
titration of 100 ml aqueous CPM
sample. This calculation assumes no
waters of hydration.
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.
12.2.3
Mass of Inorganic CPM (mg).
12.2.4
Total Mass of CPM (mg).
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]
sradovich on DSK3GMQ082PROD with PROPOSALS
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.
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Method Performance
(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/
m3);
(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
EP08SE17.002</GPH>
13.0
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.
EP08SE17.001</GPH>
12.3 Emissions Test Report. You
must prepare a test report following the
guidance in EPA Guideline Document
043.
EP08SE17.004</GPH>
Concentration of CPM (mg/
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12.2.5
dscf).
Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules
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 https://www3.epa.gov/ttn/emc/
approalt/alt-011.pdf.
17.0
References
sradovich on DSK3GMQ082PROD with PROPOSALS
(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.
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16:39 Sep 07, 2017
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(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
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42523
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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Figure 1. Schematic of Condensable Particulate Sampling Train
Set nitrogen flow rate
to 14 lpm or M@
EP08SE17.006</GPH>
Figure 2. Nitrogen Purge (Entire CPM Train)
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•
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42525
CPM Filter
Set nitrogen flow rate
141pm
Filter
I
Collected
Set nitrogen flow rate
to 14 lpm or llH@
Figure 3. Nitrogen Purge (Alternative Configurations)
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Collected
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CPM Impinger Field Data Page
Plant
Date
Source ID
Run Number
Mass of Liquid Collected
CPM Impingers
Dropout
Impinger
Back-up
Impinger
Moisture Trap
Impinger
Silica Gel
----
----
CPM Filter
Temp.
Moisture
Trap Temp. 3
CF)
CF)
Final- g
Initial- g
VP - Water added to purge train - ml 1
Mass of water collected
2
Total mass of water collected
Condition of Silica Gel
Post-Test Purge
Time
(HH:MM)
Nitrogen
Flowratelpm
Start
End
1
Convert volume of water to mass by multiplying volume by density of water (lg/ml)
Final Mass - (Initial mass - water added for purge)
3
If applicable
2
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Figure 4. CPM Impinger Data Sheet
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Time
(min)
DGM
Gas Meter
Reading
(cf)
AP
Velocity
Head
Pressure
("H2 0)
Llli
Meter
Pressure
("H2 0)
Meter
Vacuum
("Hg)
Post
"Hg
Cp - Pitot Cal.
ion Nozzle Diameter- in
Frm 00041
Traverse
Point
Number
Ambient Pres. - "Hg
!Barometric Pres - "Hg
Static Press. - "H20
Assumed%M
!Probe Length
Leak Checks
Sample Train VacuumPre
Sample Train Rate - cfm
IPitot Tube
Exit to
Moisture
Probe
Filter
CPMFilter
Trap
Tm
Temperatur Temperatur Temperatur Temperatur Inlet to Dry
Gas Meter
e
e
e
e
CF)
CF)
CF)
CF)
CF)
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Figure 5. Field Data Sheet
Tm
Outlet to
Dry Gas
Meter
CF)
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16:39 Sep 07, 2017
Plant
ocation
Operator
Date
Run Number
Sample Box
MeterBoxiD
Pitot Tube ID
Nozzle ID
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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
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Figure 6. Field Train Proof Blank Condensable Particulate Calculations
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)
N
(Section 10.2)
Volume oftitrant (V)
t
(Section 11.2.2.2)
Mass ofNH4 added (m)
ml
(Equation 1)
For CPM Blank Weights
mg
Inorganic Field Train ProofBlank Mass(mib) (Section 9.9)
-------------------------
Organic Field Train Proof Blank Mass (mob) (Section 9.9)
mg
mg
Mass of Field Train Proof Blank (Mfb) (max. 2 mg)
(Equation 2)
For CPM Train Weights
mg
Mass of Organic CPM (m 0 ) (Section 11.2.3)
mg
Mass oflnorganic CPM (m) (Equation 3)
1
mg
Total CPM Mass (m cpm ) (Equation 4)
mg
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Figure 7. CPM Work Table
42530
Federal Register / Vol. 82, No. 173 / Friday, September 8, 2017 / Proposed Rules
Collect SailiJ?le
Using Filterable and
Condensable Methods
~
Measure Sample Volumes
8.5.3
1
Extract CPM
Filter
11.2.1
Combine Filter Extract
w/Container #1 - Impinger
Aqueous SailiJ?le
11.2 .1.1
~
+
Combine Filter Extract w/
Container #2
Organic Train
Rinse
11.2 .1.2
~
!
Extract
Combined Aqueous
Inorganic
Fraction
11.2 .2
Combine Organic
Extract w/
Organic Train
Rinse Container #2
11.2. 3
f-+
f--.+
Evaporate
Organic
Fraction (Room
Temperature
11.2. 3
Desiccate and
Weigh Organic CPM
to Constant Weight
and ReEort Results
11.2. 3
I_.,
~
Two Step
Evaporation to
Dryness
(Heated and
Room Temp.)
11.2 .2 .1
Desiccate and
Weigh Aqueous
Inorganic
Fraction
11.2 .2 .1
_.,
T
Constant Weight
Requirement Met?
..---- ----..
NO
Yes
Reconstitute
sample to 100 ml
11.2 .2 .1
ReEort Results
11.2 .2 .1
~
Two Step
Evaporation to
Dryness
(Heated and
Room Temp.
11.2 .2. 3
f---+
-+
Desiccate and
Weigh Aqueous
Inorganic
Fraction
11.2.2.3
____,..
Correct Mass for
~ added and
ReEort Results
11.2.2.4
Figure 8. CPM Sample Processing Flow Chart
[FR Doc. 2017–18425 Filed 9–7–17; 8:45 am]
BILLING CODE 6560–50–C
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Titrate
Sample with
0.1 N ~OH
11.2 .2 .2
]]>Agencies
[Federal Register Volume 82, Number 173 (Friday, September 8, 2017)]
[Proposed Rules]
[Pages 42508-42530]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2017-18425]
=======================================================================
-----------------------------------------------------------------------
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.
-----------------------------------------------------------------------
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 https://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 https://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
shappley.ned@epa.gov 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 https://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 https://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: shappley.ned@epa.gov.
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 https://www.regulations.gov or email. Send or deliver
information identified as CBI to only the following address: OAQPS
Document Control Officer (Room C404-02), U.S. EPA, Research Triangle
Park,
[[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 https://www2.epa.gov/laws-regulations/laws-and-executive-orders.
A. Executive Order 12866: Regulatory Planning and Review and Executive
Order 13563: Improving Regulation and Regulatory Review
This action is not a significant regulatory action and was,
therefore, not submitted to the Office of Management and Budget (OMB)
for review.
B. Executive Order 13771: Reducing Regulations and Controlling
Regulatory Costs
This action is 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 https://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
https://www.archives.gov/federal_register/code_of_federal_regulattions/ibr_locations.html.
4.0 Interferences
[Reserved]
5.0 Safety
Disclaimer. Because the performance of this method may require the
use of hazardous materials, operations, and equipment, you should
develop a health and safety plan to ensure the safety of your employees
who are on site conducting the particulate emission test. Your plan
should conform with all applicable Occupational Safety and Health
Administration, Mine Safety and Health Administration, and Department
of Transportation regulatory requirements. Because of the unique
situations at some facilities and because some facilities may have more
stringent requirements than is required by state or federal laws, you
may have to develop procedures to conform to the plant health and
safety requirements.
6.0 Equipment and Supplies
The equipment used in the filterable particulate portion of the
sampling train is described in Methods 5 and 17 of appendix A-1 through
A-3 and A-6 to part 60 and Method 201A of appendix M to this part. The
equipment used in the CPM portion of the train is described in this
section.
6.1 Condensable Particulate Sampling Train Components. The sampling
train for this method is used in addition to filterable particulate
collection using Method 5 of appendix A-3 to part 60, Method 17 of
appendix A-6 to part 60, or Method 201A of appendix M to this part.
This method includes the following exceptions or additions:
6.1.1 Probe Extension and Liner. The probe extension between the
filterable particulate filter and the condenser must be glass- or
fluoropolymer-lined. Follow the specifications for the probe liner
specified in section 6.1.1.2 of Method 5 of appendix A-3 to part 60.
6.1.2 Condenser and Impingers. You must add the following
components to the filterable particulate sampling train: A vertical
condenser, followed by a water dropout impinger or flask, followed by a
modified Greenburg-Smith impinger (backup impinger) with an open tube
tip as described in section 6.1.1.8 of Method 5 of appendix A-3 to part
60.
6.1.3 Dropout Impinger Insert for Nitrogen Purge. You must use a
leak-free ground glass fitting with a long glass or PTFE stem (e.g.,
modified Greenburg-Smith impinger insert or purge stem, etc.) for the
water dropout impinger to perform the nitrogen purge of the sampling
train. The glass stem must be designed so that the tip of the stem is
\1/2\'' from the bottom of the impinger.
6.1.4 CPM Filter Holder. The modified Greenburg-Smith impinger is
followed by a filter holder that is either glass, stainless steel (316
or equivalent), or fluoropolymer-coated stainless steel. Commercial
size filter holders are available depending on project requirements.
Use a commercial filter holder capable of supporting 47 mm or greater
diameter filter. Commercial size filter holders contain a fluoropolymer
O-ring, stainless steel, ceramic or fluoropolymer filter support and a
final fluoropolymer O-ring. At the exit of the CPM filter, install a
fluoropolymer-coated or stainless steel encased thermocouple that is in
direct contact with the gas stream.
6.2 Sample Recovery Equipment
6.2.1 Condensable PM Recovery. Use the following equipment to
quantitatively determine the amount of CPM recovered from the sampling
train.
(a) Nitrogen purge line. You must use inert tubing and fittings
capable of delivering at least 14 liters/min of nitrogen gas to the
impinger train from a standard gas cylinder (see Figures 2 and 3 of
section 18). You may use standard 0.6 centimeters (\1/4\ inch) tubing
and compression fittings in conjunction with an adjustable pressure
regulator and needle valve.
(b) Rotameter. You must use a rotameter capable of measuring gas
flow up to 20 liters/min. The rotameter must be accurate to five
percent of full scale.
(c) Nitrogen gas purging system. Compressed ultra-pure nitrogen,
regulator, and filter must be capable of providing at least 14 liters/
min purge gas for one hour through the sampling train.
(d) Sample bottles (500 ml). You must use amber glass bottles or
other non-reactive bottles (e.g., High Density Linear Polyethylene
(HDLPE), or PTFE) pre-cleaned sample bottles for inorganic samples.
Amber glass bottles are required for organic samples and must be
prepared according to section 8.4 of this method.
6.2.2 Analysis Equipment. The following equipment is necessary for
CPM sample analysis:
(a) Separatory Funnel. Glass, 1 liter.
(b) Weighing Containers. Fluoropolymer beaker liners or other low-
mass vessels which are unreactive to the sample or atmosphere.
Note: The use of an anti-static device(s) during gravimetric
analysis to prevent static from interfering with the analysis is
recommended when using Fluoropolymer or similar beaker liners.
(c) Glass Beakers. 300 to 500 ml.
(d) Drying Equipment. A desiccator containing anhydrous calcium
sulfate that is maintained below 10 percent relative humidity, and a
hot plate or oven equipped with temperature control.
(e) Glass Pipets. 5 ml.
(f) Burette. Glass, 0 to 100 ml in 0.1 ml graduations.
(g) Analytical Balance. Analytical balance capable of weighing at
least 0.0001 g (0.1 mg).
(h) pH Meter. The pH meter must be capable of determining the
acidity of liquid within 0.1 pH units.
[[Page 42517]]
(i) Sonication Device. The device must have a minimum sonication
frequency of 20 kHz and be approximately four to six inches deep to
accommodate the sample extractor tube.
(j) Leak-Proof Sample Containers. Containers used for sample and
blank recovery must not contribute more than 0.05 mg of residual mass
to the CPM measurements.
(k) Wash bottles. Any container material is acceptable, but wash
bottles used for sample and blank recovery must not contribute more
than 0.1 mg of residual mass to the CPM measurements.
7.0 Reagents and Standards
7.1 Sample Collection. To collect a sample, you will need a CPM
filter, crushed ice, and silica gel. You must also have water and
nitrogen gas to purge the sampling train. You will find additional
information on each of these items in the following summaries.
7.1.1 CPM Filter. You must use a nonreactive, non-disintegrating
polymer filter that does not have an organic binder and does not
contribute more than 0.5 mg of residual mass to the CPM measurements.
The CPM filter must also have an efficiency of at least 99.95 percent
(less than 0.05 percent penetration) on 0.3 micrometer dioctyl
phthalate particles. You may use test data from the supplier's quality
control program to document the CPM filter efficiency.
7.1.2 Silica Gel. Use an indicating-type silica gel of 6 to 16
mesh. You must obtain approval of the Administrator for other types of
desiccants (equivalent or better) before you use them. Allow the silica
gel to dry for 2 hours at 175 [deg]C (350 [deg]F) if it is being
reused. You do not have to dry new silica gel if the indicator shows
the silica gel is active for moisture collection.
7.1.3 Water. Use deionized, ultra-filtered water that contains 1.0
parts per million by weight (ppmw) (1 mg/L) residual mass or less to
recover and extract samples.
7.1.4 Crushed Ice. Obtain from the best readily available source.
7.1.5 Nitrogen Gas. Use Ultra-High Purity compressed nitrogen or
equivalent to purge the sampling train. The compressed nitrogen you use
to purge the sampling train must contain no more than 1 parts per
million by volume (ppmv) oxygen, 1 ppmv total hydrocarbons as carbon,
and 2 ppmv moisture. The compressed nitrogen must not contribute more
than 0.1 mg of residual mass per purge.
7.2 Sample Recovery and Analytical Reagents. You will need acetone,
hexane, anhydrous calcium sulfate, ammonia hydroxide, and deionized
water for the sample recovery and analysis. Unless otherwise indicated,
all reagents must conform to the specifications established by the
Committee on Analytical Reagents of the American Chemical Society. If
such specifications are not available, then use the best available
grade. Additional information on each of these items is in the
following paragraphs:
7.2.1 Acetone. Use acetone that is stored in a glass bottle. Do not
use acetone from a metal container because it normally produces a high
residual mass in the laboratory and field reagent blanks. You must use
acetone that has a blank value less than 1.0 ppmw (0.1 mg/100 g)
residue.
7.2.2 Hexane, American Chemical Society Grade or Equivalent. You
must use hexane that has a blank residual mass value less than 1.0 ppmw
(0.1 mg/100 g) residue.
7.2.3 Water. Use deionized, ultra-filtered water that contains 1.0
ppmw (1.0 mg/L) residual mass or less to recover material caught in the
impinger.
7.2.4 Condensable Particulate Sample Desiccant. Use indicating-type
anhydrous calcium sulfate to desiccate water and organic extract
residue samples prior to weighing.
7.2.5 Ammonium Hydroxide. Use National Institute of Standards and
Technology (NIST)-traceable or equivalent (0.1 N) ammonium hydroxide
(NH4OH).
7.2.6 Standard Buffer Solutions. Use one buffer solution with a
neutral pH and a second buffer solution with an acid pH of no less than
4.
8.0 Sample Collection, Preservation, Storage, and Transport
8.1 Qualifications. This is a complex test method. To obtain
reliable results, you should be trained and experienced with in-stack
filtration systems (such as, cyclones, impactors, and thimbles) and
impinger and moisture train systems.
8.2 Preparations. Clean all glassware used to collect and analyze
samples prior to field tests as described in Section 8.4 prior to use.
Cleaned glassware must be used at the start of each new source category
tested at a single facility. You must analyze laboratory reagent blanks
(water, acetone, and hexane) before field tests to verify low blank
concentrations for the reagent lot(s) used. Follow the pretest
preparation instructions in Section 8.1 of Method 5.
8.3 Site Setup. You must follow the procedures required in Methods
5, 17, or 201A, whichever is applicable to your test requirements
including:
(a) Determining the sampling site location and traverse points.
(b) Calculating probe/cyclone blockage (as appropriate).
(c) Verifying the absence of cyclonic flow.
(d) Completing a preliminary velocity profile, and selecting a
nozzle(s) and sampling rate.
8.3.1 Sampling Site Location. Follow the standard procedures in
Method 1 of appendix A-1 to part 60 to select the appropriate sampling
site. Choose a location that maximizes the distance from upstream and
downstream flow disturbances.
8.3.2 Traverse Points. Use the required number of traverse points
at any location, as found in in the method used to collect the
filterable particulate. You must prevent the disturbance and capture of
any solids accumulated on the inner wall surfaces by maintaining a 1
inch distance from the stack wall (0.5 inch for sampling locations less
than 24 inches in diameter).
8.4 Sampling Train Preparation. A schematic of the sampling train
used in this method is shown in Figure 1 of section 18. All glassware
that is used to collect and analyze samples should be cleaned
sufficiently to meet the maximum field train proof blank contribution
to be subtracted from the test results in section 9.9 (0.002g or 2.0
mg). Cleaning glassware prior to the test with soap and water, then
rinsing with tap water, followed by deionized water, acetone, and
finally, hexane is recommended. After cleaning, you should bake
glassware at 300 [deg]C for 6 hours prior to beginning tests at each
source category sampled at a facility. Prior to each sampling run, the
train glassware used to collect condensable PM must be rinsed
thoroughly with acetone, hexane, and then deionized, ultra-filtered
water that contains 1 ppmw (1 mg/L) residual mass or less.
Note: Due the length of most probes, it is not practical to heat
them in an oven. After cleaning the probe liners, it is recommended
to heat the probe to the maximum temperature practical for the probe
sheath for a period of at least 3 hours. Then rinse thoroughly with
acetone, hexane, and deionized, ultra-filtered water.
8.4.1 Condenser and Water Dropout Impinger. Add a vertical
condenser and a water dropout impinger without bubbler tube after the
final probe extension that connects the in-stack or out-of-stack hot
filter assembly with the CPM sampling train. This vertical condenser
must be constructed in a manner that prevents the pooling of the
condensate liquid within the condenser and be capable of cooling the
stack gas to less than or equal to 30 [deg]C (85 [deg]F).
[[Page 42518]]
At the start of the tests, the condenser and water dropout impingers
must be clean, without any water or reagent added.
8.4.2 Backup Impinger. The water dropout impinger is followed by a
modified Greenburg-Smith impinger (backup impinger) with no taper (see
Figure 1 of section 18). Place the water dropout and backup impingers
in an insulated box with water at less than or equal to 30 [deg]C (less
than or equal to 85 [deg]F). At the start of the tests, the backup
impinger must be free of any residual solvents from the recovery or
glassware preparation.
8.4.3 CPM Filter. Place a filter holder with a filter meeting the
requirements in section 7.1.1 after the backup impinger. The connection
between the CPM filter and the moisture trap impinger must include a
thermocouple fitting that provides a leak-free seal between the
thermocouple and the stack gas.
8.4.4 Moisture Traps. You must use a modified Greenburg-Smith
impinger containing 100 ml of water, or the alternative described in
Method 5 of appendix A-3 to part 60, followed by an impinger containing
200 to 300 g of indicating-type silica gel to collect moisture that
passes through the CPM filter. You must maintain the gas temperature
below 20 [deg]C (68 [deg]F) at the exit of the moisture traps.
8.4.5 Weighing of Impingers (Pretest). Weigh each impinger to 0.1
g, including the silica gel impinger prior to train assembly using the
field balance. Record the weights of each impinger on the CPM Impinger
Data Sheet (Figure 4).
8.4.6 Leak-Check (Pretest). Use the procedures outlined in Method 5
of appendix A-3 to part 60, Method 17 of appendix A-6 to part 60, or
Method 201A of appendix M to this part as appropriate to leak check the
entire sampling system. Specifically, perform the following procedures:
8.4.6.1 Sampling train. You must pretest the entire sampling train
for leaks. The pretest leak-check must have a leak rate of not more
than 0.02 actual cubic feet per minute or 4 percent of the average
sample flow during the test run, whichever is less. Additionally, you
must conduct the leak-check at a vacuum equal to or greater than the
vacuum anticipated during the test run. Record the leak-check results
on the field test data sheet (see Figure 5). (Note: Conduct leak-checks
during port changes only as allowed by the filterable particulate
method used with this method.)
8.4.6.2 Pitot tube assembly. After you leak-check the sample train,
perform a leak-check of the pitot tube assembly. Follow the procedures
outlined in section 8.4.1 of Method 5.
8.5 Sampling Train Operation. Operate the sampling train as
described in the filterable particulate sampling method (i.e., Method 5
of appendix A-3 to part 60, Method 17 of appendix A-6 to part 60, or
Method 201A of appendix M to this part) with the following additions or
exceptions:
8.5.1 Impinger and CPM Filter Assembly
8.5.1.1 During sampling, monitor the moisture condensation in the
water dropout impinger and backup impinger. If the accumulated water
from moisture condensation overwhelms (i.e., the water level is more
than approximately one-half the capacity of the water dropout impinger)
the water dropout impinger, or if water accumulates in the backup
impinger sufficient to cover the impinger insert tip, then you must
interrupt the sampling run, leak check the Method 202 portion of the
sampling train, replace the water dropout and/or backup impingers with
new pre-weighed impinger(s), reassemble, leak check the sampling train,
and then resume the sampling run. Weigh the impingers removed from the
sampling train and purge the water collected as soon as practical
following the procedures in section 8.5.3.
8.5.1.2 You must include the weight of the moisture in your
moisture calculation and you must combine the recovered water with the
appropriate sample fraction for subsequent CPM analysis.
8.5.1.3 Use the field data sheet to record the CPM filter
temperature readings at the beginning of each sample time increment and
when sampling is halted. Maintain the CPM filter greater than 20 [deg]C
(greater than 65 [deg]F) but less than or equal to 30 [deg]C (less than
or equal to 85 [deg]F) during sample collection.
8.5.2 Leak-Check (Post-Test). Conduct the leak rate check according
to the filterable particulate sampling method used during sampling.
Conduct the leak-check at a vacuum equal to or greater than the maximum
vacuum achieved during the test run. Record the leak-check results on
the field test data sheet. If the leak rate of the sampling train
exceeds 0.02 actual cubic feet per minute or 4 percent of the average
sampling rate during the test run (whichever is less), then the run is
invalid and you must repeat it.
8.5.3 Weighing of Impingers (Post-test). You must weigh each
impinger to 0.1 g after the completion of the testing and prior to the
post-test nitrogen purge and record these weights on the CPM Impinger
data sheet. Alternatively, you may choose to weigh each impinger after
completion of the post-test nitrogen purge. If this option is chosen,
you must do the following in addition to the procedures of section
8.5.4. Purge the sampling train from the water dropout impinger to the
exhaust of the moisture traps (see Figure 2). You must maintain the
temperature of the moisture traps following the CPM filter to prevent
removal of moisture during the purge. If necessary, add more ice during
the purge to maintain the gas temperature measured at the exit of the
silica gel impinger below 20 [deg]C (68 [deg]F).
Note: You should also note the color of the indicating silica
gel to determine whether it has been completely spent, and record
its condition on the CPM Impinger Data Sheet.
8.5.4 Post-Test Nitrogen Purge. As soon as possible after the post-
test leak-check, conduct the nitrogen purge. If no water was collected
before the CPM filter, then you may skip the remaining purge steps and
proceed with sample recovery (see section 8.5.5). If any water was
collected before the CPM filter, you must purge the CPM sampling train.
8.5.4.1 You may purge the entire CPM sample collection train from
the water dropout impinger through the CPM filter holder outlet or you
may quantitatively transfer the water collected in the water dropout
impinger to the backup impinger and purge only the backup impinger and
the CPM filter and holder (see Figure 3).
8.5.4.2 If you choose to conduct a purge of the entire CPM sampling
train, you must place the dropout impinger insert into the water
dropout impinger, and the impinger tip must extend at least 1
centimeter below the water level of the impinger catch.
8.5.4.3 If the tip of the impinger insert does not extend below the
water level (including the water transferred from the water dropout
impinger if this option was chosen), you must add a measured amount of
degassed, deionized ultra-filtered water that contains 1 ppmw (1 mg/L)
residual mass or less until the impinger tip is at least 1 centimeter
below the surface of the water. You must record the amount of water
added to the water dropout impinger (Vp) (see Figure 4 of section 18)
to correct the moisture content of the effluent gas. (Note: Prior to
use, water must be degassed using a nitrogen purge bubbled through the
water for at least 15 minutes to remove dissolved oxygen.)
8.5.4.4 To perform the nitrogen purge, you must start with no flow
of gas running through the clean purge line and fittings. Connect the
purge nitrogen in-line filter outlet to the input of the
[[Page 42519]]
impinger train to be purged. Increase the nitrogen flow gradually to
avoid over-pressurizing the impinger array. You must purge the CPM
train at a minimum of 14 liters per minute. Record the time (hh:mm),
nitrogen flowrate, and the temperature(s) of the CPM filter and
moisture trap (if applicable) at the start of the nitrogen purge on the
CPM Impinger Data Sheet.
8.5.4.5 During the purge procedure, maintain the gas temperature
measured at the exit of the CPM filter greater than 20 [deg]C (65
[deg]F), but less than or equal to 30 [deg]C (85 [deg]F). Continue the
purge under these conditions for at least 1 hour, recording the CPM
temperature and nitrogen rotameter value every 10 minutes. At the
conclusion of the purge, turn off the nitrogen delivery system. Record
the time (hh:mm) of the purge and the temperature of the CPM filter at
the start of the nitrogen purge on the CPM Impinger Data Sheet.
8.5.5 Sample Recovery
8.5.5.1 Filterable PM samples. Recovery of the filterable PM
samples involves the quantitative transfer of PM according to the
filterable particulate sampling method used (i.e., Method 5 of appendix
A-3 to part 60, Method 17 of appendix A-6 to part 60, or Method 201A of
appendix M to this part).
8.5.5.2 CPM Container #1, Aqueous liquid impinger contents.
Quantitatively transfer liquid from the dropout and the backup
impingers prior to the CPM filter into a clean, leak-proof container
labeled with test identification and ``CPM Container #1, Aqueous Liquid
Impinger Contents.'' Rinse all sampling train components including the
back half of the filterable PM filter holder, the probe extension (if
applicable), condenser, each impinger and the connecting glassware, and
the front half of the CPM filter housing twice with water. Recover the
rinse water, and add it to CPM Container #1. Mark the liquid level on
the container.
8.5.5.3 CPM Container #2, Organic rinses. Follow the water rinses
of the back half of the filterable PM filter holder, probe extension
(if applicable), condenser, each impinger, and all of the connecting
glassware and front half of the CPM filter with an acetone rinse.
Recover the acetone rinse into a clean, leak-proof amber glass
container labeled with test identification and ``CPM Container #2,
Organic Rinses.'' Then repeat the entire rinse procedure with two
rinses of hexane, and save the hexane rinses in the same container as
the acetone rinse (CPM Container #2). Mark the liquid level on the
container.
8.5.5.4 CPM Container #3, CPM filter sample. Use tweezers and/or
clean disposable surgical gloves to remove the filter from the CPM
filter holder. Place the filter in the Petri dish labeled with test
identification and ``CPM Container #3, Filter Sample.''
8.5.5.5 CPM Container #4, Acetone field reagent blank. Take a
minimum of 200 ml of the acetone directly from the wash bottle you used
for sample recovery and place it in a clean, leak-proof amber glass
container labeled with test identification and ``CPM Container #4,
Acetone Field Reagent Blank'' (see section 11.2.6 for analysis). Mark
the liquid level on the container. Collect one acetone field reagent
blank from each lot of acetone used for the test.
8.5.5.6 CPM Container #5, Water field reagent blank. Take a minimum
of 200 ml of the water directly from the wash bottle you used for
sample recovery and place it in a clean, leak-proof container labeled
with test identification and ``CPM Container #5, Water Field Reagent
Blank'' (see section 11.2.7 for analysis). Mark the liquid level on the
container. Collect one water field reagent blank from each lot of water
used for the test.
8.5.5.7 CPM Container #6, Hexane field reagent blank. Take a
minimum of 200 ml of the hexane directly from the wash bottle you used
for sample recovery and place it in a clean, leak-proof amber glass
container labeled with test identification and ``CPM Container #6,
Hexane Field Reagent Blank'' (see section 11.2.8 for analysis). Mark
the liquid level on the container. Collect one hexane field reagent
blank from each lot of hexane used for the test.
8.5.5.8 Field train proof blank. To demonstrate the cleanliness of
sampling train glassware, you must prepare a full sampling train to
serve as a field train proof blank just as it would be prepared for
sampling, including the filterable PM method front half, probe
extension (if applicable), condenser, impingers, CPM filter, and
transfer line. Transport and assemble the field train proof blank
sample train to the sampling location and perform a pre-test leak check
as if it were an actual sample train. Hold this train at the sampling
location for the same amount of time as a test run unless otherwise
specified by the Administrator, and perform a post-test leak check on
this train at the end of the actual test sampling time. After the post-
test leak check, you must conduct a nitrogen purge of the field train
proof blank sample as specified in section 8.5.4. For the nitrogen
purge, you must add 100 ml of deionized ultra-filtered water and
replicate the nitrogen purge procedures that you will use for the test
runs. After conducting the nitrogen purge, recover the field train
proof blank as described in sections 8.5.5.8.1 through 8.5.5.8.3.
8.5.5.8.1 CPM Container #7, Field train proof blank, inorganic
rinses. Rinse the probe extension, condenser, each impinger and the
connecting glassware, and the front half of the CPM filter housing
twice with water. Recover the rinse water and place it in a clean,
leak-proof container labeled with test identification and ``CPM
Container #7, Field Train Proof Blank, Inorganic Rinses.'' Mark the
liquid level on the container.
8.5.5.8.2 CPM Container #8, Field train proof blank, organic
rinses. Follow the water rinse of the probe extension, condenser, each
impinger and the connecting glassware, and the front half of the CPM
filter housing with an acetone rinse. Recover the acetone rinse into a
clean, leak-proof container labeled with test identification and ``CPM
Container #8, Field Train Proof Blank, Organic Rinses.'' Then repeat
the entire rinse procedure with two rinses of hexane and recover the
hexane rinses into the same container as the acetone rinse (CPM
Container #10). Mark the liquid level on the container.
8.5.5.8.3 CPM Container #9, Field train proof blank, filter sample.
Use tweezers and/or clean disposable surgical gloves to remove the
filter from the CPM filter holder. Place the filter in the Petri dish
labeled with test identification and ``CPM Container #9, Field Train
Proof Blank, Filter Sample.''
8.5.6 Sample Transport procedures. Containers must remain in an
upright position at all times during shipping. You do not have to ship
the containers under dry or blue ice. However, samples should be
maintained at or below 30 [deg]C (85 [deg]F) during shipping.
9.0 Quality Control
9.1 Daily Quality Checks. You must perform daily quality checks of
field log notebooks and data entries and calculations using data
quality indicators from this method and your site-specific test plan.
You must review and evaluate recorded and transferred raw data,
calculations, and documentation of testing procedures. You must initial
or sign log notebook pages and data entry forms that were reviewed.
9.2 Calculation Verification. Verify the calculations by
independent, manual checks. You must flag any suspect data and identify
the nature of the problem and potential effect on data quality. After
you complete the test, prepare a data summary and compile all the
calculations and raw data sheets.
9.3 Conditions. You must document data and information on the
process
[[Page 42520]]
unit tested, the particulate control system used to control emissions,
any non-particulate control system that may affect particulate
emissions, the sampling train conditions, and weather conditions.
Discontinue the test if the operating conditions may cause non-
representative particulate emissions.
9.4 Field Balance Calibration Check. Record the results of the
calibration check procedures on field balances each day that they are
used as required in section 10.3.
9.5 Glassware. Use class A volumetric glassware for titrations, or
calibrate your equipment against NIST-traceable glassware.
9.6 Laboratory Analytical Balance
9.6.1 Maintain the location of the analytical balance (i.e.,
weighing room) at 20 [deg]C 3 [deg]C (68[emsp14][deg]F
5[emsp14][deg]F).
9.6.2 Maintain the location the analytical balance (i.e., weighing
room) at 35 to 50 percent relative humidity. Alternatively, it is
acceptable for the percent relative humidity to be less than 35
percent. In either case, you should maintain the relative humidity
within 10 percent relative humidity for sampling weighings.
9.6.3 Record and report the temperature and relative humidity of
the analytical balance location for each measurement performed.
9.6.4 Calibration Check. Record the calibration check of your
laboratory analytical balance at least once each day that you weigh CPM
samples. Audit the balance using at least one ASTM E617-13 Class 2
tolerance (or better) calibration weight, within 1 g to 5 g of the
weight of the sample plus container you will be weighing.
9.7 Laboratory Reagent Blanks. You should analyze blanks of water,
acetone, and hexane used for field recovery and sample analysis.
Analyze and report at least one sample (500 ml minimum) of each lot of
reagents that you plan to use for sample recovery and analysis. These
blanks are not required by the test method, but analyzing reagent
blanks before field use is recommended to verify low reagent blank
concentrations.
9.8 Field Reagent Blanks. You must analyze and report the results
of each lot of reagent used for the field test.
9.9 Field Train Proof Blank. You must recover a minimum of one
field train proof blank for each new source category at a single
facility using glassware prepped according to section 8.4. You must
assemble the sampling train as it will be used for testing, including
the filterable PM method front half, CPM filter, and transfer line. You
must prepare and recover the field train proof blank as described in
section 8.5.5.8. From each field sample weight, you will subtract the
condensable particulate mass you determine with this field train proof
blank or 0.002 g (2.0 mg), whichever is less, unless otherwise
specified by the regulatory authority.
10.0 Calibration and Standardization
Maintain a field log notebook of all condensable particulate
sampling and analysis calibrations. Include copies of the relevant
portions of the calibration and field logs in the final test report.
10.1 Thermocouple Calibration. You must calibrate the thermocouples
using the procedures described in section 10.3.1 of Method 2 of
appendix A-1 to part 60 or Alternative Method 2, Thermocouple
Calibration (ALT-011) (https://www.epa.gov/emc). Calibrate each
temperature sensor at a minimum of three points over the anticipated
range of use against a NIST-traceable thermometer. Alternatively, a
reference thermocouple and potentiometer calibrated against NIST
standards can be used.
10.2 Ammonium Hydroxide. The 0.1 N NH4OH used for
titrations in this method is made as follows: Add 7 ml of concentrated
(14.8 M) NH4OH to 1 liter of water. Standardize against
certified standard of 0.1 N H2SO4, and calculate
the exact normality using a procedure parallel to that described in
section 10.5 of Method 6 of appendix A-4 to 40 CFR part 60.
Alternatively, purchase 0.1 N NH4OH that has been
standardized against a NIST reference material. Record the normality on
the CPM Work Table (see Figure 6 of section 18).
10.3 Field Balance Calibration Check. Check the calibration of the
balance used to weigh impingers with a weight that is at least 500 g or
within 50 g of a loaded impinger. The weight must be ASTM E617-13
``Standard Specification for Laboratory Weights and Precision Mass
Standards'' Class 6 (or better). Daily, before use, the field balance
must measure the weight within 0.5 g of the certified mass
and record the results. If the balance calibration check fails, perform
corrective measures and repeat the check before using balance.
10.4 Analytical Balance Calibration. Perform a multipoint
calibration (at least five points spanning the operational range) of
the analytical balance before the first use, and semiannually
thereafter. The calibration of the analytical balance must be conducted
using ASTM E617-13 ``Standard Specification for Laboratory Weights and
Precision Mass Standards'' Class 2 (or better) tolerance weights. Audit
the balance each day it is used for gravimetric measurements by
weighing at least one ASTM E617-13 Class 2 tolerance (or better)
calibration weight that corresponds to 50 to 150 percent of the weight
of one filter or between 1 g and 5 g and record the results. If the
scale cannot reproduce the value of the calibration weight to within
0.5 mg of the certified mass, perform corrective measures and conduct
the multipoint calibration before use.
11.0 Analytical Procedures
11.1 Analytical Data Sheets
(a) Record the filterable particulate field data on the appropriate
(i.e., Method 5, 17, or 201A) analytical data sheets. Record the
condensable particulate data on the CPM Work Table (see Figure 7 of
section 18).
(b) Visually inspect the liquid level mark on each sample container
and record on the CPM Work Table whether leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the
Administrator, to correct the final results.
11.2 Condensable PM Analysis. See the flow chart in Figure 8 of
section 18 for the steps to process and combine fractions from the CPM
train.
11.2.1 Container #3, CPM Filter Sample. Extract the CPM filter as
described in this section.
11.2.1.1 Extract the water soluble (aqueous or inorganic) CPM from
the CPM filter by placing it into a clean extraction container or
flask. Add sufficient deionized, ultra-filtered water to cover the
filter (e.g., 10 ml of water). Place the extractor container into a
sonication bath and extract the water-soluble material for a minimum of
2 minutes. Combine the aqueous extract with the contents of Container
#1. Repeat this extraction step twice for a total of three extractions.
11.2.1.2 Extract the organic soluble CPM from the CPM filter by
adding sufficient hexane to cover the filter (e.g., 10 ml of hexane).
Place the extractor tube into a sonication bath and extract the organic
soluble material for a minimum of two minutes. Combine the organic
extract with the contents of Container #2. Repeat this extraction step
twice for a total of three extractions.
11.2.2 CPM Container #1, Aqueous Liquid Impinger Contents. Analyze
the water-soluble CPM in Container #1 as described in this section.
Place the contents of Container #1 into a separatory funnel. Add
approximately 30 ml of hexane to the funnel, mix well, and pour off the
upper organic phase. Repeat this procedure twice with 30 ml
[[Page 42521]]
of hexane each time combining the organic phase from each extraction.
Each time, leave a small amount of the organic/hexane phase in the
separatory funnel, ensuring that no water is collected in the organic
phase. This extraction should yield about 90 ml of organic extract.
Combine the organic extract from Container #1 with the organic train
rinse in Container #2.
11.2.2.1 Determine the inorganic fraction weight. Transfer the
aqueous fraction from the extraction to a clean 500 ml or smaller
beaker. Evaporate to no less than 10 ml liquid on a hot plate or in the
oven at 105 [deg]C and allow to dry at room temperature (not to exceed
30 [deg]C (85[emsp14][deg]F)). Following evaporation, desiccate the
residue for 24 hours in a desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least 6 hours to a constant weight.
(See section 3.0 for a definition of constant weight.) Report results
to the nearest 0.1 mg on the CPM Work Table (see Figure 6 of section
18) and proceed directly to section 11.2.3. If the residue cannot be
weighed to constant weight, re-dissolve the residue in 100 ml of
deionized distilled ultra-filtered water that contains 1 ppmw (1 mg/L)
residual mass or less and continue to section 11.2.2.2.
11.2.2.2 You must ensure that water and volatile acids have
completely evaporated before neutralizing nonvolatile acids in the
sample. Only after failure to reach constant weight and rehydration,
per section 11.2.2.1, use titration to neutralize acid in the sample
and remove water of hydration. Calibrate the pH meter with the neutral
and acid buffer solutions immediately prior to the titration of the
samples. Then titrate the sample with 0.1 N NH4OH to a pH of
7.0, as indicated by the pH meter. Record the volume of titrant used on
the CPM Work Table (see Figure 6 of section 18).
11.2.2.3 Using a hot plate or an oven at 105 [deg]C, evaporate the
aqueous phase to approximately 10 ml. Quantitatively transfer the
beaker contents to a clean, 50 ml pre-tared weighing container and
evaporate to dryness at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least 6
hours to a constant weight. (See section 3.0 for a definition of
constant weight.) Report results to the nearest 0.1 mg on the CPM Work
Table (see Figure 6 of section 18).
11.2.2.4 Calculate the correction factor to subtract the
NH4\+\ retained in the sample using Equation 1 in section
12.
11.2.3 CPM Container #2, Organic Fraction Weight Determination.
Analyze the organic soluble CPM in Container #2 as described in this
section. Place the organic phase in a clean glass beaker. Evaporate the
organic extract at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood to not less than
10 ml. Quantitatively transfer the beaker contents to a clean 50 ml
pre-tared weighing container and evaporate to dryness at room
temperature (not to exceed 30 [deg]C (85[emsp14][deg]F)) and pressure
in a laboratory hood. Following evaporation, desiccate the organic
fraction for 24 hours in a desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least 6 hours to a constant weight
(i.e., less than or equal to 0.5 mg change from previous weighing), and
report results to the nearest 0.1 mg on the CPM Work Table (see Figure
6 of section 18).
11.2.4 Container #4, Acetone Field Reagent Blank. Use 200 ml of
acetone from the blank container used for this analysis. Transfer 200
ml of the acetone field reagent blank to a clean 250 ml beaker.
Evaporate the acetone at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood to approximately
10 ml. Quantitatively transfer the beaker contents to a clean pre-tared
weighing container, and evaporate to dryness at room temperature (not
to exceed 30 [deg]C (85[emsp14][deg]F)) and pressure in a laboratory
hood. Following evaporation, desiccate the residue for 24 hours in a
desiccator containing anhydrous calcium sulfate. Weigh at intervals of
at least 6 hours to a constant weight (i.e., less than or equal to 0.5
mg change from previous weighing), and report results to the nearest
0.1 mg on Figure 5 of section 19.
11.2.5 Container #5, Water Field Reagent Blank. Use 200 ml of the
water from the blank container for this analysis. Transfer the water to
a clean 250 ml beaker, and evaporate to approximately 10 ml liquid in
the oven at 105 [deg]C. Quantitatively transfer the beaker contents to
a clean 50 ml pre-tared weighing container and evaporate to dryness at
room temperature (not to exceed 30 [deg]C (85[emsp14][deg]F)) and
pressure in a laboratory hood. Following evaporation, desiccate the
residue for 24 hours in a desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least 6 hours to a constant weight
(i.e., less than or equal to 0.5 mg change from previous weighing) and
report results to the nearest 0.1 mg on Figure 5 of section 18.
11.2.6 Container #6, Hexane Field Reagent Blank. Use 200 ml of
hexane from the blank container for this analysis. Transfer 150 ml of
the hexane to a clean 250 ml beaker. Evaporate the hexane at room
temperature (not to exceed 30 [deg]C (85[emsp14][deg]F)) and pressure
in a laboratory hood to approximately 10 ml. Quantitatively transfer
the beaker contents to a clean 50 ml pre-tared weighing container and
evaporate to dryness at room temperature (not to exceed 30 [deg]C
(85[emsp14][deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least 6
hours to a constant weight (i.e., less than or equal to 0.5 mg change
from previous weighing), and report results to the nearest 0.1 mg on
Figure 5 of section 18.
12.0 Calculations and Data Analysis
12.1 Nomenclature. Report results in International System of Units
(SI units) unless the regulatory authority for testing specifies
English units. The following nomenclature is used.
[Delta]H@ = Pressure drop across orifice at flow rate of
0.75 SCFM at standard conditions, inches of water column (Note
Specific to each orifice and meter box).
17.03 = mg/milliequivalents for ammonium ion.
ACFM = Actual cubic feet per minute.
Ccpm = Concentration of the condensable PM in the stack
gas, dry basis, corrected to standard conditions, milligrams/dry
standard cubic foot.
mc = Mass of the NH4\+\ added to sample to
form ammonium sulfate, mg.
mcpm = Mass of the total condensable PM, mg.
mfb = Mass of total CPM in field train proof blank, mg.
mg = Milligrams.
mg/dscf = Milligrams per dry standard cubic foot.
mg/L = Milligrams per liter.
mi = Mass of inorganic CPM, mg.
mib = Mass of inorganic CPM in field train proof blank,
mg.
mo = Mass of organic CPM, mg.
mob = Mass of organic CPM in field train blank, mg.
mr = Mass of dried sample from inorganic fraction, mg.
N = Normality of ammonium hydroxide titrant.
ppmv = Parts per million by volume.
ppmw = Parts per million by weight.
Vm(std) = Volume of gas sample measured by the dry gas
meter, corrected to standard conditions, dry standard cubic meter
(dscm) or dry standard cubic foot (dscf) as defined in Equation 5-1
of Method 5.
Vt = Volume of NH4OH titrant, ml.
Vp = Volume of water added during train purge.
12.2 Calculations. Use the following equations to complete the
calculations required in this test method. Enter the appropriate
results from these calculations on the CPM Work Table (see Figure 7 of
section 18).
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12.2.1 Mass of ammonia correction. Correction for ammonia added
during titration of 100 ml aqueous CPM sample. This calculation assumes
no waters of hydration.
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9.9, the mass of the field train proof blank, mfb, shall not
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(Eq. 2)12.2.3 Mass of Inorganic CPM (mg).
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(Eq. 3)12.2.4 Total Mass of CPM (mg).
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(Eq. 4)12.2.5 Concentration of CPM (mg/dscf).
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12.3 Emissions Test Report. You must prepare a test report
following the guidance in EPA Guideline Document 043.
13.0 Method Performance
A field evaluation (NCASI 2017) of Method 202 incorporating Best
Practices showed that the detection limit was 1.6 for total CPM;
consisting of approximately 1.0 mg for organic CPM and approximately
0.6 mg for inorganic CPM. This field evaluation also demonstrated that
the expected blank value of the field train proof blank was less than
1.8 mg.
14.0 Pollution Prevention
[Reserved]
15.0 Waste Management
Solvent and water are evaporated in a laboratory hood during
analysis. No liquid waste is generated in the performance of this
method. Organic solvents used to clean sampling equipment should be
managed as Resource Conservation and Recovery Act organic waste.
16.0 Alternative Procedures
16.1 Alternative Field Train Proof Blank Procedure. The following
procedure may be utilized with approval by the regulatory authority at
stationary sources with environments with significant ambient PM
concentrations that could positively bias the results of the Method 202
samples collected. This procedure would permit you to subtract up to
0.0039 g (3.9 mg) from the measured condensable particulate mass.
16.1.1 The facility must request this alternative prior to the test
program, and the request must be approved by the regulatory authority
prior to the testing. The request may include the following elements:
(1) Documented adherence to the Best Practices for Method 202 by
the tester. This documentation may include:
(a) Tester's Method 202 standard operating procedure (SOP);
(b) Residual mass of the laboratory reagent blanks (Reagent ID,
Manufacturer, Lot Number);
(c) Tester-specific Method Detection Limit;
(d) Training records.
(2) Justification by the facility that the environment around the
sampling location is likely to bias the CPM results. This justification
may include:
(a) Schematic of the facility identifying locations that may
contribute to environmental bias;
(b) Ambient PM concentration (mg/m\3\);
(c) Previous test results (i.e., field train proof blank results).
16.1.2 Upon the regularity authority approval, you will recover a
minimum of two field train proof blanks for each source category tested
at the subject facility using glassware prepped according to section
8.4 of this method. You must perform the field train proof blank
evaluations as described in section 9.9 of this method.
16.1.3 From each field sample weight, you will subtract the average
condensable particulate mass you determine with all of the duplicate
field train proof blank trains or 0.0039 g (3.9 mg), whichever is less
unless the difference between highest and lowest values of the field
train proof blanks is >1.0 mg. If the agreement is >1.0 mg, then you
must subtract the lowest
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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 https://www3.epa.gov/ttn/emc/approalt/alt-011.pdf.
17.0 References
(1) Commonwealth of Pennsylvania, Department of Environmental
Resources. 1960. Chapter 139, Sampling and Testing (Title 25, Rules
and Regulations, part I, Department of Environmental Resources,
Subpart C, Protection of Natural Resources, Article III, Air
Resources). January 8, 1960.
(2) DeWees, W.D. and K.C. Steinsberger. 1989. ``Method Development
and Evaluation of Draft Protocol for Measurement of Condensable
Particulate Emissions.'' Draft Report. November 17, 1989.
(3) DeWees, W.D., K.C. Steinsberger, G.M. Plummer, L.T. Lay, G.D.
McAlister, and R.T. Shigehara. 1989. ``Laboratory and Field
Evaluation of EPA Method 5 Impinger Catch for Measuring Condensable
Matter from Stationary Sources.'' Paper presented at the 1989 EPA/
AWMA International Symposium on Measurement of Toxic and Related Air
Pollutants. Raleigh, North Carolina. May 1-5, 1989.
(4) Electric Power Research Institute (EPRI). 2008. ``Laboratory
Comparison of Methods to Sample and Analyze Condensable PM.'' EPRI
Agreement EP-P24373/C11811 Condensable Particulate Methods: EPRI
Collaboration with EPA, October 2008.
(5) Nothstein, Greg. Masters Thesis. University of Washington.
Department of Environmental Health. Seattle, Washington.
(6) Richards, J., T. Holder, and D. Goshaw. 2005. ``Optimized Method
202 Sampling Train to Minimize the Biases Associated with Method 202
Measurement of Condensable PM Emissions.'' Paper presented at Air &
Waste Management Association Hazardous Waste Combustion Specialty
Conference. St. Louis, Missouri. November 2-3, 2005.
(7) Texas Air Control Board, Laboratory Division. 1976.
``Determination of Particulate in Stack Gases Containing Sulfuric
Acid and/or Sulfur Dioxide.'' Laboratory Methods for Determination
of Air Pollutants. Modified December 3, 1976.
(8) Puget Sound Air Pollution Control Agency, Engineering Division.
1983. ``Particulate Source Test Procedures Adopted by Puget Sound
Air Pollution Control Agency Board of Directors.'' Seattle,
Washington. August 11, 1983.
(9) U.S. Environmental Protection Agency, Federal Reference Methods
1 through 5 and Method 17, 40 CFR 60, appendix A-1 through A-3 and
A-6.
(10) U.S. Environmental Protection Agency. 2008. ``Evaluation and
Improvement of Condensable PM Measurement,'' EPA Contract No. EP-D-
07-097, Work Assignment 2-03, October 2008.
(11) U.S. Environmental Protection Agency. 2005. ``Laboratory
Evaluation of Method 202 to Determine Fate of SO2 in
Impinger Water,'' EPA Contract No. 68-D-02-061, Work Assignment 3-
14, September 30, 2005.
(12) U.S. Environmental Protection Agency. 2010. ``Field Valuation
of an Improved Method for Sampling and Analysis of Filterable and
Condensable Particulate Matter.'' Office of Air Quality Planning and
Standards, Sector Policy and Program Division Monitoring Policy
Group. Research Triangle Park, NC 27711.
(13) Wisconsin Department of Natural Resources. 1988. Air Management
Operations Handbook, Revision 3. January 11, 1988.
(14) U.S. Environmental Protection Agency. 2016. ``EPA Method 202
Best Practices Handbook.'' Office of Air Quality Planning and
Standards, Air Quality Assessment Division, Measurements Technology
Group. Research Triangle Park, NC 27711.
(15) National Council for Air and Stream Improvement. Research Brief
submitted to the US EPA. May 25, 2017. ``Method 202 Zero Bias Study
When Incorporating Draft Best Practices Developed by the US EPA.''
NCASI Southern Research Center. Newberry, Florida 32669.
18.0 Tables, Diagrams, Flowcharts, and Validation Data
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[FR Doc. 2017-18425 Filed 9-7-17; 8:45 am]
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