Methods for Measurement of Filterable PM10, 80118-80172 [2010-30847]
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Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Part 51
[EPA–HQ–OAR–2008–0348; FRL–9236–2]
RIN 2060–AO58
Methods for Measurement of Filterable
PM10 and PM2.5 and Measurement of
Condensable PM Emissions From
Stationary Sources
Environmental Protection
Agency (EPA).
ACTION: Final rule.
AGENCY:
This action promulgates
amendments to Methods 201A and 202.
The final amendments to Method 201A
add a particle-sizing device to allow for
sampling of particulate matter with
mean aerodynamic diameters less than
or equal to 2.5 micrometers (PM2.5 or
fine particulate matter). The final
amendments to Method 202 revise the
sample collection and recovery
procedures of the method to reduce the
formation of reaction artifacts that could
lead to inaccurate measurements of
condensable particulate matter.
Additionally, the final amendments to
Method 202 eliminate most of the
hardware and analytical options in the
existing method, thereby increasing the
precision of the method and improving
the consistency in the measurements
obtained between source tests
performed under different regulatory
authorities.
This action also announces that EPA
is taking no action to affect the already
established January 1, 2011 sunset date
for the New Source Review (NSR)
transition period, during which EPA is
not requiring that State NSR programs
address condensable particulate matter
emissions.
DATES: This final action is effective on
January 1, 2011.
ADDRESSES: EPA has established a
docket for this action under Docket ID
No. EPA–HQ–OAR–2008–0348. All
documents are listed in the https://www.
regulations.gov index. Although listed
in the index, some information is not
publicly available, e.g., confidential
business information (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 form. Publicly available docket
materials are available either
electronically at https://www.regulations.
gov or in hard copy at the EPA Docket
Center EPA/DC, EPA West, Room 3334,
1301 Constitution Ave., NW.,
Washington, DC. The Public Reading
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SUMMARY:
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Room 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 Center is (202) 566–1742.
FOR FURTHER INFORMATION CONTACT: For
general information, contact Ms.
Candace Sorrell, U.S. EPA, Office of Air
Quality Planning and Standards, Air
Quality Assessment Division,
Measurement Technology Group (E143–
02), Research Triangle Park, NC 27711;
telephone number: (919) 541–1064; fax
number; (919) 541–0516; e-mail address:
sorrell.candace@epa.gov. For technical
questions, contact Mr. Ron Myers, U.S.
EPA, Office of Air Quality Planning and
Standards, Sector Policies and Programs
Division, Measurement Policy Group
(D243–05), Research Triangle Park, NC
27711; telephone number: (919) 541–
5407; fax number: (919) 541–1039;
e-mail address: myers.ron@epa.gov.
SUPPLEMENTARY INFORMATION:
Acronyms and Abbreviations. The
following acronyms and abbreviations
are used in this document.
Dpmax maximum velocity pressure
Dpmin minimum velocity pressure
μm micrometers
ASTM American Society for Testing and
Materials
AWMA Air and Waste Management
Association
CAA Clean Air Act
CBI confidential business information
CCM Controlled Condensation Method
CPM condensable PM
DOP dioctyl phthalate
DOT Department of Transportation
DQO data quality objective
MSHA Mine Safety and Health
Administration
NAAQS National Ambient Air Quality
Standards
NSR New Source Review
NTTAA National Technology Transfer and
Advancement Act of 1995
OSHA Occupational Safety and Health
Administration
PCB polychlorinated biphenyl
PM particulate matter
PM10 particulate matter less than or equal to
10 micrometers
PM2.5 particulate matter less than or equal
to 2.5 micrometers
ppmw parts per million by weight
PTFE polytetrafluoropolymer
RCRA Resource Conservation and Recovery
Act
RFA Regulatory Flexibility Act
SBA Small Business Administration
SIP State Implementation Plan
SO2 sulfur dioxide
TDS total dissolved solids
TTN Technology Transfer Network
UMRA Unfunded Mandates Reform Act
www World Wide Web
The information in this preamble is
organized as follows:
I. General Information
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A. Does this action apply to me?
B. Where can I obtain a copy of this action
and other related information?
C. What is the effective date?
D. Judicial Review
II. Background
A. Why is EPA issuing this final action?
B. Particulate Matter National Ambient Air
Quality Standards
C. Measuring PM Emissions
1. Method 201A
2. Method 202
III. Summary of Changes Since Proposal
A. Method 201A
B. Method 202
C. How will the final amendments to
methods 201A and 202 affect existing
emission inventories, emission
standards, and permit programs?
IV. Summary of Final Methods
A. Method 201A
B. Method 202
V. Summary of Public Comments and
Responses
A. Method 201A
B. Method 202
C. Conditional Test Method 039 (Dilution
Method)
VI. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory
Planning and Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act
D. Unfunded Mandates Reform Act
E. Executive Order 13132: Federalism
F. Executive Order 13175: Consultation
and Coordination With Indian Tribal
Governments
G. Executive Order 13045: Protection of
Children From Environmental Health
and Safety Risks
H. Executive Order 13211: Actions
Concerning Regulations That
Significantly Affect Energy Supply,
Distribution, or Use
I. National Technology Transfer and
Advancement Act
J. Executive Order 12898: Federal Actions
To Address Environmental Justice in
Minority Populations and Low-Income
Populations
K. Congressional Review Act
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 total particulate
matter (PM), total PM with mean
aerodynamic diameters less than or
equal to 10 micrometers (μm) (PM10), or
total PM2.5, where EPA Method 202 is
incorporated as a component of the
applicable test method.
In addition, this action applies to you
if federal, State, or local agencies take
certain additional independent actions.
For example, this action applies to
sources through actions by State and
local agencies that implement
condensable PM (CPM) control
measures to attain the National Ambient
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Air Quality Standards (NAAQS) for
PM2.5 and specify the use of Method 202
to demonstrate compliance with the
control measures. State and local
agencies that specify the use of Method
201A or 202 would have to implement
the following: (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 Method 201A or 202 (or an
incorporated method based upon
Method 201A or 202). This action also
applies to stationary sources that are
required to meet new applicable CPM
requirements established through
federal or State permits or rules, such as
Category
NAICS a
Industry ............................................
332410 ...........................................
332410 ...........................................
332410 ...........................................
324110 ...........................................
562213 ...........................................
322110 ...........................................
325188 ...........................................
327310 ...........................................
327410 ...........................................
211111, 212111, 212112, 212113
331312, 331314 .............................
331111, 331513 .............................
321219, 321211, 321212 ..............
a North
New Source Performance Standards and
New Source Review (NSR), which
specify the use of Method 201A or 202
to demonstrate compliance with the
control measures.
The source categories and entities
potentially affected include, but are not
limited to, the following:
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.
B. Where can I obtain a copy of this
action and other related information?
In addition to being available in the
docket, an electronic copy of these final
rules are also available on the World
Wide Web (https://www.epa.gov/ttn/)
through the Technology Transfer
Network (TTN). Following the
Administrator’s signature, a copy of
these final rules will be posted on the
TTN’s policy and guidance page for
newly proposed or promulgated rules at
https://www.epa.gov/ttn/oarpg. The TTN
provides information and technology
exchange in various areas of air
pollution control.
C. What is the effective date?
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The final rule amendments are
effective on January 1, 2011. Section
553(d) of the Administrative Procedure
Act (APA), 5 U.S.C. Chapter 5, generally
provides that rules may not take effect
earlier than 30 days after they are
published in the Federal Register. EPA
is issuing this final rule under section
307(d)(1) of the Clean Air Act, which
states: ‘‘The provisions of section 553
through 557 * * * of Title 5 shall not,
except as expressly provided in this
section, apply to actions to which this
subsection applies.’’ Thus, section
553(d) of the APA does not apply to this
rule. EPA is nevertheless acting
consistently with the purposes
underlying APA section 553(d) in
making this rule effective on January 1,
2011. Section 5 U.S.C. 553(d)(3) allows
an effective date less than 30 days after
publication ‘‘as otherwise provided by
the agency for good cause found and
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published with the rule.’’ As explained
below, EPA finds that there is good
cause for these rules to become effective
on or before January 1, 2011, even if this
date is not 30 days from date of
publication in the Federal Register.
While this action is being signed prior
to December 1, 2010, there may be a
delay in the publication of this rule as
it contains many complex diagrams,
equations, and charts, and is relatively
long in length. The purpose of the
30-day waiting period prescribed in 5
U.S.C. 553(d) is to give affected parties
a reasonable time to adjust their
behavior and prepare before the final
rule takes effect. Where, as here, the
final rule will be signed and made
available on the EPA website more than
30 days before the effective date, but
where the publication may be delayed
due to the complexity and length of the
rule, that purpose is still met. Moreover,
since permitting authorities and
regulated entities may need to rely on
the methods described in these rules to
carry out requirements of the SIP and
NSR implementation rules that become
effective on January 1, 2011 (see section
III.C, infra), there would be unnecessary
regulatory confusion if a publication
delay caused this rule to become
effective after January 1, 2011.
Accordingly, we find good cause exists
to make this rule effective on or before
January 1, 2011, consistent with the
purposes of 5 U.S.C. 553(d)(3).1
1 We
recognize that this rule could be published
at least 30 days before January 1, 2011, which
would negate the need for this good cause finding,
and we plan to request expedited publication of this
rule in order to decrease the likelihood of a
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D. Judicial Review
Under section 307(b)(1) of the Clean
Air Act (CAA), judicial review of this
final action is available only by filing a
petition for review in the United States
Court of Appeals for the District of
Columbia Circuit by February 22, 2011.
Under CAA section 307(b)(2), the
requirements established by this action
may not be challenged separately in any
civil or criminal proceedings brought by
EPA to enforce these requirements.
Section 307(d)(7)(B) of the CAA
further provides that ‘‘[o]nly an
objection to a rule or procedure which
was raised with reasonable specificity
during the period for public comment
(including any public hearing) may be
raised during judicial review.’’ This
section also provides a mechanism for
EPA to convene a proceeding for
reconsideration, ‘‘[i]f the person raising
an objection can demonstrate to EPA
that it was impracticable to raise such
objection within [the period for public
comment] or if the grounds for such
objection arose after the period for
public comment (but within the time
specified for judicial review) and if such
objection is of central relevance to the
outcome of the rule.’’ Any person
seeking to make such a demonstration to
us should submit a Petition for
Reconsideration to the Office of the
Administrator, U.S. EPA, Room 3000,
publication delay. However, as we cannot know the
date of publication in advance of signing this rule,
we are proceeding with this good cause finding for
an effective date on or before January 1, 2011, in
an abundance of caution in order to avoid the
unnecessary regulatory confusion noted above.
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Ariel Rios Building, 1200 Pennsylvania
Ave., NW., Washington, DC 20460, with
a copy to both the person(s) listed in the
preceding FOR FURTHER INFORMATION
CONTACT section, and the Associate
General Counsel for the Air and
Radiation Law Office, Office of General
Counsel (Mail Code 2344A), U.S. EPA,
1200 Pennsylvania Ave., NW.,
Washington, DC 20460.
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II. Background
A. Why is EPA issuing this final action?
Section 110 of the CAA, 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 (SIP) 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 inventories and
analyses used in the State’s attainment
demonstrations must consider PM10 and
PM2.5 emissions from stationary sources
that are significant contributors of
primary PM10 and PM2.5 emissions.
Primary or direct 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.
Appendix A to subpart A of 40 CFR
part 51 (Requirements for Preparation,
Adoption, and Submittal of
Implementation Plans) defines primary
PM10 and PM2.5 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
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, EPA
previously developed and promulgated
Method 201A (Determination of PM10
Emissions (Constant Sampling Rate
Procedure)) and Method 202
(Determination of Condensable
Particulate Emissions from Stationary
Sources) in 40 CFR part 51, appendix M
(Recommended Test Methods for State
Implementation Plans).
On April 17, 1990 (56 FR 65433), EPA
promulgated Method 201A in appendix
M of 40 CFR part 51 to provide a test
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method for measuring filterable PM10
emissions from stationary sources. In
EPA Method 201A, a gas sample is
extracted at a constant flow rate through
an in-stack sizing device that directs
particles with aerodynamic diameters
less than or equal to 10 μm to a filter.
The particulate mass collected on the
filter is determined gravimetrically after
removal of uncombined water.
On December 17, 1991 (56 FR 65433),
EPA promulgated Method 202 in
appendix M of 40 CFR part 51 to
provide a test method for measuring
CPM from stationary sources. Method
202 uses 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 used by State and local
regulatory entities at the time Method
202 was being developed.
In this action, we are finalizing
amendments to Methods 201A and 202
to improve the measurement of fine PM
emissions. For Method 201A, the final
amendments add a particle-sizing
device to allow for sampling of PM2.5
emissions. For Method 202, the final
amendments will (1) revise the sample
collection and recovery procedures of
the method to reduce the potential for
formation of reaction artifacts that are
not related to the primary emission of
CPM from the source but may be
counted erroneously as CPM when
using Method 202, and (2) eliminate
most of the hardware and analytical
options in the existing method. These
changes increase the precision of
Method 202 and improve the
consistency in the measurements
obtained between source tests
performed under different regulatory
authorities.
B. Particulate Matter National Ambient
Air Quality Standards
Section 108 and 109 of the CAA
govern the establishment and revision of
the NAAQS. Section 108 of the CAA (42
U.S.C. 7408) directs the Administrator
to identify and list ‘‘air pollutants’’ that
‘‘in his judgment, may reasonably be
anticipated to endanger public health
and welfare’’ and whose ‘‘presence
* * * in the ambient air results from
numerous or diverse mobile or
stationary sources’’ and to issue air
quality criteria for those that are listed.
Air quality criteria are intended to
‘‘accurately reflect the latest scientific
knowledge useful in indicating the kind
and extent of identifiable effects on
public health or welfare which may be
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expected from the presence of [a]
pollutant in ambient air * * *.’’ Section
109 of the CAA (42 U.S.C. 7409) directs
the Administrator to propose and
promulgate primary and secondary
NAAQS for pollutants listed under CAA
section 108 to protect public health and
welfare, respectively. Section 109 of the
CAA also requires review of the NAAQS
at 5-year intervals and that an
independent scientific review
committee ‘‘shall complete a review of
the criteria * * * and the national
primary and secondary ambient air
quality standards * * * and shall
recommend to the Administrator any
new * * * standards and revisions of
existing criteria and standards as may be
appropriate * * *.’’ Since the early
1980s, this independent review function
has been performed by the Clean Air
Scientific Advisory Committee.
Initially, EPA established the PM
NAAQS on April 30, 1971 (36 FR 8186),
based on the original criteria document
(Department of Health, Education, and
Welfare, 1969). The reference method
specified for determining attainment of
the original standards was the highvolume sampler, which collects PM up
to a nominal size of 25 to 45 μm
(referred to as total suspended
particulates or TSP). On October 2, 1979
(44 FR 56730), EPA announced the first
periodic review of the air quality criteria
and PM NAAQS, and significant
revisions to the original standards were
promulgated on July 1, 1987 (52 FR
24634). In that decision, EPA changed
the indicator for particles from TSP to
PM10. When that rule was challenged,
the court upheld revised standards in all
respects. Natural Resources Defense
Council v. Administrator, 902 F. 2d 962
(D.C. Cir. 1990, cert. denied, 498 U.S.
1082 (1991).
In April 1994, EPA announced its
plans for the second periodic review of
the air quality criteria and PM NAAQS,
and the Agency promulgated significant
revisions to the NAAQS on July 18,
1997 (62 FR 38652). In that decision,
EPA revised the PM NAAQS in several
respects. While EPA determined that the
PM NAAQS should continue to focus on
particles less than or equal to 10 μm in
diameter (PM10), EPA also determined
that the fine and coarse fractions of
PM10 should be considered separately.
EPA added new standards, using PM2.5
as the indicator for fine particles (with
PM2.5 referring to particles with a
nominal mean aerodynamic diameter
less than or equal to 2.5 μm), and using
PM10 as the indicator for purposes of
regulating the coarse fraction of PM10.
Following promulgation of the 1997
PM NAAQS, petitions for review were
filed by a large number of parties
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addressing a broad range of issues. In
May 1999, a three-judge panel of the
U.S. Court of Appeals for the District of
Columbia Circuit issued an initial
decision that upheld EPA’s decision to
establish fine particle standards.
American Trucking Associations v.
EPA, 175 F.3d 1027, 1055 (D.C. Cir.
1999), reversed in part on other grounds
in Whitman v. American Trucking
Associations, 531 U.S. 457 (2001). The
panel also found ‘‘ample support’’ for
EPA’s decision to regulate coarse
particle pollution, but vacated the 1997
PM10 standards concluding that EPA
had not provided a reasonable
explanation justifying use of PM10 as an
indicator for coarse particles. (Id. at
1054–55.) Pursuant to the court’s
decision, EPA removed the vacated
1997 PM10 standards but retained the
pre-existing 1987 PM10 standards (65 FR
80776, December 22, 2000).
On October 23, 1997, EPA published
its plans for the third periodic review of
the air quality criteria and PM NAAQS
(62 FR 55201), including the 1997 PM2.5
standards and the 1987 PM10 standards.
On October 17, 2006, EPA issued its
final decision to revise the primary and
secondary PM NAAQS to provide
increased protection of public health
and welfare respectively (71 FR 61144).
With regard to the primary and
secondary standards for fine particles,
EPA revised the level of the 24-hour
PM2.5 standard to 35 μg per cubic meter
(μg/m3), retained the level of the annual
PM2.5 annual standard at 15 μg/m3, and
revised the form of the annual PM2.5
standard by narrowing the constraints
on the optional use of spatial averaging.
With regard to the primary and
secondary standards for PM10, EPA
retained the 24-hour PM10 standard (150
μg/m3) and revoked the annual standard
because available evidence generally
did not suggest a link between long-term
exposure to current ambient levels of
coarse particles and health or welfare
effects.
C. Measuring PM Emissions
Section 110 of the CAA, as amended
(42 U.S.C. 7410), requires State and
local air pollution control agencies to
develop and submit plans (SIP) for EPA
approval that provide for the
attainment, maintenance, and
enforcement of the NAAQS in each air
quality control region (or portion
thereof) within such State. 40 CFR part
51 (Requirements for Preparation,
Adoption, and Submittal of
Implementation Plans) specifies the
requirements for SIP. Appendix A to
subpart A of 40 CFR part 51, defines
primary PM10 and PM2.5 as including
both the filterable and condensable
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fractions of PM. Filterable PM consists
of those particles 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
train. Condensable PM is the material
that is in vapor phase at stack
conditions but which condenses and/or
reacts upon cooling and dilution in the
ambient air to form solid or liquid PM
immediately after discharge from the
stack.
Promulgation of the 1987 NAAQS
created the need for methods to quantify
PM10 emissions from stationary sources.
In response, EPA developed and
promulgated the following test methods:
• Method 201A—Determination of
PM10 Emissions (Constant Sampling
Rate Procedure), and
• Method 202—Determination of
Condensable Particulate Emissions from
Stationary Sources.
1. Method 201A
Method 201A is a test method for
measuring filterable PM10 emissions
from stationary sources. With the
exception of the PM10-sizing device, the
current Method 201A sampling train is
the same as the sampling train used for
EPA Method 17 of appendix A–3 to 40
CFR part 60.
Method 201A cannot be used to
measure emissions from stacks that have
entrained moisture droplets (e.g., from a
wet scrubber stack) since these stacks
may have water droplets that are larger
than the cut size of the PM10 sizing
device. The presence of moisture would
prevent an accurate measurement of
total PM10 since any PM10 dissolved in
larger water droplets would not be
collected by the sizing device and
would consequently be excluded in
determining total PM10 mass. To
measure PM10 in stacks where water
droplets are known to exist, EPA’s
Technical Information Document 09
(Methods 201 and 201A in Presence of
Water Droplets) recommends use of
Method 5 of appendix A–3 to 40 CFR
part 60 (or a comparable method) and
consideration of the total particulate
catch as PM10 emissions.
Method 201A is also not applicable
for stacks with small diameters (i.e., 18
inches or less). The presence of the instack nozzle/cyclones and filter
assembly in a small duct will cause
significant cross-sectional area
interference and blockage leading to
incorrect flow calculation and particle
size separation. Additionally, the type
of metal used to construct the Method
201A cyclone may limit the
applicability of the method when
sampling at high stack temperatures
(e.g., stainless steel cyclones are
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reported to gall and seize at
temperatures greater than 260 °C).
2. Method 202
Method 202 measures CPM from
stationary sources. Method 202 contains
several optional procedures that were
intended to accommodate the various
test methods used by State and local
regulatory entities at the time Method
202 was being developed.
When conducted consistently and
carefully, Method 202 provides
acceptable precision for most emission
sources. Method 202 has been used
successfully in regulatory programs
where the emission limits and
compliance demonstrations are
established based on a consistent
application of the method and its
associated options. However, when the
same emission source is tested using
different combinations of the optional
procedures, there appears to be large
variations in the measured CPM
emissions. Additionally, during
validation of the promulgated 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. We
consistently maintain that the artifact
formation can be reduced by at least 90
percent if a one-hour nitrogen purge of
the impinger water is used to remove
SO2 before it can form sulfuric acid (this
is our preferred application of the
Method 202 optional procedures).
Inappropriate use or omission of the
preferred or optional procedures in
Method 202 can increase the potential
for artifact formation.
Considering the potential for
variations in measured CPM emissions,
we believe that further verification and
refinement of Method 202 is appropriate
to minimize the potential for artifact
formation. We performed several studies
to assess artifact formation when using
Method 202. The results of our 1998
laboratory study and field evaluation
commissioned to evaluate the impinger
approach can be found in ‘‘Laboratory
and Field Evaluation of EPA’s Method
5 Impinger Catch for Measuring
Condensible Matter from Stationary
Sources’’ at https://www.epa.gov/ttn/
emc/methods/m202doc1.pdf.
The 1998 study verified the need for
a nitrogen purge when SO2 is present in
stack gas and provided guidance for
analyzing the collected samples. In
2005, an EPA contractor conducted a
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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 at https://
www.epa.gov/ttn/emc/methods/
m202doc2.pdf. This report also verified
the need for a nitrogen purge and
identified the primary factors that affect
artifact formation.
Also in 2005, a private testing
contractor presented a possible minor
modification to Method 202 at the Air
and Waste Management Association
(AWMA) specialty conference. The
proposed modification, as described in
their presentation titled ‘‘Optimized
Method 202 Sampling Train to
Minimize the Biases Associated with
Method 202 Measurement of
Condensable Particulate Matter
Emissions,’’ involved the elimination of
water from the first impingers. The
presentation (available at https://
www.epa.gov/ttn/emc/methods/
m202doc3.pdf) concluded that
modification of the promulgated method
to use dry impingers resulted in a
significant additional reduction in the
sulfate artifact.
In 2006, we began to conduct
laboratory studies in collaboration with
several stakeholders to characterize the
artifact formation and other
uncertainties associated with
conducting Method 202 and to identify
procedures that would minimize
uncertainties when using Method 202.
Since August 2006, we conducted two
workshops in Research Triangle Park,
NC to present and request comments on
our plan for evaluating potential
modifications to Method 202 that would
reduce artifact formation, and also to
discuss (1) Our progress in
characterizing the performance of the
modified method, (2) issues that require
additional investigation, (3) the results
of our laboratory studies, and (4) our
commitments to extend the
investigation through stakeholders
external to EPA. Another meeting was
held with experienced stack testers and
vendors of emissions monitoring
equipment to discuss hardware issues
associated with modifications of the
sampling equipment and the glassware
for the proposed CPM test method.
Summaries of the method evaluations,
as well as meeting minutes from our
workshops, can be found at https://
www.epa.gov/ttn/emc/methods/
method202.html.
The laboratory studies that were
performed fulfill a commitment in the
preamble to the Clean Air Fine Particle
Implementation Rule (72 FR 20586,
April 25, 2007) to examine the
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relationship between several critical
CPM sampling and analysis parameters
and, to the extent necessary, promulgate
revisions to incorporate improvements
in the method. While these
improvements in the stationary source
test method for CPM will provide for
more accurate and precise measurement
of all PM, the addition of PM2.5 as an
indicator of health and welfare effects
by the 1997 NAAQS revisions generates
the need to quantify PM2.5 emissions
from stationary sources. To respond to
this need, we are promulgating revisions
to incorporate this capability into the
test method for filterable PM10.
III. Summary of Changes Since
Proposal
The methods in this final action
contain several changes that were made
as a result of public comments. The
following sections present a summary of
the changes to the methods. We explain
the reasons for these changes in detail
in the Summary of Public Comments
and Responses section of this preamble.
A. Method 201A
Method 201A contains the following
changes and clarifications:
• Revised Section 1.5 to clarify that
Method 201A cannot be used to
measure emissions from stacks that have
entrained moisture droplets (e.g., from a
wet scrubber stack).
• Removed the language in proposed
Section 1.5 regarding ambient air
contributions to PM. The decision to
correct results for ambient air
contributions is up to the permitting or
regulatory authority.
• Added definitions of Primary PM,
Filterable PM, Primary PM2.5, Primary
PM10, and CPM to Section 3.0.
• Added a requirement to Sections
6.1.3 and 8.6.3 stating that the filter
must not be compressed between the
gasket and the filter housing.
• Clarified the sample recovery and
analysis equipment in Section 6.2,
including acceptable materials of
construction, analytical balance, and
fluoropolymer (polytetrafluoroethylene)
beaker liners.
• Revised Section 6.2 to add
performance-based, residual mass
contribution specifications for
containers rather than specifying the
type of container that must be used
(storage containers must not contribute
more than 0.1 mg of residual mass to the
CPM measurements).
• Revised Section 8.3.1 (regarding
sampling ports) to state that a 4-inch
port should be adequate for the single
PM2.5 (or single PM10) sampling
apparatus. However, testers will not be
able to use conventional 4-inch ports if
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the combined dimension of the PM10
cyclone and the nozzle extending from
the cyclone exceeds the internal
diameter of the port.
• Clarified the sampling procedures
in Section 8.3.1 for cases where the
PM2.5 cyclone is used without the PM10
cyclone. In these cases, samples are
collected using the procedures specified
in Section 11.3.2.2 of EPA Method 1,
and the sampling time is extended at the
replacement sampling point to include
the duration of the unreachable traverse
points.
• Revised Section 8.3.2.2 to clarify
that Method 201A is not applicable for
stack diameters less than 26.5 inches
when the combined PM10/PM2.5 cyclone
is used. The in-stack nozzle/cyclones
and filter assembly in stacks less than
26.5 inches in diameter would cause
significant cross-sectional area
interference and blockage, leading to
incorrect flow calculation and particle
size separation.
• Revised Section 8.5.5 to express the
maximum failure rate of values outside
the minimum-maximum velocity
pressure range in terms of percent of
values outside the range instead of the
number of traverse points outside the
range.
• Revised section 8.6.1 to clarify that
alternative designs are acceptable for
fastening caps or covers to cyclones to
avoid galling of the cyclone component
threads in hot stacks. The method may
be used at temperatures up to 1,000°F
using stainless steel cyclones that are
bolted together, rather than screwed
together. Using ‘‘break-away’’ stainless
steel bolts facilitates disassembly and
circumvents the problem of thread
galling.
• Clarified sampling procedures in
Section 8.7.3.3 to maintain the
temperature of the cyclone sampling
head within ± 10 °C of the stack
temperature and to maintain flow until
after removing and before inserting the
sampling head.
• Revised Section 11.2.7 to allow the
use of tared fluoropolymer beaker liners
for the acetone field reagent blank.
B. Method 202
Method 202 contains the following
changes and clarifications:
• Clarified the terminology used to
refer to laboratory and field blanks
throughout the method.
• For health and safety reasons,
replaced the use of methylene chloride
with hexane throughout the method.
• Clarified Section 1.2 by moving the
discussion of filterable PM methods
used in conjunction with Method 202 to
Section 1.5.
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• Clarified Section 1.6 to specify that
Method 202 can be used for measuring
CPM in stacks that contain entrained
moisture if the sampling temperature is
sufficiently high to keep the moisture in
the vapor phase.
• Moved the recommendation to
develop a health and safety plan from
Section 9.4 to Section 5.0.
• Added amber glass bottles to the list
of sample recovery equipment in
Section 6.2.
• Added alternatives (fluoropolymer
beaker liners or fluoropolymer baggies)
to weighing tins to the list of analytical
equipment in Section 6.2.2 (Section 6.3
of the proposed method).
• Added specifications for sample
drying equipment in Section 6.2.2
(Section 6.3 of the proposed method).
• Clarified Section 6.3.7 regarding the
use of an analytical balance with
sensitivity to 0.00001 g (0.01 milligram).
• Added an option to use a
colorimetric pH indicator instead of a
pH meter in Section 6.2.2 (Section 6.3
of the proposed method).
• Added a sonication device to the
list of analytical equipment in Section
6.2.2 (Section 6.3 of the proposed
method).
• Added performance-based, residual
mass contribution specifications for
containers and wash bottles in Section
6.2.2 (Section 6.3 of the proposed
method) rather than specifying the type
of container that must be used.
• Replaced the prescriptive language
regarding filter materials in Section
7.1.1 with performance-based
requirements limiting the residual mass
contribution.
• Replaced the prescriptive language
regarding water quality in Section 7.1.3
with performance-based requirements
for residual mass content.
• Clarified Section 8.2 to specify that
cleaned glassware must be used at the
start of each new source category tested
at a single facility.
• Added a performance-based option
to Section 8.4 to conduct a field train
proof blank rather than meeting the
glassware baking requirements in
Section 8.2.
• Clarified the sampling train
configuration for the nitrogen purge
procedures in Section 8.5.3.2 regarding
pressurized purges.
C. How will the final amendments to
methods 201A and 202 affect existing
emission inventories, emission
standards, and permit programs?
We anticipate that over time the
changes in the test methods finalized in
this action will result in, among other
positive outcomes, more accurate
emissions inventories of direct PM
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emissions and emissions standards that
are more indicative of the actual impact
of the source on the ambient air quality.
Accurate emission inventories are
critical for regulatory agencies to
develop the control strategies and
demonstrations necessary to attain air
quality standards. When implemented,
the test method revisions should
improve our understanding of PM
emissions due to the increased
availability of more accurate emission
tests and eventually through the
incorporation of less biased test data
into existing emissions factors. For
CPM, the use of the revised method
could reveal a reduced level of CPM
emissions from a source compared to
the emissions that would have been
measured using Method 202 as typically
performed. However, there may be some
cases where the revised test method
would reveal an increased level of CPM
emissions from a source, depending on
the relative emissions of filterable and
CPM emissions from the source. For
example, the existing Method 202
allows complete evaporation of the
water containing inorganic PM at 105 °C
(221 °F), where the revised method
requires the last 10 ml of the water to
be evaporated at room temperature (not
to exceed 30 °C (85 °F)), thereby
retaining the CPM that would evaporate
at the increased temperature.
Prior to our adoption of the 1997
PM2.5 NAAQS, several State and local
air pollution control agencies had
developed emission inventories that
included CPM. Additionally, some
agencies established enforceable CPM
emissions limits or otherwise required
that PM emissions testing include
measurement of CPM. While this
approach was viable in cases where the
same test method was used to develop
the CPM regulatory limits and to
demonstrate facility compliance, there
are substantial inconsistencies within
and between States regarding the
completeness and accuracy of CPM
emission inventories and the test
methods used to measure CPM
emissions and demonstrate facility
compliance.
These amendments would serve to
mitigate the potential difficulties that
can arise when EPA and other
regulatory entities attempt to use the
test data from State and local agencies
with inconsistent CPM test methods to
develop emission factors, determine
program applicability, or to establish
emissions limits for CPM emission
sources within a particular jurisdiction.
For example, problems can arise when
the test method used to develop a CPM
emission limit is not the same as the test
method specified in the rule for
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demonstrating compliance because the
different test methods may quantify
different components of PM (e.g.,
filterable versus condensable). Also,
when emissions from State inventories
are modeled to assess compliance with
the NAAQS, the determination of direct
PM emissions may be biased high or
low, depending on the test methods
used to estimate PM emissions, and the
atmospheric conversion of SO2 to
sulfates (or sulfur trioxide, SO3) may be
inaccurate or double-counted.
Additionally, some State and local
regulatory authorities have assumed that
EPA Method 5 of appendix A–3 to 40
CFR part 60 (Determination of
Particulate Matter Emissions from
Stationary Sources) provides a
reasonable estimate of PM10 emissions.
This assumption is incorrect because
Method 5 does not provide particle
sizing of the filterable component and
does not quantify particulate caught in
the impinger portion of the sampling
train. Similar assumptions for
measurements of PM2.5 will result in
greater inaccuracies.
With regard to State permitting
programs, we recognize that, in some
cases, existing best available control
technology, lowest achievable emission
rate, or reasonably available control
technology limits have been based on an
identified control technology, and that
the data used to determine the
performance of that technology and to
establish the limits may have focused on
filterable PM and, thus, did not
completely characterize PM emissions
to the ambient air. While the source test
methods used by State programs that
developed the applicable permit limit
may not have fully characterized the PM
emissions, we have no information that
would indicate that the test methods are
inappropriate indicators of the control
technologies’ performance for the
portion of PM emissions that was
addressed by the applicable
requirement. As promulgated in the
Clean Air Fine Particle Implementation
Rule, after January 1, 2011, States are
required to consider inclusion of CPM
emissions in new or revised emissions
limits that they establish. We will defer
to the individual State’s judgment as to
whether, and at what time it is
appropriate to revise existing facility
emission limits or operating permits to
incorporate information from the
revised CPM test method when it is
promulgated.
With regard to operating permits, the
title V permit program does not
generally impose new substantive air
quality control requirements. In general,
after emissions limits are established as
CAA requirements under the SIP or a
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SIP-approved pre-construction review
permit, they are included in the title V
permits. Obviously, title V permits
should be updated to reflect any
revision of existing emission limits or
new emission limits created in the
context of the underlying applicable
requirements. Also, if a permit contains
previously promulgated test methods, it
is not a given that the permit would
always have to be revised should these
test method changes be finalized (e.g.,
where test methods are incorporated
into existing permits through
incorporation by reference, no permit
terms or conditions would necessarily
have to change to reflect changes to
those test methods). In any event, the
need for action related to emissions
source permitting, due to these changes
to the test methods, would be
determined based upon several factors
such as the exact wording of the existing
operating permit, the requirements of
the EPA-approved SIP, and any changes
that may need to be made to preconstruction review permits with
respect to CPM measurement (e.g.,
emissions estimates may be based upon
a source test method that did not
measure CPM or upon a set of Method
202 procedures that underestimated
CPM emissions).
In recognition of these issues, the
Clean Air Fine Particle Implementation
Rule contains provisions establishing a
transition period for developing
emission limits for condensable direct
PM2.5 that are needed to demonstrate
attainment of the PM2.5 NAAQS. The
transition period for CPM is the time
period during which the new rules and
NSR permits issued to stationary
sources are not required to address the
condensable fraction of the sources’ PM
emissions. The end date of the
transition period (January 1, 2011) was
adopted in the final Clean Air Fine
Particle Implementation Rule (72 FR
20586, April 25, 2007) and in the final
Implementation of the New Source
Review Program for Particulate Matter
Less Than 2.5 Micrometers (PM2.5) rule
(73 FR 28321, May 16, 2008). As
discussed in these two rules, the intent
of the transition period (which ends
January 1, 2011) was to allow time for
EPA to issue a CPM test method through
notice and comment rulemaking, and
for sources and States to collect
additional total primary (filterable and
condensable) PM2.5 emissions data to
improve emissions information to the
extent possible. In the PM2.5 NSR
Implementation Rule, we stated that as
part of this test methods rulemaking, we
would ‘‘take comment on an earlier
closing date for the transition period in
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the NSR program if we are on track to
meet our expectation to complete the
test method rule much earlier than
January 1, 2011’’ (73 FR 28344). In the
notice of proposed rulemaking for this
final rule on amendments to Method
201A and 202, EPA sought comment on
whether to end the NSR transition
period for CPM early (74 FR 12976). In
this final rule, EPA is taking no action
to affect the already established January
1, 2011 sunset date for the NSR
transition period.
Source test data collected with the use
of this updated test method will be
incorporated into the tools (e.g.,
emission factors, emission inventories,
air quality modeling) used to
demonstrate the attainment of air
quality standards. Areas that are
designated nonattainment for the 1997
PM2.5 NAAQS, and that have approved
attainment dates of 2014 or 2015, are
required to develop a mid-course review
in 2011. If it is determined that
additional control measures are needed
to ensure the area will be on track to
attain the standard by the attainment
date, any new direct PM2.5 emission
limits adopted by the State must address
the condensable fraction and the
filterable fraction of PM2.5. Additionally,
the new test data could be used to
improve the applicability and
performance evaluations of various
control technologies.
IV. Summary of Final Methods
A. Method 201A
Method 201A measures PM emissions
from stationary sources. The
amendments to Method 201A add a
PM2.5 measurement device (PM2.5
cyclone) that allows the method to
measure filterable PM2.5, filterable PM10,
or both filterable PM2.5 and filterable
PM10. The method can also be used to
measure coarse particles (i.e., the
difference between measured PM10
concentration and the measured PM2.5
concentration).
The amendments also add a PM2.5
cyclone to create a sampling train that
includes a total of two cyclones (one
cyclone to segregate particles with
aerodynamic diameters greater than 10
μm and one cyclone to segregate
particles with aerodynamic diameters
greater than 2.5 μm) and a final filter to
collect particles with aerodynamic
diameters less than or equal to 2.5 μm.
The PM2.5 cyclone is inserted between
the PM10 cyclone and the filter of the
Method 201A sampling train.
The revised method has several
limitations. The method cannot be used
to measure emissions from stacks that
have entrained moisture droplets (e.g.,
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from a wet scrubber stack) because size
separation of the water droplets is not
representative of the dry particle size
released into the air. In addition, the
method is not applicable for stacks with
diameters less than 25.7 inches when
the combined PM10/PM2.5 cyclone is
used. Also, the method may not be
suitable for sources with stack gas
temperatures exceeding 260 °C (500 °F)
when cyclones with screw-together caps
are used because the threads of the
cyclone components may gall or seize,
thus preventing the recovery of the
collected PM. However, the method may
be used at temperatures up to 1,000 °F
when using stainless steel cyclones that
are bolted together rather than screwed
together. Using ‘‘break-away’’ stainless
steel bolts facilitates disassembly and
circumvents the problem of thread
galling. The method may also be used at
temperatures up to 2,500 °F when using
specialty high-temperature alloys.
B. Method 202
Method 202 measures concentrations
of CPM in stationary source sample gas
after the filterable PM has been removed
using another test method such as
Method 5, 17, or 201A. The CPM
sampling train begins at the back half of
the filterable PM filter holder and
consists of a condenser, two dry
impingers (temperatures maintained to
less than 30 °C (85 °F)), and a CPM filter
(temperature maintained between 20 °C
(65 °F) and 30 °C (85 °F)). During the
test, sample gases are cooled and CPM
is collected in the dry impingers and on
the CPM filter. As soon as possible after
the post-test leak check has been
conducted, any water collected in the
dry impingers is purged with nitrogen
gas for at least one hour to remove
dissolved SO2 gas.
After the nitrogen purge, the sampling
train components downstream of the
filterable PM filter (i.e., the probe
extension (if any), condenser,
impingers, front half of CPM filter
holder, and the CPM filter) are rinsed
with water to recover the inorganic
CPM. The water rinse is followed by an
acetone rinse and a hexane rinse to
recover the organic CPM. The CPM filter
is extracted using water to recover the
inorganic components and hexane to
recover the organic portion. The
inorganic and organic fractions are then
dried and the residues weighed. The
sum of both fractions represents the
total CPM collected by Method 202.
V. Summary of Public Comments and
Responses
In response to the March 25, 2009
proposed revisions to EPA Methods
201A and 202, EPA received public
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comment letters from industry
representatives, trade associations, State
agencies, and environmental
organizations. The public comments
submitted to EPA addressed the
proposed revisions to Methods 201A
and 202 and our request for comments
on whether to end the transition period
for CPM in the NSR program on a date
earlier than the current end date of
January 1, 2011.
This section provides responses to the
more significant public comments
received on the proposed revisions to
Methods 201A and 202. Summaries and
responses for all comments related to
the proposed revisions to Methods 201A
and 202, including those addressed in
this preamble, are contained in the
response to comments document
located in the docket for this final action
(Docket ID No. EPA–HQ–OAR–2008–
0348).
A. Method 201A
1. Speciation
Comment: One commenter stated that
EPA should include guidance in
Method 201A concerning speciation of
the constituents present in the PM10,
PM10–PM2.5, and PM2.5 size fractions.
The commenter believes this
information should be provided to
support the use of speciated PM10,
PM10–PM2.5, and PM2.5 data in source
apportionment studies.
Response: EPA did not revise the
method to provide guidance for
speciation of various particle fractions
for source apportionment because
Method 201A is not a speciation
method. However, with judicious
selection of filter media, sources may
use this method for speciating the less
volatile metals and use these data in
source apportionment studies. Including
details to adapt this method for
speciation analysis would unduly
increase the complexity of the method
without increasing the precision of the
mass measurements.
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2. Catch Weight and Sampling Times
Comment: Several commenters
requested that EPA specify the
minimum solids catch weights needed
in the PM10 and PM2.5 size fractions to
help testing organizations determine the
necessary sampling times, especially for
sources with low PM concentrations.
Other commenters expressed concern
about extended sampling times that
would be necessary to obtain enough
sample to weigh accurately. One
commenter stated that a reasonable limit
must be put on sampling volume to
limit potentially unnecessary sampling
time and exorbitant stack testing costs
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that could quickly escalate with such a
requirement.
Response: We agree with the
commenters that collecting sufficient
weighable mass is important for the
method to be precise. We also
understand that the sampling rate used
to attain the cyclone cut-points is
typically less than the rate used during
Method 5 sampling. However, EPA did
not revise the method to dictate a
minimum sampling volume or
minimum catch weight that would be
necessary to obtain a valid sample. One
reason for not specifying a minimum
sampling volume or minimum catch
weight is that different regulatory
authorities and testing programs have
differing measurement goals. For
example, some regulatory authorities
will accept less precision if results are
well below compliance limits. State
agencies or individual regulated
facilities may develop data quality
objectives (DQO) for the test program,
which may specify minimum detection
limits, and/or minimum sample volume,
and/or catch weight that would
demonstrate that DQO can be met. Stack
samplers should take into consideration
the compliance limits set by their
regulatory authority and determine the
minimum amount of stack gas needed to
show compliance if the mass of
particulate is below the detection limit.
Stack testers can use the minimum
detection limit to determine the
minimum stack gas volume. The stack
tester may be able to estimate the
necessary stack gas volume based on
how much PM the source or source
category is expected to emit (which
could be determined from a previous
test or from knowledge of the emissions
for that source category).
Alternatively, the minimum detection
limit for a source can be determined by
calculating the percent relative standard
deviation for a series of field train
recovery blanks. You will not be able to
measure below the average train
recovery blank level, and EPA
recommends calculating a tester-specific
detection limit by multiplying the
standard deviation of field recovery
train blanks by the appropriate
‘‘Student’s t value’’ (e.g., for seven field
train recovery blanks, the standard
deviation of the results would be
multiplied by three). Short of having
Method 201A field recovery train blanks
for cyclone and filter components of the
sampling train, you may use the
detection limit determined from EPA
field tests.
An estimated detection limit was
determined from an EPA field
evaluation of proposed Method 201A
(see ‘‘Field Evaluation of an Improved
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Method for Sampling and Analysis of
Filterable and Condensable PM,’’ Docket
ID No. EPA–HQ–OAR–2008–0348). The
estimated detection limit was calculated
from the standard deviation of the
differences from 10 quadruplicate
sampling runs multiplied by the
appropriate ‘‘Student’s t value’’ (n¥1 =
9). Detection limits determined in this
manner were (1) Total filterable PM:
2.54 mg; (2) PM10: 1.44 mg; and (3)
PM2.5: 1.35. These test runs showed
more filterable particulate in the PM2.5
fraction, and total filterable particulate
detection limits may be biased high due
to the small particulate mass collected
in the fraction greater than PM10.
Comment: Two commenters
questioned the use of reference methods
to correct for ambient air in Section 1.5
of the proposed Method 201A. One
commenter believed that the statement
would be used as a means to blame noncompliance on ambient contributions
and would result in legal challenges and
disputes of test results. The other
commenter questioned whether it was
the intent of EPA to not allow the use
of the CPM test method for lowtemperature sources.
Response: We agree with the
commenters that Section 1.5 of the
proposed method was unclear. Thus,
Section 1.5 (Additional Methods) has
been removed from the final method.
For sources that have very low PM
emissions, such as processes that burn
clean fuels (e.g., natural gas) and/or use
large volumes of dilution air (e.g., gas
turbines and thermal oxidizers), any
ambient air particulate introduced into
the process operation could be a large
component of total outlet PM emissions.
However, the decision to correct results
for fine PM measurements to account for
ambient air contributions is up to the
permitting or regulatory authority. It is
likely that these adjustments would be
limited to gas turbines and possibly
sources fired with clean natural gas.
Comment: Commenters expressed
concern about the lack of a test method
to measure PM2.5 in stacks with
entrained moisture. Another commenter
urged EPA to continue work to identify
or develop a method for measuring
filterable (or total) PM at sources with
entrained moisture droplets in the stack
(e.g., units with wet stacks due to wet
flue gas desulfurization or wet
scrubbers). Commenters requested that
EPA provide guidance or identify a
viable alternative for high-moisture
stacks as soon as possible. One
commenter stated that when conducting
emission testing at facilities with similar
wet stack conditions as described in the
proposal preamble (74 FR 12973), that
they support EPA’s position on the
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limitations of the proposed Method
201A.
One commenter was not satisfied with
the use of Method 5 as the only
acceptable method for sources with
entrained water droplets. To provide
more accurate emissions data for
sources with ‘‘wet’’ stacks, the
commenter is sponsoring the
development of an advanced manual
sampling technique that can accurately
measure filterable PM2.5 in stacks with
entrained water droplets. The
commenter expects to complete field
tests of this method in the near future.
The commenter will share laboratory
and field test evaluations of this new
method. The commenter believes that
this new method for filterable PM2.5
emissions in ‘‘wet’’ stacks will be highly
compatible with proposed Method 201A
for filterable PM2.5 emission testing in
‘‘dry’’ stacks.
Response: We are currently
developing a method to measure PM in
stacks with saturated water vapors and
laboratory testing is ongoing. EPA has
committed a significant budget and
personnel to developing an acceptable
method for sources with wet stacks and
we plan to offer the method and
protocol as soon as possible. EPA’s
method development and evaluation is
focused on the ‘‘Dried Particle Method’’
(See ‘‘Lab Work to Evaluate PM2.5
Collection with a Dilution Monitoring
Device for Data Gathering for Emission
Factor Development (Final Report)’’ in
Docket ID No. EPA–HQ–OAR–2008–
0348) that directly measures the mass
emission rate of particles with specified
aerodynamic size. In the meantime, the
promulgated amendments to Methods
201A and 202 improve their
performance and reduce known
artifacts. Testers should use these final,
amended methods until a PM2.5 method
for stack gases containing water droplets
is promulgated.
Regarding the advanced manual
sampling technique that the commenter
is currently developing for use in ‘‘wet’’
stacks, EPA acknowledges the sampling
evaluations being conducted by the
commenter. When the data become
available, we will review the data to
determine if the consistency and
performance achieved by the advanced
manual sampling technique referenced
by the commenter are comparable to
EPA’s wet-stack sampling method
currently under development. If the data
are comparable, we will consider
whether the commenter’s sampling
technique should be addressed (e.g., as
an alternative method) when we
propose an EPA wet-stack, particlesizing method in the future.
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Comment: Several commenters
disagreed with EPA’s recommendation
to use Method 5 on stacks with
entrained moisture and to consider all
the collected mass to be PM2.5.
Commenters stated that the
categorization of all PM measured by
Method 5 as PM2.5 overstates the true
emissions. One commenter supported
EPA’s recommendation to use Method 5
to determine PM10/PM2.5 filterable mass
when measuring emissions following a
wet scrubber. Another commenter stated
that when conducting emissions testing
at facilities with similar wet stack
conditions, as described in the proposal
preamble (74 FR 12973), they supported
EPA’s position on the limitations of the
proposed Method 201A.
Response: EPA acknowledges that
using Method 5 on stacks with
entrained moisture and assuming that
the catch is PM2.5 can potentially
overestimate PM2.5 concentrations. EPA
Method 5 measures total PM mass
emissions from stationary sources.
Method 5 does not specifically isolate
PM10 or PM2.5. Method 17, similar to
Method 5, measures total PM mass
emissions, but it uses an in-stack filter
operating at stack temperature instead of
a heated probe and out-of-stack heated
filter and thus, is suitable for only dry
sources.
Monitoring the emission of PM10 or
PM2.5 from a wet gas stream is a
challenging problem that has not been
addressed successfully despite
considerable effort. A consensus method
to provide this information has not
emerged. EPA has determined that
particulate from wet stacks is expected
to be primarily PM10 under most
conditions typical of good wet scrubber
design and operation. University of
North Carolina particle physicists
performed theoretical calculations based
on a wet scrubber operating at 10,000
parts per million by weight (ppmw)
total dissolved solids (TDS) with water
droplets up to 50 μm in size (see
‘‘Development of Plans for Monitoring
Emissions of PM2.5 and PM10 from
Stationary Sources With Wet Stacks,’’
Docket ID No. EPA–HQ–OAR–2008–
0348). They determined that water
droplets under these conditions, when
dried, would generate particles of 10 μm
or less. Using the same theoretical basis
(i.e., the ratio of TDS to water droplet
size), EPA expects that water droplets
up to 10 μm in size would generate
dried particles of 2 μm or less and that
water droplets up to 20 μm would
generate dried particles up to 4 μm or
less.
Based on wet scrubber operation and
typical mist eliminator performance,
EPA has determined that the Method 5
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filterable particulate measurements are a
satisfactory approximation of PM2.5
filterable particulate from controlled
wet stack emissions. It is the States’ or
regulatory authorities’ responsibility to
interpret EPA’s recommendation to use
Method 5 when measuring PM in stacks
containing water droplets and to
consider all of the collected material to
be PM2.5.
Because a completely acceptable
method for measuring PM2.5 in wet
stacks is not currently available, EPA
understands the need to support the
States with a PM2.5 method for wet
stacks. EPA is currently developing this
method and laboratory testing is
ongoing. EPA has committed a
significant budget and personnel to
developing an acceptable method for
sources with wet stacks, as explained
above. In the meantime, the
promulgated amendments to Methods
201A and 202 improve their
performance and reduce known
artifacts. Testers should use these final,
amended methods until a PM2.5 method
for wet stack conditions is promulgated.
Comment: Several commenters
expressed concern about the limitation
of the method for stack temperatures
greater than 500 °F. One commenter
asked that EPA investigate a possible
modification to the method to utilize
sampling equipment that can withstand
higher stack temperatures. The
commenter also introduced the
possibility of moving the particle sizing
device, at least for PM2.5, out of the stack
and into a heated box, enabling use of
a glass-lined probe for sampling.
Another commenter stated that the
operator of a hot stack should not be
required to ‘‘take extraordinary
measures’’ (such as using the metal
Inconel) when such measures are not
defined in the method, no less tested in
the field for accuracy. The commenter
encouraged EPA to develop an
acceptable substitute method for hot
stacks. As an alternative, the commenter
recommended that Method 5 testing, in
conjunction with AP–42 particle size
distribution data specific to glass
furnaces, should be used for
measurement of PM2.5 in hot stacks.
Response: EPA investigated
additional alternatives to allow the use
of screwed together cyclones at elevated
stack temperatures. As a result of this
investigation, EPA has revised Section
8.6.1 of Method 201A to allow the
method to be used at temperatures up to
1,000 °F (538 °C) using stainless steel
cyclones that are bolted together, rather
than screwed together. Using ‘‘breakaway’’ stainless steel bolts facilitates
disassembly and circumvents the
problem of thread galling. If the
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stainless steel bolts seize, over-torquing
such bolts causes them to break at the
bolt head, thus releasing the cyclones
without damaging the cyclone flanges
(see ‘‘Review of Draft EPA Test Methods
201A and 202 Related to the Use of High
Temperature and Out-of-Stack Cyclone
Collection,’’ Southern Research Institute,
EPA Docket ID No. EPA–HQ–OAR–
2008–0348). The method can be used at
temperatures up to 2,500 °F using
specially constructed high-temperature
stainless steel alloys (Hastelloy or
Haynes 230) with bolt-together closures
using break-away bolts (see also
‘‘Development of Particle Size Test
Methods for Sampling High
Temperature and High Moisture
Sources,’’ California Environmental
Protection Agency, Air Resources Board
Research Division, 1994, NTIS PB95–
170221).
Regarding the use of a heated box
external to the stack to house the
cyclones, EPA disagrees with this
approach because of the potential for
significant losses of particulate in the
nozzle and probe liner. EPA expects that
transport losses for particles in the size
range of interest would be significant
enough to materially affect the
measurement results. These losses
would be caused by deposition
primarily by impaction in the sampling
nozzle (at the flow rates used in PM10
and PM2.5 sampling) and settling losses
in horizontal probes. (See ‘‘Review of
Draft EPA Test Methods 201A and 202
Related to the Use of High Temperature
and Out-of-Stack Cyclone Collection,
Southern Research Institute,’’ EPA
Docket ID No. EPA–HQ–OAR–2008–
0348.)
Sampling from ducts smaller than
allowed by the blockage criteria or from
ducts at high temperatures presents
challenges that should be addressed by
the source tester in conjunction with the
regulatory authority. Method 201A does
not permit the use of a nozzle and probe
extension leading to an external heated
oven to house the cyclones that would
otherwise block stack flow or operate at
stack temperatures beyond acceptable
limits. Conventional screwed-together
cyclones are designed to operate in
stacks that have a blockage of less than
three percent and have a temperature of
less than 500 °F.
Regarding the use of AP–42 as a
replacement for PM10 or PM2.5
compliance testing, EPA has determined
that this is not appropriate because of
the uncertainty in the data due to
variations in the particle sizing used to
generate AP–42 emission factors. EPA’s
AP–42 particle-sizing data for sources
controlled by wet scrubbers are based
upon particle sizing methodologies that
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are affected by the same influences and
uncertainties that make particle sizing
in stacks with entrained water droplets
a challenging technical issue. Particlesizing information in AP–42 is based
primarily upon data collected in the
1970s and early 1980s. The
uncertainties associated with methods
used during this period of time result in
particle-sizing data that are dated and
may not reflect the best sampling
technology or the emissions from
current control devices. Particle-sizing
data from the 1970s employed many
measurement methodologies that were
found to introduce indeterminate biases
in the particle sizing data. Also, source
testers implemented measurement
methods in different ways to deal with
particle-sizing methodology and sourcespecific measurement challenges. The
inconsistencies associated with
addressing measurement challenges and
indeterminate biases led to higher
uncertainties associated with the
measurement method results. Therefore,
AP–42 should not be used as a
replacement for contemporary
emissions testing.
However, it may be acceptable to
allow limited application of AP–42
particle size distributions as screening
assessments when the underlying
biases, uncertainties, and variations of
the particle-sizing are taken into
consideration. For example, one simple
method involves using terms that
include factors (such as the TDS of the
recirculating scrubber water, estimated
water droplet size distribution of the
exit gas, and total liquid mass) that are
already used to calculate approximate
emission factors. Instruments are
commercially available that can
continuously monitor TDS and water
flow rate, and the output from these
instruments could feed into an emission
factor to provide a continuous estimate
of emissions that varies with process
conditions. However, work needs to be
done to evaluate the reliability and bias
of this type of candidate estimation
method. The required data inputs for
this type of estimation model need to be
identified and the likelihood that these
inputs can be provided by the emission
source needs to be confirmed. Once the
input data can be readily obtained, the
estimation model(s) needs to be
evaluated to bring the most promising
methods to fruition. (See ‘‘Development
of Plans for Monitoring Emissions of
PM2.5 and PM10 from Stationary Sources
with Wet Stacks, Department of
Environmental Sciences and
Engineering, University of North
Carolina at Chapel Hill under
subcontract to MACTEC Federal
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Programs,’’ EPA Contact No: EP–D–05–
096, Work Assignment 2–05, August
2007; Docket ID No. EPA–HQ–OAR–
2008–0348).
Comment: Several commenters
requested changes to Section 6 of
Method 201A regarding equipment and
supplies. One commenter questioned
the use of glass dishes and glass 250 ml
beakers for drying the filter and rinses
in proposed Method 201A. Another
commenter stated that, at a minimum,
the method should specify glass
beakers, 50 ml weighing tins, and an
analytical balance with a resolution of
0.00001 g (0.01 mg). One commenter
recommended that polyethylene
transfer/storage bottles should be
allowed to minimize the chance of
breakage when in the field.
Response: We revised Sections 6.2,
11.2.4, and 11.2.7 of Method 201A to
allow the use of fluoropolymer beaker
liners for evaporating the particulate
rinse solvent and the acetone field
reagent blank, desiccating particulate to
constant weight, and weighing
particulate samples in the final
evaporation step. We revised Section
6.2, consistent with the commenter’s
suggestions, and added glass beakers
and an analytical balance with a
resolution of 0.00001 g (0.01 mg) to the
sample recovery and analytical
equipment list. However, we did not
include weighing tins because we
determined that quantitative transfer of
particles in acetone from a beaker to a
weighing tin is not necessary and adds
unnecessary imprecision to the final
sample weight. Alternatively, EPA has
changed the method to allow
fluoropolymer beaker liners to be used
to evaporate and weigh the samples.
EPA revised Section 6.2.1 of Method
201A by defining sample recovery items
consistently with Method 5, except for
wash bottles and sample storage bottles.
Any container material is acceptable for
wash bottles and storage bottles, but the
container must not contribute more than
0.05 mg of residual mass to the CPM
measurements.
Comment: Several commenters
expressed concern about the proposed
requirement to use a 6-inch sampling
port. One commenter pointed out that
using a 6-inch sampling port would be
required only for the combined
PM10/PM2.5 sampling apparatus.
Another commenter stated that the
physical dimensions of the cyclone
would also cause problems with
installation in the generally small fryer
and dryer stacks. Another commenter
noted that the partitioning of the
filterable solids using bulky, in-stack
cyclones creates several logistical and
practical problems. The commenter
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stated that the size of the in-stack
separation cyclones requires
6-inch to 8-inch sampling ports that do
not exist at the vast majority of
stationary sources potentially affected
by this final action.
Response: EPA understands the
commenters’ concerns regarding
sampling port diameter requirements.
However, facilities that are required to
use Method 201A are responsible for
ensuring that the stack has the
appropriately sized sampling ports. The
need for the larger port diameter has not
changed from the requirement as stated
in the 1990 version of this method. We
revised Section 8.3.1 of Method 201A to
more clearly describe when a 4-inch
port may not accommodate the PM10
particle-sizing cyclone and the nozzle
that extends from the cyclone and to
highlight the need for a larger port in
such situations.
Comment: One commenter requested
that EPA adjust the allowable number of
traverse points that fall outside of the
range of the Dpmin and Dpmax for cases in
which more than the recommended
maximum 12 traverse points are
sampled by Method 201A. Many
agencies require that more than the
recommended maximum 12 traverse
points be sampled if total filterable
particulate is being determined. The
commenter requested that the number of
allowed out-of-range values be adjusted
to match the stated failure rates
expressed as percentages.
Response: EPA agrees that increasing
the number of allowable traverse points
outside the range Dpmin and Dpmax is
appropriate when more than the
recommended number of traverse points
are sampled. EPA has modified Section
8.5.5 of the method to allow 16 percent
failure rate rounded to the nearest
whole number for PM2.5 only and 8
percent failure rate rounded to the
nearest whole number if the course
fraction for PM10 determination is
included.
Comment: One commenter requested
that EPA add a new section in Section
8.3.2 to address ducts with diameters
less than 18 inches. The commenter
stated that the new section should state
that ducts with diameters less than 18
inches have blockage effects ranging
from five to ten percent. Therefore,
according to the commenter, when a test
is conducted on these small ducts, the
observed velocity pressures must be
adjusted for the estimated blockage
factor whenever the combined sampling
apparatus blocks more than three
percent of the stack or duct.
For stacks smaller than 18 inches, one
commenter asked if there would still be
a blockage issue even when following
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the proposed Method 201A procedures,
especially as the stack diameter gets
smaller. The commenter also asked if
there was a lower limit of stack diameter
where the method cannot be used.
One commenter stated that when
conducting emissions testing at facilities
with similar small stack (less than 18
inches in diameter) conditions, as
described in the proposal preamble (74
FR 12973), their experience supported
EPA’s position on the limitations of the
proposed Method 201A. Another
commenter pointed out an error in
Section 8.7.2.3 that implied that the
method could be used on stacks with
diameters less than 18 inches.
Another commenter requested that if
testing of stacks less than 18 inches in
diameter is still allowed and the testers
are required to use Method 1A, then the
option of using a standard pitot tube
should apply.
Response: We revised Section 8.7.2.3
of Method 201A to clarify the lower
limits of stack diameter for different
sampling configurations. The combined
PM10/PM2.5 filter sampling head and
pitot tube is not applicable for stacks
with a diameter less than 26.5 inches
because the blockage is greater than six
percent. Blockage above six percent is
not allowed for the combined PM10/
PM2.5 filter sampling head and pitot
tube. However, measurements for only
PM2.5 may be possible using only a
PM2.5 cyclone, pitot tube, and in-stack
filter for stacks with a diameter less than
26.5 inches. If the blockage exceeds
three percent but is less than six percent
in that configuration, you must follow
the procedures outlined in Method 1A
to conduct tests on stacks less than 26.5
inches in diameter. In addition, you
must conduct the velocity traverse
downstream of the sampling location or
immediately before the test run.
We also modified Section 10.1 of the
method to allow standard pitot tubes to
be used downstream when significant
blockage exists. As stated in Section
8.3.2.2, you must adjust the observed
velocity pressures for the estimated
blockage factor whenever the sampling
apparatus blocks three to six percent of
the stack or duct.
Comment: One commenter requested
that the specification for the maximum
allowable acetone blank value be
changed from 0.001 percent by weight
to either 1 ppmw or 0.0001 percent by
weight to be consistent with the reagent
specification stated in Section 7.2.1 of
the method.
Response: We agree with the
commenter that maximum allowable
acetone blank value should be
consistent with the reagent specification
stated in Section 7.2.1. Thus, we revised
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Section 12.3.2.3 of the final method to
specify the maximum allowable acetone
blank in terms of weight per volume of
acetone (0.1 mg per 100 ml solvent),
rather than percent weight.
Comment: One commenter expressed
concern about the approach in Section
12.3.2.3 of the proposed method. The
commenter stated that subtracting the
acetone blank mass from the individual
sample masses would be acceptable if
the volumes of the acetone rinses are all
exactly 100 ml. However, according to
the commenter, this was not reality, and
the accuracy of determining the blank
correction suffers from this approach.
The commenter suggested that rather
than subtracting the mass of the acetone
rinse blank dry residue directly from the
sample masses, the concentration of the
acetone rinse blank should be calculated
as the mg of dry residue per ml of
acetone rinse blank volume limited to
the concentration of residue at 1 ppmw.
The commenter stated that this
concentration of the dry residue would
be multiplied by the volume of the
acetone in ml used to collect and
recover each sample from the sampling
head. The commenter stated that the
resulting mass would be subtracted from
the dry residue mass determined for the
sample of interest. According to the
commenter, this approach will provide
a more accurate determination of the
dry residue mass from the acetone rinse
blank due to processing a larger volume
of acetone, and assessment of the blank
mass correction for each sample as it
will be proportional to the amount of
acetone used to collect each sample.
The commenter stated that the liquid
volume of the samples and blanks could
be determined by either direct
volumetric measurement or by
multiplying the wet weight of the
sample or blank by the density of the
reagent at 20 °C.
Response: We agree with the
commenter and with the commenter’s
suggested equation. Therefore, we
revised Section 12.3.2.3 of the final
method to accommodate different
acetone rinse volumes. However, the
correction must be proportional to the
amount of solvent used. Some testers
may use more solvent due to heavy
deposits that are difficult to remove,
while other testers may use less solvent.
Therefore, the maximum adjustment is
0.1 mg per 100 ml of the acetone used
from the sample recovery.
B. Method 202
1. Extraction Solvent
Comment: Three commenters noted
that methylene chloride is highly toxic.
One commenter stated the use of
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methylene chloride poses significant
exposure risks to field test personnel,
plant personnel working in the area of
the mobile laboratory, and agency test
observers. Two commenters stated that
Method 202 should specify a less toxic
solvent than methylene chloride, such
as n-hexane.
One commenter stated that EPA
should sponsor a set of tests to confirm
that n-hexane or another less-toxic
solvent provides the sample rinse
effectiveness as methylene chloride.
Another commenter encouraged EPA to
conduct future studies to identify a
solvent to replace methylene chloride in
Proposed Method 202 and in other EPA
reference methods.
Another commenter stated that the
use of methylene chloride (a known
carcinogen) as the cleaning and recovery
solvent will require safety departments
to develop procedures for appropriate
handling on-site and the use of personal
protection equipment for personnel that
may be exposed to the solvent. The
commenter noted that toluene, which is
used in EPA Method 23, is a technically
acceptable alternative to methylene
chloride. The commenter suggested that
EPA review the use of toluene as a
replacement for methylene chloride in
Method 202 (and OTM 028).
Response: The extraction solvent
specified in a particular test method is
dependent on the analyte(s) of interest.
If the target analyte is known, an
appropriate solvent can be identified
that has the desired recovery
performance for that analyte. For
Method 202, the pollutant measured by
the method, CPM, is defined by the
method (i.e., whatever remains after the
sample recovery procedures is
considered to be CPM regardless of its
analyte group). Although no single
solvent is universally applicable to all
analyte groups, methylene chloride was
chosen for the proposed method based
upon studies (‘‘IERL–RTP Procedures
Manual, Level 1, Environmental
Assessment’’; EPA–600/2–76–160a; June
1976) that showed it was the optimum
solvent to recover polar and non-polar
CPM.
We acknowledge the commenters’
concerns regarding the toxicity of
methylene chloride and the exposure
hazards associated with its use, and we
agree that the use of an alternative
solvent is justified. However, because
the recovery performance of solvents
has been previously evaluated to
support various EPA programs, we
disagree with the commenters that
additional studies are necessary to
identify a suitable alternative solvent.
In identifying an alternative solvent,
we initially considered specifying
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toluene because its extraction
performance for non-polar compounds
is similar to methylene chloride.
However, because the vapor pressure of
toluene is lower than methylene
chloride, additional time would be
needed to evaporate the organic samples
to dryness at room temperature (30°C or
less). Because the additional
evaporation time would be an
additional burden on testing contractors
and present the risk of losing
condensable organic compounds, we
rejected toluene as the replacement
solvent.
We also evaluated the solvents used
for organic compound recovery in the
analytical methods developed by EPA’s
Office of Solid Waste (https://
www.epa.gov/epawaste/hazard/
testmethods/sw846/online/
3_series.htm). We reviewed EPA’s ‘‘Test
Methods for Evaluating Solid Waste,
Physical/Chemical Methods’’ (SW–846),
which was developed to support the
Resource Conservation and Recovery
Act (RCRA) program, to identify test
methods that covered the same types of
compounds expected to comprise CPM.
Based upon our review of SW–846, we
identified Method M–3550c (Ultrasonic
Extraction) as a comparable method (M–
3550c is used to extract semi-volatile
organic compounds from waste
samples). Section 7.4 of M–3550c,
which discusses extraction solvents,
lists the following extraction solvents by
class of compound:
• Acetone/hexane or acetone/
methylene chloride can be used to
extract semivolatile organics.
• Acetone/hexane or acetone/
methylene chloride can be used to
extract organochlorine pesticides.
• Acetone/hexane, acetone/
methylene chloride, or hexane can be
used to extract polychlorinated
biphenyls (PCB).
Of the above compound classes, the
class that most closely relates to the
type of high-molecular weight
hydrocarbons expected to comprise
organic CPM is PCB. Hexane is also
listed as an alternative solvent (when
used in combination with acetone) for
the other compounds classes discussed
in Section 7.4. Consequently, based
upon this analysis, we have replaced
methylene chloride with hexane in the
final method.
2. Sample and Blank Containers
Comment: One commenter
recommended that EPA revise the
proposed method to specify the
container type for each container (i.e.,
glass or plastic), and also whether the
lid should have a Teflon® liner or
whether another liner is acceptable.
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Response: We disagree with the
commenter that the method should
specify the material of construction of
containers used for sample and blank
recovery procedures. Although we
believe that the most appropriate
containers are constructed of glass and
equipped with a fluoropolymer lid, we
also believe that testing contractors
should have the flexibility to select the
type of containers that meet the
performance specifications of the
method. Therefore, we have revised the
proposed method to add a performancebased specification for containers.
Section 6.2.2 of the final method
specifies that the containers used for
sample and blank recovery procedures
must not contribute more than 0.05 mg
of residual mass to the CPM
measurements.
Accompanying edits were also made
to the CPM container language in
Section 8.5.4 (Sample Recovery).
3. CPM Filter
Comment: One commenter suggested
that the language in Section 7.1.1 of the
proposed method be revised to replace
the term ‘‘Filter’’ with ‘‘CPM Filter’’ and
replace ‘‘Teflon®’’ with ‘‘Teflon®,
fluoropolymer or chemically
equivalent.’’ Another commenter stated
that the final method should allow for
alternatives to Teflon® filters, such as
quartz, polytetrafluoropolymer (PTFE)
coated, or PTFE filters.
Response: Based upon the comments
received regarding the CPM filter, we
revised the language in Section 7.1.1 to
include performance-based
specifications for the CPM filter rather
than specifying a particular type of
filter. Section 7.1.1 of the final method
specifies that the CPM filter must be a
non-reactive, non-disintegrating filter
that does not contribute more than 0.5
mg of residual mass to the CPM
measurements. The CPM filter must
have an efficiency of at least 99.95
percent (less than 0.05 percent
penetration) on 0.3 μm particles.
Documentation of the CPM filter’s
efficiency is based upon test data from
the supplier’s quality control program.
In selecting the appropriate CPM
filter, testing contractors should avoid
the mistake of equating the dioctyl
phthalate size for the test particles to the
pore size for the filter. Filters with pore
sizes larger than the test particles can
retain a high percentage of very small
particles. In our evaluation of different
types of filters, we determined that filter
sizes of 47 mm are marginal, if not
unacceptable, for use. Additionally, we
believe that hydrophobic filters should
be used to avoid absorption of water
onto the CPM filter.
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4. Water Specifications
Comment: Two commenters suggested
that the final method specify the level
of residue allowed for the water used to
clean glassware and recovery samples,
as was specified for acetone and
methylene chloride. One commenter
stated that the maximum percent
residue by weight of the water should be
specified to be consistent with the
reagent specifications for acetone and
methylene chloride. Three commenters
noted that a residual mass level is not
available for ASTM International
D1193–06, Type I water.
Response: The purpose of the field
reagent blanks is to provide a testing
contractor with information to target
corrective actions, if necessary, if they
have difficulty in meeting the residual
mass allowance in the method. The
method does not require analysis of
field reagent blank samples, and the
field reagent blank values are not used
in correcting CPM measurements.
However, we acknowledge that Figure 3
could be misleading with regard to the
field reagent blanks, and we have
revised Figure 3 of the final method to
remove the entries for the field reagents.
We acknowledge that the residue
level is not specified for ASTM
International D1193–06, Type I water,
and we agree with the commenters that
the method should specify a residual
mass level for water used to prepare
glassware and recover samples.
Therefore, we have revised Sections
7.1.3 and 7.2.3 of the final method to
specify that glassware preparation and
sampling recovery must be conducted
using deionized, ultra-filtered water that
meets a residual blank value of 1 ppmw
or less. We have also made
accompanying changes to water
specified in Sections 8.4, 8.5.3.2, and
11.2.2.1 of the final method. We believe
that this performance specification will
provide flexibility to testing contractors
in obtaining deionized, ultra-filtered
water (e.g., water could be purchased
with a vendor guarantee or the
contractor could evaluate water they
produce by evaporation and weighing of
the residue).
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5. Glassware Baking Requirements
Comment: Several commenters stated
that the proposed requirement in
Section 8.4 to bake glassware at 300°C
for six hours was excessive. Several
commenters stated that they had
conducted experimental tests that
showed that a lower baking temperature
(e.g., 125°C for three hours) was
sufficient to achieve the blank
allowance specified in the method. One
commenter stated that, based upon their
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experiments, no benefit was obtained
from baking glassware. Another
commenter stated that they had
conducted numerous test runs on noncombustion sources without baking
glassware and had achieved acceptable
blank results. The commenter noted that
there might be some emission sources
where baking of glassware could be
needed to meet the blank requirements,
but the commenter stated that the
mandatory baking requirements did not
seem to be necessary for all sources.
Another commenter stated that there is
no laboratory data to determine if a
lower temperature could be sufficient to
achieve low background masses. Based
upon experimental results, the
commenter suggested allowing the use
of baking of glassware at 125°C for three
hours.
One commenter stated that, because
the presence of silicone grease on
impinger surfaces is highly unlikely due
to the prevalence of O-rings, baking the
glassware at 125°C for three hours after
cleaning is adequate. The commenter
added that the baking requirements
should be revised because hightemperature baking would destroy or
deteriorate the O-rings typically used to
seal impinger components. The
commenter stated that the effort to
remove these O-rings before baking and
then replace them after baking is timeconsuming. Several commenters noted
that the high-temperature baking
requirements would be overly expensive
(e.g., for large, high-temperature ovens)
and time-consuming.
Another commenter stated that the
requirement for glassware baking only
prior to the test makes little sense. The
commenter questioned why the
glassware could not be rinsed with the
recovery solvents as is done between
runs. The commenter noted that the
proposed method mandates a reagent
blank and questioned why the reagent
blank could not be changed to a proof
blank with a limit.
One commenter stated that the
requirement to bake glassware at 300 °C
for six hours should be optional because
it has not been possible to fully evaluate
the supporting data and the need for
such high temperature is not readily
apparent for all situations. The
commenter noted that the ‘‘Draft Project
Report—Evaluation and Improvement of
Condensable Particulate Measurement’’
may contain this information and
recommended that the effect of pre-bake
temperature and time on cleanliness of
blanks be clearly presented in this
report and include a table comparing
the effect of 300 °C for six hours versus
lower glassware preparation
temperatures. Otherwise, according to
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the commenter, this requirement would
require the stack tester to bring to the
testing site a large amount of precleaned glassware, much more than
what is currently normal for such
testing.
One commenter suggested that testing
contractors be allowed to meet the blank
level specified in the method however
they can. The commenter stated that the
prescriptive temperature requirement,
particularly in light of the fact that there
are no data showing that the 2 mg blank
cannot be achieved at lower
temperatures or through other means,
did not serve a purpose. Another
commenter recommended that the tester
start with baked glassware for the first
test and then be allowed to perform
additional tests reusing the same
glassware after it has been cleaned by
chemical methods. If the chemical
cleaning of the glassware is not
adequate, the commenter noted that
blank values would likely elevate,
possibly eliminating the test from
consideration. If the blanks do not
elevate, the commenter stated that this
scenario would be very cost-effective
and would conserve resources.
Response: Method 202 has the
potential to measure CPM at very low
levels. Consequently, the glassware used
in the sampling train must be free from
contamination to maximize the
precision and accuracy of the CPM
measurements. The glassware cleaning
requirements contained in the proposed
revisions to Method 202 were based
upon experimental results that
indicated that the allowable blank
correction of the method could not be
achieved without thorough cleaning and
baking of the glassware at 300 °C for six
hours.
Based upon our review of the public
comments received regarding the baking
requirements, we have determined that
it is appropriate to provide a
performance-based option in Section 8.4
for demonstrating the cleanliness of
glassware used during the emission test.
The option provides testing contractors
with flexibility when preparing
glassware while maintaining the
cleanliness requirements of the method.
As an alternative to baking glassware,
the final method allows testing
contractors to perform a proof blank of
the sampling train. Field train proof
blanks are recovered on-site from a
clean, fully assembled sampling train
prior to the first emissions test and
provide the best indication of the lowest
residual mass achievable by the tester.
Field train recovery blanks are
recovered from a sampling train after it
has been used to collect emissions
samples and has been rinsed in
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preparation for the second or third test
in a series at a particular source. Use of
field train recovery blanks allows the
tester to account for and manage
additional uncertainty that may be
attributed to the tester’s ability to clean
the sampling train between test runs in
the field.
6. Nitrogen Purge
Comment: Three commenters
requested that the nitrogen purge
procedures specified in Section 8.5 of
the proposed method be revised to
allow for the dry gas meter to be
disconnected from the sampling train
before the nitrogen purge is be
conducted. Two commenters stated that
EPA should eliminate the portion of
Figure 2 that shows the meter box and
revise the text in the proposed Method
202 to require purging in a clean
environment without the need for a
meter box. Three commenters added
that allowing the dry gas meter to be
disconnected from the sampling train
would decrease the delay between tests
(i.e., the dry gas meter could be used
with a new sampling train while the
purge is being conducted on the
previous train). Three commenters also
stated that requiring the dry gas meter
to be connected to the sampling train
during the purge will force testing
contractors to bring extra equipment
(e.g., sampling trains, dry gas meters) to
the sampling site.
Three commenters suggested that the
purge should be conducted at the
sample recovery location (e.g., mobile
laboratory) rather than at the actual
sampling location (e.g., roof, stack
sampling platform). Two commenters
noted that it is not practical to haul
nitrogen cylinders to the sampling
location. One commenter suggested that,
after the final leak check, the open ends
of the impinger train could be capped
during transport to the sample recovery
area to reduce the possibility of oxygen
contamination. The commenter noted
that the sample would not be exposed
to any more air than when immediately
connecting to the nitrogen purge line.
Several commenters suggested that
the proposed method be revised to
allow testing contractors to conduct a
positive-pressure purge instead of a
negative-pressure purge using the dry
gas meter. One commenter suggested
that the purge gas flow rate be
monitored by a rotameter instead of
using the dry gas meter. The commenter
noted that the flow rate is better
regulated upstream of the impingers
rather than downstream by the dry gas
meter and using the rotameter to
regulate the purge gas flow rate would
reduce the potential for pressurizing the
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sampling train. Another commenter
expressed concerns that if the vacuum
drawn by the dry gas meter does not
match the pressure from the nitrogen
tank, then the impingers could become
over-pressurized which could
compromise the integrity of the
sampling train components.
One commenter recommended that
the proposed testing protocol be
modified to allow the tester to
disassemble the impinger train to
measure for moisture content prior to
conducting the required nitrogen purge.
One commenter noted that weighing the
impingers prior to the nitrogen purge
would provide a more accurate moisture
catch determination and the need to
measure the amount of degassed
deionized water that is added (if any)
would be eliminated. Three commenters
added that, if the moisture content of
the impingers is determined before the
nitrogen purge, then testing contractors
should be allowed to purge only the
knock-out impinger, backup impinger,
CPM filter, and first moisture trap
impinger. One commenter stated that if
the sampling train is purged by pushing
nitrogen through the sampling train (i.e.,
positive pressure purge), then the
sampling train components after the
CPM filter thermocouple could be
disconnected from the train before
beginning the purge. One commenter
suggested that the purge be conducted
through a Teflon® tube inserted through
a stopper into the impinger arm and
then into the liquid to avoid
compounding errors associated with
adding water to the first impinger (if
needed). The commenter stated that this
would alleviate the need to break the
fitting or add water, and prevent the
potentially compounding error of water
addition. Another commenter requested
that a Teflon® line be inserted down
and through the short-stem impinger
extending below the water level in the
impinger catch. The commenter stated
that this would reduce the potential for
breaking glassware and contamination
when removing/inserting glassware
stems.
Three commenters suggested that the
nitrogen purge requirements be revised
to allow for any liquid collected in the
first (drop-out) impinger to be
transferred to the second (backup)
impinger. The commenters noted that
this approach would decrease the
potential for contamination because a
new piece of glassware (the long-stem
impinger) would not be introduced into
the sampling train. One commenter
recommended that, after the liquid is
transferred to the second impinger, the
first impinger should be removed from
the sampling train prior to the purge.
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Response: It was our intent in the
proposed Method 202 to allow testing
contractors the option of conducting
either a pressurized purge (i.e., without
the dry gas meter box and pump
attached to the sampling train) or a
vacuum purge (i.e., with the dry gas
meter box attached to the sampling
train). However, we acknowledge that
the language in Section 8.5.3 and the
sampling train depicted in Figure 2 of
the proposed method were unclear.
Consequently, we have revised Section
8.5.3 and Figure 2 and added Figure 3
to the final method to clarify that a
pressurized purge is an acceptable
alternative.
With regard to the commenters’
suggestion to allow testing contractors
to conduct the nitrogen purge at the
sample recovery location instead of at
the sampling location, we continue to
believe that testing contractors should
have the flexibility to conduct the
nitrogen purge at the location of their
choosing; therefore, the final method
does not specify where the purge must
be conducted. However, testing
contractors should conduct the purge as
soon as practicable after the post-test
leak check to reduce the potential for
artifact formation in the impinger water.
With regard to the alternative
sampling train configuration for the
purge, we agree with the commenters
that testing contractors should be
allowed the option of determining the
amount of moisture collected prior to
conducting the nitrogen purge,
transferring any water collected prior to
the CPM filter to the second impinger,
and performing the nitrogen purge on
the second impinger and the CPM filter
only. Therefore, Section 8.5.3.2 of the
final method contains an alternative
purge procedure.
We disagree with the commenter’s
suggestion to insert a Teflon® tube into
the first impinger for conducting the
nitrogen purge. Using the configuration
suggested by the commenters, there is
no provision to maintain the
temperature of the purge gas.
Consequently, we believe that a Teflon®
or other inert line used to purge the
CPM train is not an acceptable
alternative. Therefore, we are not
revising Section 8.5.3.2 to allow the use
of a Teflon® tube.
C. Conditional Test Method 039
(Dilution Method)
Comment: Several commenters urged
EPA to continue the development of
dilution-based test methods for
measuring PM2.5. One commenter
supported EPA’s work through the
stakeholder process to decrease and
eliminate other pollutant interferences
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that can affect the accurate
measurement of emissions of fine
particles, particularly for wet stacks and
high volume/low concentration gas
streams. Another commenter
encouraged EPA to use the stakeholder
process, similar to that used for
Methods 201A and 202, to move
towards the promulgation of dilution
methods and other test methods that can
better measure emissions from hightemperature and high-moisture sources.
One commenter asserted that dilution
methods more correctly simulate the
atmospheric process leading to the
formation and deposition of PM in the
atmosphere. Another commenter
expected that EPA’s evaluation of an air
dilution method would show that it is
even more useful in accurately
measuring direct PM2.5 filterable and
condensable data for high temperature
sources than the revised Methods 201A
and 202.
Response: EPA continues to evaluate
the precision and bias of PM2.5 collected
using dilution methods. In addition to
EPA’s hardware design, several other
hardware designs have been proposed
that utilize dilution. While limited
evaluations of EPA’s hardware design
have been performed, the other
hardware designs proposed have more
limited evaluations. The consensus
standards body, ASTM International,
has embarked on preparation of a
standard method for dilution sampling
of particulate material. We will continue
to evaluate dilution method procedures
and support the efforts of the ASTM
International in their development of a
standard dilution-based test method for
sampling PM. In addition to these
development efforts, several other
factors influence EPA’s decision to
delay proposing a dilution based
sampling method. One factor is that
there is no widely accepted dilution
method available at this time. Another
factor is that the available dilution
sampling hardware configurations share
few of the equipment used by any of the
existing sampling methods. As a result,
testing contractors would be required to
invest in this new equipment. This
capital investment would require a
higher charge for testing than for the
existing methods. In addition, since
dilution sampling is somewhat more
complex, contractors are likely to
initially charge a premium for this more
complex testing. Lastly, the availability
of hardware and experienced
individuals to perform dilution
sampling is extremely limited. EPA
recognizes that there are limited
applications where dilution sampling
provides advantages over the standard
test methods. As a result, we encourage
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sources that encounter these situations
to request that the regulatory authority
that established the requirement to use
this method to approve the use of
dilution sampling as an alternative to
the test method specified for
determining compliance.
Comment: One commenter
maintained that use of a test method to
define what constitutes CPM for all
sources is neither necessary, nor (in
some cases) useful. For sources, like
coal-fired boilers, where the only true
condensable sulfate specie from coal
combustion is sulfuric acid, the
commenter stated that CPM could be
better quantified by direct measurement
using the Controlled Condensation
Method (CCM). The commenter said
that States should be allowed and, in
the case of units with wet scrubbers,
encouraged to use such direct
measurements like CCM to quantify
known CPM instead of using Method
202. According to the commenter, if the
use of CCM is not allowed, Method 202
should include a procedure that allows
sources to correct Method 202 results
using results from simultaneous CCM
test runs. In this procedure, according to
the commenter, the source would be
subtracting out essentially the same
units of sulfate from Method 202 as
would be added back in from the CCM
results. If, on the other hand, sulfate
artifacts do exist, the commenter said
that the source would be subtracting ‘‘x’’
units of sulfate from Method 202 and
adding back ‘‘y’’ units of sulfate from
CCM to get an accurate measurement.
Response: While SO3 may be the most
abundant CPM emitted from coal fired
combustion, there is indication that
other compounds comprise CPM. Few
speciation tests of coal and oil
combustion have been preformed, but
those that have indicate the presence of
not only sulfate but also chloride,
nitrate, ammonium ion, and a range of
inorganic elements that are potentially
components for CPM (including
phosphorous, arsenic, and selenium). In
addition, speciation tests have been able
to identify components representing
only about 60 percent of the mass.
Therefore, the specific correction for
sulfuric acid from coal combustion
source emissions proposed by the
commenter would add to the
complexity of the method for all source
categories while providing an advantage
to only one specific source category.
EPA continues to review methods that
involve controlled condensation for
sulfuric acid. Because no standard
method is available for controlled
condensate measurement of sulfuric
acid, we have determined that providing
additional guidance or correction of
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Method 202 results is premature. EPA is
following current efforts by ASTM
International to develop a standard
controlled condensate method for
sulfuric acid. In the meantime, testers
and facilities should petition their
regulatory authority to approve
alternative data treatment for specific
sources.
VI. Statutory and Executive Order
Reviews
A. Executive Order 12866: Regulatory
Planning and Review
This action is not a ‘‘significant
regulatory action’’ under the terms of
Executive Order (EO) 12866 (58 FR
51735, October 4, 1993) and is,
therefore, not subject to review under
the EO.
B. Paperwork Reduction Act
This action does not impose an
information collection burden under the
provisions of the Paperwork Reduction
Act, 44 U.S.C. 3501 et seq. Burden is
defined at 5 CFR 1320.3(b). The final
amendments do not contain any
reporting or recordkeeping
requirements. The final amendments
revise two existing source test methods
to allow one method to perform
additional particle sizing at 2.5 μm and
to improve the precision and accuracy
of the other test method.
C. Regulatory Flexibility Act
The Regulatory Flexibility Act (RFA)
generally requires an agency to prepare
a regulatory flexibility analysis of any
rule subject to notice and comment
rulemaking requirements under the
Administrative Procedure Act or any
other statute unless the agency certifies
that the rule will not have a significant
economic impact on a substantial
number of small entities. Small entities
include small businesses, small
organizations, and small governmental
jurisdictions.
For purposes of assessing the impacts
of this rule on small entities, small
entity is defined as: (1) A small business
as defined by the Small Business
Administration’s (SBA) regulations at 13
CFR 121.201; (2) a small governmental
jurisdiction that is a government of a
city, county, town, school district or
special district with a population of less
than 50,000; and (3) a small
organization that is any not-for-profit
enterprise which is independently
owned and operated and is not
dominant in its field.
After considering the economic
impacts of this final rule on small
entities, I certify that this action will not
have a significant economic impact on
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a substantial number of small entities.
This final rule will not impose any
requirements on small entities. Most of
the emission sources that will be
required by State regulatory agencies
(and federal regulators after 2011) to
conduct tests using the revised methods
are those that have PM emissions of 100
tons per year or more. EPA expects that
few, if any, of these emission sources
will be small entities.
Although this final action will not
have a significant economic impact on
a substantial number of small entities,
EPA nonetheless has tried to reduce the
impact of this final action on small
entities. This final rule does not require
any entities to use these final test
methods. Such a requirement would be
mandated by a separate independent
regulatory action. However, upon
promulgation of this final action, some
entities may be required to use these test
methods as a result of existing permits
or regulations. Since the cost to use the
final test methods is comparable to the
cost of the methods they replace, little
or no significant economic impact to
small entities will accompany the
increased precision and accuracy of the
final test methods. After January 1,
2011, when the transition period
established in the Clean Air Fine
Particle Implementation Rule expires,
States are required to consider inclusion
of pollutants measured by these test
methods in new or revised regulations.
The economic impacts caused by any
new or revised State regulations for fine
PM would be associated with those
State rules and not with this final action
to modify the existing test methods.
Consequently, we believe that this final
action imposes little if any adverse
economic impact to small entities.
D. Unfunded Mandates Reform Act
This rule contains no federal
mandates under the provisions of Title
II of the Unfunded Mandates Reform
Act of 1995 (UMRA), 2 U.S.C. 1531–
1538 for State, local, and tribal
governments or the private sector. The
incremental costs associated with
conducting the revised test methods
(expected to be less than $1,000 per test)
do not impose a significant burden on
sources. Thus, this final action is not
subject to the requirements of sections
202 and 205 of the UMRA.
This rule is also not subject to the
requirements of section 203 of UMRA
because it contains no regulatory
requirements that might significantly or
uniquely affect small governments. The
low incremental cost associated with
the revised test methods mitigates any
significant or unique effects on small
governments.
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E. 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, as specified in
Executive Order 13132. In cases where
a source of PM2.5 emissions is owned by
a State or local government, those
governments may incur minimal
compliance costs associated with
conducting tests to quantify PM2.5
emissions using the revised methods
when they are promulgated. However,
such tests would be conducted at the
discretion of the State or local
government and the compliance costs
are not expected to impose a significant
burden on those governments.
Additionally, the decision to review or
modify existing operating permits to
reflect the CPM measurement
capabilities of the final test methods is
at the discretion of State and local
governments and any effects or costs
arising from such actions are not
required by this rule. Thus, Executive
Order 13132 does not apply to this
action.
F. Executive Order 13175: Consultation
and Coordination With Indian Tribal
Governments
This action does not have tribal
implications, as specified in Executive
Order 13175 (65 FR 67249, November 9,
2000). In cases where a source of PM2.5
emissions is owned by a tribal
government, those governments may
incur minimal compliance costs
associated with conducting tests to
quantify PM2.5 emissions using the
revised methods when they are
promulgated. However, such tests
would be conducted at the discretion of
the tribal government and the
compliance costs are not expected to
impose a significant burden on those
governments. Thus, Executive Order
13175 does not apply to this action.
G. Executive Order 13045: Protection of
Children From Environmental Health
and Safety Risks
EPA interprets Executive Order 13045
(62 FR 19885, April 23, 1997) as
applying only to those regulatory
actions that concern health or safety
risks, such that the analysis required
under section 5–501 of the Executive
Order has the potential to influence the
regulation. This action is not subject to
Executive Order 13045 because it does
not establish an environmental standard
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80133
intended to mitigate health or safety
risks.
H. Executive Order 13211: Actions
Concerning Regulations That
Significantly Affect Energy Supply,
Distribution, or Use
This action is not subject to Executive
Order 13211 (66 FR 28355, May 22,
2001) because it is not a significant
regulatory action under Executive Order
12866.
I. National Technology Transfer and
Advancement Act
Section 12(d) of the National
Technology Transfer and Advancement
Act of 1995 (NTTAA), Public Law 104–
113, 12(d) (15 U.S.C. 272 note) directs
EPA to use voluntary consensus
standards in its regulatory activities
unless to do so would be inconsistent
with applicable law or otherwise
impractical. Voluntary consensus
standards are technical standards (e.g.,
materials specifications, test methods,
sampling procedures, and business
practices) that are developed or adopted
by voluntary consensus standards
bodies. NTTAA directs EPA to provide
Congress, through OMB, explanations
when the Agency decides not to use
available and applicable voluntary
consensus standards.
This action involves technical
standards. EPA has decided to use two
voluntary consensus standards that
were identified at proposal to be
applicable for use within the amended
test methods. The first voluntary
consensus standard cited in proposed
Method 202 was ASTM International
Method D2986–95a (1999), ‘‘Standard
Method for Evaluation of Air, Assay
Media by the Monodisperse DOP
(Dioctyl Phthalate) Smoke Test,’’ for its
procedures to conduct filter efficiency
tests. In the final Method 202, we
replaced the prescriptive requirement to
use a filter meeting ASTM International
D2986–95a (1999) with a performancebased requirement limiting the residual
mass contribution. The performance
based approach specifies that the CPM
filter must be a non-reactive, nondisintegrating filter that does not
contribute more than 0.5 mg of residual
mass to the CPM measurements.
Regarding efficiency, the CPM filter
must have an efficiency of at least 99.95
percent (< 0.05 percent penetration) on
0.3 μm particles.
The second voluntary consensus
standard cited in proposed Method 202
was ASTM International D1193–06,
‘‘Standard Specification for Reagent
Water,’’ for the proper selection of
distilled ultra-filtered water. In response
to public comments, we applied a
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performance-based approach in the final
Method 202 that requires deionized,
ultra-filtered water that contains 1.0
ppmw (1 mg/L) residual mass or less.
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J. Executive Order 12898: Federal
Actions To Address Environmental
Justice in Minority Populations and
Low-Income Populations
Executive Order 12898 (59 FR 7629,
February 16, 1994) establishes federal
executive policy on environmental
justice. Its main provision directs
federal agencies, to the greatest extent
practicable and permitted by law, to
make environmental justice part of their
mission by identifying and addressing,
as appropriate, disproportionately high
and adverse human health or
environmental effects of their programs,
policies, and activities on minority
populations and low-income
populations in the United States.
EPA has determined that this final
rule will not have disproportionately
high and adverse human health or
environmental effects on minority or
low-income populations because it
increases the level of environmental
protection for all affected populations
without having any disproportionately
high and adverse human health or
environmental effects on any
population, including any minority or
low-income population. The final
amendments revise existing test
methods to improve the accuracies of
the measurements that are expected to
improve environmental quality and
reduce health risks for areas that may be
designated as nonattainment.
K. Congressional Review Act
The Congressional Review Act, 5
U.S.C. 801 et seq., as added by the Small
Business Regulatory Enforcement
Fairness Act of 1996, generally provides
that before a rule may take effect, the
agency promulgating the rule must
submit a rule report, which includes a
copy of the rule, to each House of the
Congress and to the Comptroller General
of the United States. Section 808 allows
the issuing agency to make a rule
effective sooner than otherwise
provided by the CRA if the agency
makes a good cause finding that notice
and public procedure is impracticable,
unnecessary or contrary to the public
interest. This determination must be
supported by a brief statement. 5 U.S.C.
808(2). As stated previously, EPA has
made such a good cause finding,
including the reasons therefore, and
established an effective date of January
1, 2011 (see section I.C, supra). EPA will
submit a report containing this rule and
other required information to the U.S.
Senate, the U.S. House of
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Representatives, and the Comptroller
General of the United States prior to
publication of the rule in the Federal
Register. This action is not a ‘‘major
rule’’ as defined by 5 U.S.C. 804(2).
List of Subjects in 40 CFR Part 51
Administrative practice and
procedure, Air pollution control, Carbon
monoxide, Intergovernmental relations,
Lead, Nitrogen oxide, Ozone, PM,
Reporting and recordkeeping
requirements, Sulfur compounds,
Volatile organic compounds.
Dated: December 1, 2010.
Lisa P. Jackson,
Administrator.
For the reasons stated in the preamble,
title 40, chapter I of the Code of Federal
Regulations is amended as follows:
■
PART 51—[AMENDED]
1. The authority citation for part 51
continues to read as follows:
■
Authority: 23 U.S.C. 101; 42 U.S.C 7401–
7671q.
2. Amend appendix M by revising
Methods 201A and 202 to read as
follows:
■
Appendix M to Part 51—Recommended
Test Methods for State Implementation
Plans
*
*
*
*
*
METHOD 201A—DETERMINATION OF
PM10 AND PM2.5 EMISSIONS FROM
STATIONARY SOURCES (Constant
Sampling Rate Procedure)
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 filterable particulate
matter (PM) emissions equal to or less than
a nominal aerodynamic diameter of 10
micrometers (PM10) and 2.5 micrometers
(PM2.5). This method can be used to measure
coarse particles (i.e., the difference between
the measured PM10 concentration and the
measured PM2.5 concentration).
1.2 Applicability. This method addresses
the equipment, preparation, and analysis
necessary to measure filterable PM. You can
use this method to measure filterable PM
from stationary sources only. Filterable PM is
collected in stack with this method (i.e., the
method measures materials that are solid or
liquid at stack conditions). If the gas filtration
temperature exceeds 30 °C (85 °F), then you
may use the procedures in this method to
measure only filterable PM (material that
does not pass through a filter or a cyclone/
filter combination). If the gas filtration
temperature exceeds 30 °C (85 °F), and you
must measure both the filterable and
condensable (material that condenses after
passing through a filter) components of total
primary (direct) PM emissions to the
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atmosphere, then you must combine the
procedures in this method with the
procedures in Method 202 of appendix M to
this part for measuring condensable PM.
However, if the gas filtration temperature
never exceeds 30 °C (85 °F), then use of
Method 202 of appendix M to this part is not
required to measure total primary PM.
1.3 Responsibility. You are responsible
for obtaining the equipment and supplies you
will need to use this method. You must 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
results, you must have a thorough knowledge
of the following test methods found in
appendices A–1 through A–3 of 40 CFR part
60:
(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.
1.5 Limitations. You cannot use this
method to measure emissions in which water
droplets are present because the size
separation of the water droplets may not be
representative of the dry particle size
released into the air. To measure filterable
PM10 and PM2.5 in emissions where water
droplets are known to exist, we recommend
that you use Method 5 of appendix A–3 to
part 60. Because of the temperature limit of
the O-rings used in this sampling train, you
must follow the procedures in Section 8.6.1
to test emissions from stack gas temperatures
exceeding 205 °C (400 °F).
1.6 Conditions. You can use this method
to obtain particle sizing at 10 micrometers
and or 2.5 micrometers if you sample within
80 and 120 percent of isokinetic flow. You
can also use this method to obtain total
filterable particulate if you sample within 90
to 110 percent of isokinetic flow, the number
of sampling points is the same as required by
Method 5 of appendix A–3 to part 60 or
Method 17 of appendix A–6 to part 60, and
the filter temperature is within an acceptable
range for these methods. For Method 5, the
acceptable range for the filter temperature is
generally 120 °C (248 °F) unless a higher or
lower temperature is specified. The
acceptable range varies depending on the
source, control technology and applicable
rule or permit condition. To satisfy Method
5 criteria, you may need to remove the instack filter and use an out-of-stack filter and
recover the PM in the probe between the
PM2.5 particle sizer and the filter. In addition,
to satisfy Method 5 and Method 17 criteria,
you may need to sample from more than 12
traverse points. Be aware that this method
determines in-stack PM10 and PM2.5 filterable
emissions by sampling from a recommended
maximum of 12 sample points, at a constant
flow rate through the train (the constant flow
is necessary to maintain the size cuts of the
cyclones), and with a filter that is at the stack
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temperature. In contrast, Method 5 or Method
17 trains are operated isokinetically with
varying flow rates through the train. Method
5 and Method 17 require sampling from as
many as 24 sample points. Method 5 uses an
out-of-stack filter that is maintained at a
constant temperature of 120 °C (248 °F).
Further, to use this method in place of
Method 5 or Method 17, you must extend the
sampling time so that you collect the
minimum mass necessary for weighing each
portion of this sampling train. Also, if you
are using this method as an alternative to a
test method specified in a regulatory
requirement (e.g., a requirement to conduct a
compliance or performance test), then you
must receive approval from the authority that
established the regulatory requirement before
you conduct the test.
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2.0 Summary of Method
2.1 Summary. To measure PM10 and
PM2.5, extract a sample of gas at a
predetermined constant flow rate through an
in-stack sizing device. The particle-sizing
device separates particles with nominal
aerodynamic diameters of 10 micrometers
and 2.5 micrometers. To minimize variations
in the isokinetic sampling conditions, you
must establish well-defined limits. After a
sample is obtained, remove uncombined
water from the particulate, then use
gravimetric analysis to determine the
particulate mass for each size fraction. The
original method, as promulgated in 1990, has
been changed by adding a PM2.5 cyclone
downstream of the PM10 cyclone. Both
cyclones were developed and evaluated as
part of a conventional five-stage cascade
cyclone train. The addition of a PM2.5
cyclone between the PM10 cyclone and the
stack temperature filter in the sampling train
supplements the measurement of PM10 with
the measurement of PM2.5. Without the
addition of the PM2.5 cyclone, the filterable
particulate portion of the sampling train may
be used to measure total and PM10 emissions.
Likewise, with the exclusion of the PM10
cyclone, the filterable particulate portion of
the sampling train may be used to measure
total and PM2.5 emissions. Figure 1 of Section
17 presents the schematic of the sampling
train configured with this change.
3.0 Definitions
3.1 Condensable particulate matter (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 CPM
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 one percent of total
weight less tare weight, whichever is greater,
between two consecutive weighings, with no
less than six hours of desiccation time
between weighings.
3.3 Filterable particulate matter (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.
3.4 Primary particulate matter (PM) (also
known as direct PM) means particles that
enter the atmosphere as a direct emission
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from a stack or an open source. Primary PM
has two components: Filterable PM and
condensable PM. These two PM components
have no upper particle size limit.
3.5 Primary PM2.5 (also known as direct
PM2.5, total PM2.5, PM2.5, or combined
filterable PM2.5 and condensable PM) means
PM with an aerodynamic diameter less than
or equal to 2.5 micrometers. These solid
particles are emitted directly from an air
emissions source or activity, or are the
gaseous or vaporous emissions 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).
3.6 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.
4.0 Interferences
You cannot use this method to measure
emissions where water droplets are present
because the size separation of the water
droplets may not be representative of the dry
particle size released into the air. Stacks with
entrained moisture droplets may have water
droplets larger than the cut sizes for the
cyclones. These water droplets normally
contain particles and dissolved solids that
become PM10 and PM2.5 following
evaporation of the water.
5.0 Safety
5.1 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
Figure 2 of Section 17 shows details of the
combined cyclone heads used in this
method. The sampling train is the same as
Method 17 of appendix A–6 to part 60 with
the exception of the PM10 and PM2.5 sizing
devices. The following sections describe the
sampling train’s primary design features in
detail.
6.1 Filterable Particulate Sampling Train
Components.
6.1.1 Nozzle. You must use stainless steel
(316 or equivalent) or fluoropolymer-coated
stainless steel nozzles with a sharp tapered
leading edge. We recommend one of the 12
nozzles listed in Figure 3 of Section 17
because they meet design specifications
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80135
when PM10 cyclones are used as part of the
sampling train. We also recommend that you
have a large number of nozzles in small
diameter increments available to increase the
likelihood of using a single nozzle for the
entire traverse. We recommend one of the
nozzles listed in Figure 4A or 4B of Section
17 because they meet design specifications
when PM2.5 cyclones are used without PM10
cyclones as part of the sampling train.
6.1.2 PM10 and PM2.5 Sizing Device.
6.1.2.1 Use stainless steel (316 or
equivalent) or fluoropolymer-coated PM10
and PM2.5 sizing devices. You may use sizing
devices constructed of high-temperature
specialty metals such as Inconel, Hastelloy,
or Haynes 230. (See also Section 8.6.1.) The
sizing devices must be cyclones that meet the
design specifications shown in Figures 3, 4A,
4B, 5, and 6 of Section 17. Use a caliper to
verify that the dimensions of the PM10 and
PM2.5 sizing devices are within ± 0.02 cm of
the design specifications. Example suppliers
of PM10 and PM2.5 sizing devices include the
following:
(a) Environmental Supply Company, Inc.,
2142 E. Geer Street, Durham, North Carolina
27704. Telephone No.: (919) 956–9688; Fax:
(919) 682–0333.
(b) Apex Instruments, 204 Technology Park
Lane, Fuquay-Varina, North Carolina 27526.
Telephone No.: (919) 557–7300 (phone); Fax:
(919) 557–7110.
6.1.2.2 You may use alternative particle
sizing devices if they meet the requirements
in Development and Laboratory Evaluation of
a Five-Stage Cyclone System, EPA–600/7–
78–008 (https://cfpub.epa.gov/ols).
6.1.3 Filter Holder. Use a filter holder
that is stainless steel (316 or equivalent). A
heated glass filter holder may be substituted
for the steel filter holder when filtration is
performed out-of-stack. Commercial-size
filter holders are available depending upon
project requirements, including commercial
stainless steel filter holders to support 25-,
47-, 63-, 76-, 90-, 101-, and 110-mm diameter
filters. Commercial size filter holders contain
a fluoropolymer O-ring, a stainless steel
screen that supports the particulate filter, and
a final fluoropolymer O-ring. Screw the
assembly together and attach to the outlet of
cyclone IV. The filter must not be
compressed between the fluoropolymer Oring and the filter housing.
6.1.4 Pitot Tube. You must use a pitot
tube made of heat resistant tubing. Attach the
pitot tube to the probe with stainless steel
fittings. Follow the specifications for the
pitot tube and its orientation to the inlet
nozzle given in Section 6.1.1.3 of Method 5
of appendix A–3 to part 60.
6.1.5 Probe Extension and Liner. The
probe extension must be glass- or
fluoropolymer-lined. Follow the
specifications in Section 6.1.1.2 of Method 5
of appendix A–3 to part 60. If the gas
filtration temperature never exceeds 30 °C
(85 °F), then the probe may be constructed
of stainless steel without a probe liner and
the extension is not recovered as part of the
PM.
6.1.6 Differential Pressure Gauge,
Condensers, Metering Systems, Barometer,
and Gas Density Determination Equipment.
Follow the requirements in Sections 6.1.1.4
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through 6.1.3 of Method 5 of appendix A–3
to part 60, as applicable.
6.2 Sample Recovery Equipment.
6.2.1 Filterable Particulate Recovery. Use
the following equipment to quantitatively
determine the amount of filterable PM
recovered from the sampling train.
(a) Cyclone and filter holder brushes.
(b) Wash bottles. Two wash bottles are
recommended. 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.
(c) 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.
(d) Petri dishes. For filter samples; glass or
polyethylene, unless otherwise specified by
the Administrator.
(e) Graduated cylinders. To measure
condensed water to within 1 ml or 0.5 g.
Graduated cylinders must have subdivisions
not greater than 2 ml.
(f) Plastic storage containers. Air-tight
containers to store silica gel.
6.2.2 Analysis Equipment.
(a) Funnel. Glass or polyethylene, to aid in
sample recovery.
(b) Rubber policeman. To aid in transfer of
silica gel to container; not necessary if silica
gel is weighed in the field.
(c) Analytical balance. Analytical balance
capable of weighing at least 0.0001 g (0.1
mg).
(d) Balance. To determine the weight of the
moisture in the sampling train components,
use an analytical balance accurate to ± 0.5 g.
(e) Fluoropolymer beaker liners.
7.0 Reagents, Standards, and Sampling
Media
7.1 Sample Collection. To collect a
sample, you will need a filter and silica gel.
You must also have water and crushed ice.
These items must meet the following
specifications.
7.1.1 Filter. Use a nonreactive,
nondisintegrating glass fiber, quartz, or
polymer filter that does not a have an organic
binder. The 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 PM filter efficiency.
7.1.2 Silica Gel. Use an indicating-type
silica gel of 6 to 16 mesh. You must obtain
approval from the regulatory authority that
established the requirement to use this test
method to use other types of desiccants
(equivalent or better) before you use them.
Allow the silica gel to dry for two 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 is active for moisture
collection.
7.1.3 Crushed Ice. Obtain from the best
readily available source.
7.1.4 Water. Use deionized, ultra-filtered
water that contains 1.0 part per million by
weight (1 milligram/liter) residual mass or
less to recover and extract samples.
7.2 Sample Recovery and Analytical
Reagents. You will need acetone and
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anhydrous calcium sulfate 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 will likely
produce a high residue in the laboratory and
field reagent blanks. You must use acetone
with blank values less than 1 part per million
by weight residue. Analyze acetone blanks
prior to field use to confirm low blank
values. In no case shall a blank value of
greater than 0.0001 percent (1 part per
million by weight) of the weight of acetone
used in sample recovery be subtracted from
the sample weight (i.e., the maximum blank
correction is 0.1 mg per 100 ml of acetone
used to recover samples).
7.2.2 Particulate Sample Desiccant. Use
indicating-type anhydrous calcium sulfate to
desiccate samples prior to weighing.
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 instack filtration systems (such as cyclones,
impactors, and thimbles) and impinger and
moisture train systems.
8.2 Preparations. Follow the pretest
preparation instructions in Section 8.1 of
Method 5 of appendix A–3 to part 60.
8.3 Site Setup. You must complete the
following to properly set up for this test:
(a) Determine the sampling site location
and traverse points.
(b) Calculate probe/cyclone blockage.
(c) Verify the absence of cyclonic flow.
(d) Complete a preliminary velocity profile
and select a nozzle(s) and sampling rate.
8.3.1 Sampling Site Location and
Traverse Point Determination. 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.
(a) Traverse points. The required maximum
number of total traverse points at any
location is 12, as shown in Figure 7 of
Section 17. 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 36.4 inches in
diameter with the pitot tube and 32.4 inches
without the pitot tube). During sampling,
when the PM2.5 cyclone is used without the
PM10, traverse points closest to the stack
walls may not be reached because the inlet
to a PM2.5 cyclone is located approximately
2.75 inches from the end of the cyclone. For
these cases, you may collect samples using
the procedures in Section 11.3.2.2 of Method
1 of appendix A–3 to part 60. You must use
the traverse point closest to the unreachable
sampling points as replacement for the
unreachable points. You must extend the
sampling time at the replacement sampling
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point to include the duration of the
unreachable traverse points.
(b) Round or rectangular duct or stack. If
a duct or stack is round with two ports
located 90° apart, use six sampling points on
each diameter. Use a 3x4 sampling point
layout for rectangular ducts or stacks.
Consult with the Administrator to receive
approval for other layouts before you use
them.
(c) Sampling ports. You must determine if
the sampling ports can accommodate the instack cyclones used in this method. You may
need larger diameter sampling ports than
those used by Method 5 of appendix A–3 to
part 60 or Method 17 of appendix A–6 to part
60 for total filterable particulate sampling.
When you use nozzles smaller than 0.16 inch
in diameter and either a PM10 or a combined
PM10 and PM2.5 sampling apparatus, the
sampling port diameter may need to be six
inches in diameter to accommodate the entire
apparatus because the conventional 4-inch
diameter port may be too small due to the
combined dimension of the PM10 cyclone
and the nozzle extending from the cyclone,
which will likely exceed the internal
diameter of the port. A 4-inch port should be
adequate for the single PM2.5 sampling
apparatus. However, do not use the
conventional 4-inch diameter port in any
circumstances in which the combined
dimension of the cyclone and the nozzle
extending from the cyclone exceeds the
internal diameter of the port. (Note: If the
port nipple is short, you may be able to
‘‘hook’’ the sampling head through a smaller
port into the duct or stack.)
8.3.2 Probe/Cyclone Blockage
Calculations. Follow the procedures in the
next two sections, as appropriate.
8.3.2.1 Ducts with diameters greater than
36.4 inches. Based on commercially available
cyclone assemblies for this procedure, ducts
with diameters greater than 36.4 inches have
blockage effects less than three percent, as
illustrated in Figure 8 of Section 17. You
must minimize the blockage effects of the
combination of the in-stack nozzle/cyclones,
pitot tube, and filter assembly that you use
by keeping the cross-sectional area of the
assembly at three percent or less of the crosssectional area of the duct.
8.3.2.2 Ducts with diameters between
25.7 and 36.4 inches. Ducts with diameters
between 25.7 and 36.4 inches have blockage
effects ranging from three to six percent, as
illustrated in Figure 8 of Section 17.
Therefore, when you conduct tests on these
small ducts, you must adjust the observed
velocity pressures for the estimated blockage
factor whenever the combined sampling
apparatus blocks more than three percent of
the stack or duct (see Sections 8.7.2.2 and
8.7.2.3 on the probe blockage factor and the
final adjusted velocity pressure,
respectively). (Note: Valid sampling with the
combined PM2.5/PM10 cyclones cannot be
performed with this method if the average
stack blockage from the sampling assembly is
greater than six percent, i.e., the stack
diameter is less than 26.5 inches.)
8.3.3 Cyclonic Flow. Do not use the
combined cyclone sampling head at sampling
locations subject to cyclonic flow. Also, you
must follow procedures in Method 1 of
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appendix A–1 to part 60 to determine the
presence or absence of cyclonic flow and
then perform the following calculations:
(a) As per Section 11.4 of Method 1 of
appendix A–1 to part 60, find and record the
angle that has a null velocity pressure for
each traverse point using an S-type pitot
tube.
(b) Average the absolute values of the
angles that have a null velocity pressure. Do
not use the sampling location if the average
absolute value exceeds 20°. (Note: You can
minimize the effects of cyclonic flow
conditions by moving the sampling location,
placing gas flow straighteners upstream of
the sampling location, or applying a modified
sampling approach as described in EPA
Guideline Document GD–008, Particulate
Emissions Sampling in Cyclonic Flow. You
may need to obtain an alternate method
approval from the regulatory authority that
established the requirement to use this test
method prior to using a modified sampling
approach.)
8.3.4 Preliminary Velocity Profile.
Conduct a preliminary velocity traverse by
following Method 2 of appendix A–1 to part
60 velocity traverse procedures. The purpose
of the preliminary velocity profile is to
determine all of the following:
(a) The gas sampling rate for the combined
probe/cyclone sampling head in order to
meet the required particle size cut.
(b) The appropriate nozzle to maintain the
required gas sampling rate for the velocity
pressure range and isokinetic range. If the
isokinetic range cannot be met (e.g., batch
processes, extreme process flow or
temperature variation), void the sample or
use methods subject to the approval of the
Administrator to correct the data. The
acceptable variation from isokinetic sampling
is 80 to 120 percent and no more than 100
± 29 percent (two out of 12 or five out of 24)
sampling points outside of this criteria.
(c) The necessary sampling duration to
obtain sufficient particulate catch weights.
8.3.4.1 Preliminary traverse. You must
use an S-type pitot tube with a conventional
thermocouple to conduct the traverse.
Conduct the preliminary traverse as close as
possible to the anticipated testing time on
sources that are subject to hour-by-hour gas
flow rate variations of approximately ± 20
percent and/or gas temperature variations of
approximately ± 10 °C (± 50 °F). (Note: You
should be aware that these variations can
cause errors in the cyclone cut diameters and
the isokinetic sampling velocities.)
8.3.4.2 Velocity pressure range. Insert the
S-type pitot tube at each traverse point and
record the range of velocity pressures
measured on data form in Method 2 of
appendix A–1 to part 60. You will use this
later to select the appropriate nozzle.
8.3.4.3 Initial gas stream viscosity and
molecular weight. Determine the average gas
temperature, average gas oxygen content,
average carbon dioxide content, and
estimated moisture content. You will use this
information to calculate the initial gas stream
viscosity (Equation 3) and molecular weight
(Equations 1 and 2). (Note: You must follow
the instructions outlined in Method 4 of
appendix A–3 to part 60 or Alternative
Moisture Measurement Method Midget
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Impingers (ALT–008) to estimate the
moisture content. You may use a wet bulbdry bulb measurement or hand-held
hygrometer measurement to estimate the
moisture content of sources with gas
temperatures less than 71 °C (160 °F).)
8.3.4.4 Approximate PM concentration in
the gas stream. Determine the approximate
PM concentration for the PM2.5 and the PM2.5
to PM10 components of the gas stream
through qualitative measurements or
estimates from precious stack particulate
emissions tests. Having an idea of the
particulate concentration in the gas stream is
not essential but will help you determine the
appropriate sampling time to acquire
sufficient PM weight for better accuracy at
the source emission level. The collectable PM
weight requirements depend primarily on the
types of filter media and weighing
capabilities that are available and needed to
characterize the emissions. Estimate the
collectable PM concentrations in the greater
than 10 micrometer, less than or equal to 10
micrometers and greater than 2.5
micrometers, and less than or equal to 2.5
micrometer size ranges. Typical PM
concentrations are listed in Table 1 of
Section 17. Additionally, relevant sections of
AP–42, Compilation of Air Pollutant
Emission Factors, may contain particle size
distributions for processes characterized in
those sections, and appendix B2 of AP–42
contains generalized particle size
distributions for nine industrial process
categories (e.g., stationary internal
combustion engines firing gasoline or diesel
fuel, calcining of aggregate or unprocessed
ores). The generalized particle size
distributions can be used if source-specific
particle size distributions are unavailable.
Appendix B2 of AP–42 also contains typical
collection efficiencies of various particulate
control devices and example calculations
showing how to estimate uncontrolled total
particulate emissions, uncontrolled sizespecific emissions, and controlled sizespecific particulate emissions. (https://
www.epa.gov/ttnchie1/ap42.)
8.4 Pre-test Calculations. You must
perform pre-test calculations to help select
the appropriate gas sampling rate through
cyclone I (PM10) and cyclone IV (PM2.5).
Choosing the appropriate sampling rate will
allow you to maintain the appropriate
particle cut diameters based upon
preliminary gas stream measurements, as
specified in Table 2 of Section 17.
8.4.1 Gas Sampling Rate. The gas
sampling rate is defined by the performance
curves for both cyclones, as illustrated in
Figure 10 of Section 17. You must use the
calculations in Section 8.5 to achieve the
appropriate cut size specification for each
cyclone. The optimum gas sampling rate is
the overlap zone defined as the range below
the cyclone IV 2.25 micrometer curve down
to the cyclone I 11.0 micrometer curve (area
between the two dark, solid lines in Figure
10 of Section 17).
8.4.2 Choosing the Appropriate Sampling
Rate. You must select a gas sampling rate in
the middle of the overlap zone (discussed in
Section 8.4.1), as illustrated in Figure 10 of
Section 17, to maximize the acceptable
tolerance for slight variations in flow
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characteristics at the sampling location. The
overlap zone is also a weak function of the
gas composition. (Note: The acceptable range
is limited, especially for gas streams with
temperatures less than approximately 100 °F.
At lower temperatures, it may be necessary
to perform the PM10 and PM2.5 separately in
order to meet the necessary particle size
criteria shown in Table 2 of Section 17.)
8.5 Test Calculations. You must perform
all of the calculations in Table 3 of Section
17 and the calculations described in Sections
8.5.1 through 8.5.5.
8.5.1 Assumed Reynolds Number. You
must select an assumed Reynolds number
(Nre) using Equation 10 and an estimated
sampling rate or from prior experience under
the stack conditions determined using
Methods 1 through 4 to part 60. You will
perform initial test calculations based on an
assumed Nre for the test to be performed. You
must verify the assumed Nre by substituting
the sampling rate (Qs) calculated in Equation
7 into Equation 10. Then use Table 5 of
Section 17 to determine if the Nre used in
Equation 5 was correct.
8.5.2 Final Sampling Rate. Recalculate
the final Qs if the assumed Nre used in your
initial calculation is not correct. Use
Equation 7 to recalculate the optimum Qs.
8.5.3 Meter Box DH. Use Equation 11 to
calculate the meter box orifice pressure drop
(DH) after you calculate the optimum
sampling rate and confirm the Nre. (Note: The
stack gas temperature may vary during the
test, which could affect the sampling rate. If
the stack gas temperature varies, you must
make slight adjustments in the meter box DH
to maintain the correct constant cut
diameters. Therefore, use Equation 11 to
recalculate the DH values for 50 °F above and
below the stack temperature measured during
the preliminary traverse (see Section 8.3.4.1),
and document this information in Table 4 of
Section 17.)
8.5.4 Choosing a Sampling Nozzle. Select
one or more nozzle sizes to provide for near
isokinetic sampling rate (see Section 1.6).
This will also minimize an isokinetic
sampling error for the particles at each point.
First calculate the mean stack gas velocity
(vs) using Equation 13. See Section 8.7.2 for
information on correcting for blockage and
use of different pitot tube coefficients. Then
use Equation 14 to calculate the diameter (D)
of a nozzle that provides for isokinetic
sampling at the mean vs at flow Qs. From the
available nozzles one size smaller and one
size larger than this diameter, D, select the
most appropriate nozzle. Perform the
following steps for the selected nozzle.
8.5.4.1 Minimum/maximum nozzle/stack
velocity ratio. Use Equation 15 to determine
the velocity of gas in the nozzle. Use
Equation 16 to calculate the minimum
nozzle/stack velocity ratio (Rmin). Use
Equation 17 to calculate the maximum
nozzle/stack velocity ratio (Rmax).
8.5.4.2 Minimum gas velocity. Use
Equation 18 to calculate the minimum gas
velocity (vmin) if Rmin is an imaginary number
(negative value under the square root
function) or if Rmin is less than 0.5. Use
Equation 19 to calculate vmin if Rmin is ≥ 0.5.
8.5.4.3 Maximum stack velocity. Use
Equation 20 to calculate the maximum stack
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velocity (vmax) if Rmax is less than 1.5. Use
Equation 21 to calculate the stack velocity if
Rmax is ≥ 1.5.
8.5.4.4 Conversion of gas velocities to
velocity pressure. Use Equation 22 to convert
vmin to minimum velocity pressure, Dpmin.
Use Equation 23 to convert vmax to maximum
velocity pressure, Dpmax.
8.5.4.5 Comparison to observed velocity
pressures. Compare minimum and maximum
velocity pressures with the observed velocity
pressures at all traverse points during the
preliminary test (see Section 8.3.4.2).
8.5.5 Optimum Sampling Nozzle. The
nozzle you selected is appropriate if all the
observed velocity pressures during the
preliminary test fall within the range of the
Dpmin and Dpmax. Make sure the following
requirements are met then follow the
procedures in Sections 8.5.5.1 and 8.5.5.2.
(a) Choose an optimum nozzle that
provides for isokinetic sampling conditions
as close to 100 percent as possible. This is
prudent because even if there are slight
variations in the gas flow rate, gas
temperature, or gas composition during the
actual test, you have the maximum assurance
of satisfying the isokinetic criteria. Generally,
one of the two candidate nozzles selected
will be closer to optimum (see Section 8.5.4).
(b) When testing is for PM2.5 only, you are
allowed a 16 percent failure rate, rounded to
the nearest whole number, of sampling
points that are outside the range of the Dpmin
and Dpmax. If the coarse fraction for PM10
determination is included, you are allowed
only an eight percent failure rate of the
sampling points, rounded to the nearest
whole number, outside the Dpmin and Dpmax.
8.5.5.1 Precheck. Visually check the
selected nozzle for dents before use.
8.5.5.2 Attach the pre-selected nozzle.
Screw the pre-selected nozzle onto the main
body of cyclone I using fluoropolymer tape.
Use a union and cascade adaptor to connect
the cyclone IV inlet to the outlet of cyclone
I (see Figure 2 of Section 17).
8.6 Sampling Train Preparation. A
schematic of the sampling train used in this
method is shown in Figure 1 of Section 17.
First, assemble the train and complete the
leak check on the combined cyclone
sampling head and pitot tube. Use the
following procedures to prepare the sampling
train. (Note: Do not contaminate the sampling
train during preparation and assembly. Keep
all openings, where contamination can occur,
covered until just prior to assembly or until
sampling is about to begin.)
8.6.1 Sampling Head and Pitot Tube.
Assemble the combined cyclone train. The
O-rings used in the train have a temperature
limit of approximately 205 °C (400 °F). Use
cyclones with stainless steel sealing rings for
stack temperatures above 205 °C (400 °F) up
to 260 °C (500 °F). You must also keep the
nozzle covered to protect it from nicks and
scratches. This method may not be suitable
for sources with stack gas temperatures
exceeding 260 °C (500 °F) because the
threads of the cyclone components may gall
or seize, thus preventing the recovery of the
collected PM and rendering the cyclone
unusable for subsequent use. You may use
stainless steel cyclone assemblies
constructed with bolt-together rather than
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screw-together assemblies at temperatures up
to 538 °C (1,000 °F). You must use ‘‘breakaway’’ or expendable stainless steel bolts that
can be over-torqued and broken if necessary
to release cyclone closures, thus allowing
you to recover PM without damaging the
cyclone flanges or contaminating the
samples. You may need to use specialty
metals to achieve reliable particulate mass
measurements above 538 °C (1,000 °F). The
method can be used at temperatures up to
1,371 °C (2,500 °F) using specially
constructed high-temperature stainless steel
alloys (Hastelloy or Haynes 230) with bolttogether closures using break-away bolts.
8.6.2 Filterable Particulate Filter Holder
and Pitot Tube. Attach the pre-selected filter
holder to the end of the combined cyclone
sampling head (see Figure 2 of Section 17).
Attach the S-type pitot tube to the combined
cyclones after the sampling head is fully
attached to the end of the probe. (Note: The
pitot tube tip must be mounted slightly
beyond the combined head cyclone sampling
assembly and at least one inch off the gas
flow path into the cyclone nozzle. This is
similar to the pitot tube placement in Method
17 of appendix A–6 to part 60.) Securely
fasten the sensing lines to the outside of the
probe to ensure proper alignment of the pitot
tube. Provide unions on the sensing lines so
that you can connect and disconnect the
S-type pitot tube tips from the combined
cyclone sampling head before and after each
run. Calibrate the pitot tube on the sampling
head according to the most current ASTM
International D3796 because the cyclone
body is a potential source flow disturbance
and will change the pitot coefficient value
from the baseline (isolated tube) value.
8.6.3 Filter. You must number and tare
the filters before use. To tare the filters,
desiccate each filter at 20 ± 5.6 °C (68 ±
10 °F) and ambient pressure for at least 24
hours and weigh at intervals of at least six
hours to a constant weight. (See Section 3.0
for a definition of constant weight.) Record
results to the nearest 0.1 mg. During each
weighing, the filter must not be exposed to
the laboratory atmosphere for longer than
two minutes and a relative humidity above
50 percent. Alternatively, the filters may be
oven-dried at 104 °C (220 °F) for two to three
hours, desiccated for two hours, and
weighed. Use tweezers or clean disposable
surgical gloves to place a labeled (identified)
and pre-weighed filter in the filter holder.
You must center the filter and properly place
the gasket so that the sample gas stream will
not circumvent the filter. The filter must not
be compressed between the gasket and the
filter housing. Check the filter for tears after
the assembly is completed. Then screw or
clamp the filter housing together to prevent
the seal from leaking.
8.6.4 Moisture Trap. If you are measuring
only filterable particulate (or you are sure
that the gas filtration temperature will be
maintained below 30 °C (85 °F)), then an
empty modified Greenburg Smith impinger
followed by an impinger containing silica gel
is required. Alternatives described in Method
5 of appendix A–3 to part 60 may also be
used to collect moisture that passes through
the ambient filter. If you are measuring
condensable PM in combination with this
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method, then follow the procedures in
Method 202 of appendix M of this part for
moisture collection.
8.6.5 Leak Check. Use the procedures
outlined in Section 8.4 of Method 5 of
appendix A–3 to part 60 to leak check the
entire sampling system. Specifically perform
the following procedures:
8.6.5.1 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 four 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.
Enter the leak check results on the analytical
data sheet (see Section 11.1) for the specific
test. (Note: Do not conduct a leak check
during port changes.)
8.6.5.2 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 of appendix A–3 to part 60.
8.6.6 Sampling Head. You must preheat
the combined sampling head to the stack
temperature of the gas stream at the test
location (± 10 °C, ± 50 °F). This will heat the
sampling head and prevent moisture from
condensing from the sample gas stream.
8.6.6.1 Warmup. You must complete a
passive warmup (of 30–40 min) within the
stack before the run begins to avoid internal
condensation.
8.6.6.2 Shortened warmup. You can
shorten the warmup time by thermostated
heating outside the stack (such as by a heat
gun). Then place the heated sampling head
inside the stack and allow the temperature to
equilibrate.
8.7 Sampling Train Operation. Operate
the sampling train the same as described in
Section 4.1.5 of Method 5 of appendix A–3
to part 60, but use the procedures in this
section for isokinetic sampling and flow rate
adjustment. Maintain the flow rate calculated
in Section 8.4.1 throughout the run, provided
the stack temperature is within 28 °C (50 °F)
of the temperature used to calculate DH. If
stack temperatures vary by more than 28 °C
(50 °F), use the appropriate DH value
calculated in Section 8.5.3. Determine the
minimum number of traverse points as in
Figure 7 of Section 17. Determine the
minimum total projected sampling time
based on achieving the data quality
objectives or emission limit of the affected
facility. We recommend that you round the
number of minutes sampled at each point to
the nearest 15 seconds. Perform the following
procedures:
8.7.1 Sample Point Dwell Time. You
must calculate the flow rate-weighted dwell
time (that is, sampling time) for each
sampling point to ensure that the overall run
provides a velocity-weighted average that is
representative of the entire gas stream. Vary
the dwell time at each traverse point
proportionately with the point velocity.
Calculate the dwell time at each of the
traverse points using Equation 24. You must
use the data from the preliminary traverse to
determine the average velocity pressure
(Dpavg). You must use the velocity pressure
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measured during the sampling run to
determine the velocity pressure at each point
(Dpn). Here, Ntp equals the total number of
traverse points. Each traverse point must
have a dwell time of at least two minutes.
8.7.2 Adjusted Velocity Pressure. When
selecting your sampling points using your
preliminary velocity traverse data, your
preliminary velocity pressures must be
adjusted to take into account the increase in
velocity due to blockage. Also, you must
adjust your preliminary velocity data for
differences in pitot tube coefficients. Use the
following instructions to adjust the
preliminary velocity pressure.
8.7.2.1 Different pitot tube coefficient.
You must use Equation 25 to correct the
recorded preliminary velocity pressures if the
pitot tube mounted on the combined cyclone
sampling head has a different pitot tube
coefficient than the pitot tube used during
the preliminary velocity traverse (see Section
8.3.4).
8.7.2.2 Probe blockage factor. You must
use Equation 26 to calculate an average probe
blockage correction factor (bf) if the diameter
of your stack or duct is between 25.7 and
36.4 inches for the combined PM2.5/PM10
sampling head and pitot and between 18.8
and 26.5 inches for the PM2.5 cyclone and
pitot. A probe blockage factor is calculated
because of the flow blockage caused by the
relatively large cross-sectional area of the
cyclone sampling head, as discussed in
Section 8.3.2.2 and illustrated in Figures 8
and 9 of Section 17. You must determine the
cross-sectional area of the cyclone head you
use and determine its stack blockage factor.
(Note: Commercially-available sampling
heads (including the PM10 cyclone, PM2.5
cyclone, pitot and filter holder) have a
projected area of approximately 31.2 square
inches when oriented into the gas stream. As
the probe is moved from the most outer to
the most inner point, the amount of blockage
that actually occurs ranges from
approximately 13 square inches to the full
31.2 inches plus the blockage caused by the
probe extension. The average cross-sectional
area blocked is 22 square inches.)
8.7.2.3 Final adjusted velocity pressure.
Calculate the final adjusted velocity pressure
(Dps2) using Equation 27. (Note: Figures 8 and
9 of Section 17 illustrate that the blockage
effect of the combined PM10, PM2.5 cyclone
sampling head, and pitot tube increases
rapidly below stack diameters of 26.5 inches.
Therefore, the combined PM10, PM2.5 filter
sampling head and pitot tube is not
applicable for stacks with a diameter less
than 26.5 inches because the blockage is
greater than six percent. For stacks with a
diameter less than 26.5 inches, PM2.5
particulate measurements may be possible
using only a PM2.5 cyclone, pitot tube, and
in-stack filter. If the blockage exceeds three
percent but is less than six percent, you must
follow the procedures outlined in Method 1A
of appendix A–1 to part 60 to conduct tests.
You must conduct the velocity traverse
downstream of the sampling location or
immediately before the test run.
8.7.3 Sample Collection. Collect samples
the same as described in Section 4.1.5 of
Method 5 of appendix A–3 to part 60, except
use the procedures in this section for
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isokinetic sampling and flow rate adjustment.
Maintain the flow rate calculated in Section
8.5 throughout the run, provided the stack
temperature is within 28 °C (50 °F) of the
temperature used to calculate DH. If stack
temperatures vary by more than 28 °C (50 °F),
use the appropriate DH value calculated in
Section 8.5.3. Calculate the dwell time at
each traverse point as in Equation 24. In
addition to these procedures, you must also
use running starts and stops if the static
pressure at the sampling location is less than
minus 5 inches water column. This prevents
back pressure from rupturing the sample
filter. If you use a running start, adjust the
flow rate to the calculated value after you
perform the leak check (see Section 8.4).
8.7.3.1 Level and zero manometers.
Periodically check the level and zero point of
the manometers during the traverse.
Vibrations and temperature changes may
cause them to drift.
8.7.3.2 Portholes. Clean the portholes
prior to the test run. This will minimize the
chance of collecting deposited material in the
nozzle.
8.7.3.3 Sampling procedures. Verify that
the combined cyclone sampling head
temperature is at stack temperature. You
must maintain the temperature of the cyclone
sampling head within ± 10 °C (± 18 °F) of the
stack temperature. (Note: For many stacks,
portions of the cyclones and filter will be
external to the stack during part of the
sampling traverse. Therefore, you must heat
and/or insulate portions of the cyclones and
filter that are not within the stack in order
to maintain the sampling head temperature at
the stack temperature. Maintaining the
temperature will ensure proper particle
sizing and prevent condensation on the walls
of the cyclones.) To begin sampling, remove
the protective cover from the nozzle. Position
the probe at the first sampling point with the
nozzle pointing directly into the gas stream.
Immediately start the pump and adjust the
flow to calculated isokinetic conditions.
Ensure the probe/pitot tube assembly is
leveled. (Note: When the probe is in position,
block off the openings around the probe and
porthole to prevent unrepresentative dilution
of the gas stream. Take care to minimize
contamination from material used to block
the flow or insulate the sampling head during
collection at the first sampling point.)
(a) Traverse the stack cross-section, as
required by Method 1 of appendix A–1 to
part 60, with the exception that you are only
required to perform a 12-point traverse. Do
not bump the cyclone nozzle into the stack
walls when sampling near the walls or when
removing or inserting the probe through the
portholes. This will minimize the chance of
extracting deposited materials.
(b) Record the data required on the field
test data sheet for each run. Record the initial
dry gas meter reading. Then take dry gas
meter readings at the following times: the
beginning and end of each sample time
increment; when changes in flow rates are
made; and when sampling is halted. Compare
the velocity pressure measurements
(Equations 22 and 23) with the velocity
pressure measured during the preliminary
traverse. Keep the meter box DH at the value
calculated in Section 8.5.3 for the stack
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temperature that is observed during the test.
Record all point-by-point data and other
source test parameters on the field test data
sheet. Do not leak check the sampling system
during port changes.
(c) Maintain flow until the sampling head
is completely removed from the sampling
port. You must restart the sampling flow
prior to inserting the sampling head into the
sampling port during port changes.
(d) Maintain the flow through the sampling
system at the last sampling point. At the
conclusion of the test, remove the pitot tube
and combined cyclone sampling head from
the stack while the train is still operating
(running stop). Make sure that you do not
scrape the pitot tube or the combined cyclone
sampling head against the port or stack walls.
Then stop the pump and record the final dry
gas meter reading and other test parameters
on the field test data sheet. (Note: After you
stop the pump, make sure you keep the
combined cyclone head level to avoid tipping
dust from the cyclone cups into the filter
and/or down-comer lines.)
8.7.4 Process Data. You must document
data and information on the process unit
tested, the particulate control system used to
control emissions, any non-particulate
control system that may affect particulate
emissions, the sampling train conditions, and
weather conditions. Record the site
barometric pressure and stack pressure on
the field test data sheet. Discontinue the test
if the operating conditions may cause nonrepresentative particulate emissions.
8.7.4.1 Particulate control system data.
Use the process and control system data to
determine whether representative operating
conditions were maintained throughout the
testing period.
8.7.4.2 Sampling train data. Use the
sampling train data to confirm that the
measured particulate emissions are accurate
and complete.
8.7.5 Sample Recovery. First remove the
sampling head (combined cyclone/filter
assembly) from the train probe. After the
sample head is removed, perform a post-test
leak check of the probe and sample train.
Then recover the components from the
cyclone/filter. Refer to the following sections
for more detailed information.
8.7.5.1 Remove sampling head. After
cooling and when the probe can be safely
handled, wipe off all external surfaces near
the cyclone nozzle and cap the inlet to the
cyclone to prevent PM from entering the
assembly. Remove the combined cyclone/
filter sampling head from the probe. Cap the
outlet of the filter housing to prevent PM
from entering the assembly.
8.7.5.2 Leak check probe/sample train
assembly (post-test). Leak check the
remainder of the probe and sample train
assembly (including meter box) after
removing the combined cyclone head/filter.
You must conduct the leak rate at a vacuum
equal to or greater than the maximum
vacuum achieved during the test run. Enter
the results of the leak check onto the field
test data sheet. If the leak rate of the sampling
train (without the combined cyclone
sampling head) exceeds 0.02 actual cubic feet
per minute or four percent of the average
sampling rate during the test run (whichever
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is less), the run is invalid and must be
repeated.
8.7.5.3 Weigh or measure the volume of
the liquid collected in the water collection
impingers and silica trap. Measure the liquid
in the first impingers to within 1 ml using a
clean graduated cylinder or by weighing it to
within 0.5 g using a balance. Record the
volume of the liquid or weight of the liquid
present to be used to calculate the moisture
content of the effluent gas.
8.7.5.4 Weigh the silica impinger. If a
balance is available in the field, weigh the
silica impinger to within 0.5 g. Note the color
of the indicating silica gel in the last
impinger to determine whether it has been
completely spent and make a notation of its
condition. If you are measuring CPM in
combination with this method, the weight of
the silica gel can be determined before or
after the post-test nitrogen purge is complete
(See Section 8.5.3 of Method 202 of appendix
M to this part).
8.7.5.5 Recovery of PM. Recovery
involves the quantitative transfer of particles
in the following size range: greater than 10
micrometers; less than or equal to 10
micrometers but greater than 2.5
micrometers; and less than or equal to 2.5
micrometers. You must use a nylon or
fluoropolymer brush and an acetone rinse to
recover particles from the combined cyclone/
filter sampling head. Use the following
procedures for each container:
(a) Container #1, Less than or equal to
PM2.5 micrometer filterable particulate. Use
tweezers and/or clean disposable surgical
gloves to remove the filter from the filter
holder. Place the filter in the Petri dish that
you labeled with the test identification and
Container #1. Using a dry brush and/or a
sharp-edged blade, carefully transfer any PM
and/or filter fibers that adhere to the filter
holder gasket or filter support screen to the
Petri dish. Seal the container. This container
holds particles less than or equal to 2.5
micrometers that are caught on the in-stack
filter. (Note: If the test is conducted for PM10
only, then Container #1 would be for less
than or equal to PM2.5 micrometer filterable
particulate.)
(b) Container #2, Greater than PM10
micrometer filterable particulate.
Quantitatively recover the PM from the
cyclone I cup and brush cleaning and acetone
rinses of the cyclone cup, internal surface of
the nozzle, and cyclone I internal surfaces,
including the outside surface of the
downcomer line. Seal the container and mark
the liquid level on the outside of the
container you labeled with test identification
and Container #2. You must keep any dust
found on the outside of cyclone I and cyclone
nozzle external surfaces out of the sample.
This container holds PM greater than 10
micrometers.
(c) Container #3, Filterable particulate less
than or equal to 10 micrometer and greater
than 2.5 micrometers. Place the solids from
cyclone cup IV and the acetone (and brush
cleaning) rinses of the cyclone I turnaround
cup (above inner downcomer line), inside of
the downcomer line, and interior surfaces of
cyclone IV into Container #3. Seal the
container and mark the liquid level on the
outside of the container you labeled with test
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identification and Container #3. This
container holds PM less than or equal to 10
micrometers but greater than 2.5
micrometers.
(d) Container #4, Less than or equal to
PM2.5 micrometers acetone rinses of the exit
tube of cyclone IV and front half of the filter
holder. Place the acetone rinses (and brush
cleaning) of the exit tube of cyclone IV and
the front half of the filter holder in container
#4. Seal the container and mark the liquid
level on the outside of the container you
labeled with test identification and Container
#4. This container holds PM that is less than
or equal to 2.5 micrometers.
(e) Container #5, Cold impinger water. If
the water from the cold impinger used for
moisture collection has been weighed in the
field, it can be discarded. Otherwise,
quantitatively transfer liquid from the cold
impinger that follows the ambient filter into
a clean sample bottle (glass or plastic). Mark
the liquid level on the bottle you labeled
with test identification and Container #5.
This container holds the remainder of the
liquid water from the emission gases. If you
collected condensable PM using Method 202
of appendix M to this part in conjunction
with using this method, you must follow the
procedures in Method 202 of appendix M to
this part to recover impingers and silica used
to collect moisture.
(f) Container #6, Silica gel absorbent.
Transfer the silica gel to its original container
labeled with test identification and Container
#6 and seal. A funnel may make it easier to
pour the silica gel without spilling. A rubber
policeman may be used as an aid in removing
the silica gel from the impinger. It is not
necessary to remove the small amount of
silica gel dust particles that may adhere to
the impinger wall and are difficult to remove.
Since the gain in weight is to be used for
moisture calculations, do not use any water
or other liquids to transfer the silica gel. If
the silica gel has been weighed in the field
to measure water content, it can be
discarded. Otherwise, the contents of
Container #6 are weighed during sample
analysis.
(g) Container #7, Acetone field reagent
blank. Take approximately 200 ml of the
acetone directly from the wash bottle you
used and place it in Container #7 labeled
‘‘Acetone Field Reagent Blank.’’
8.7.6 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.
9.0 Quality Control
9.1 Daily Quality Checks. You must
perform daily quality checks of field log
books 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 book 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,
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prepare a data summary and compile all the
calculations and raw data sheets.
9.3 Conditions. You must document data
and information on the process unit tested,
the particulate control system used to control
emissions, any non-particulate control
system that may affect particulate emissions,
the sampling train conditions, and weather
conditions. Discontinue the test if the
operating conditions may cause nonrepresentative particulate emissions.
9.4 Field Analytical Balance Calibration
Check. Perform calibration check procedures
on field analytical balances each day that
they are used. You must use National
Institute of Standards and Technology
(NIST)-traceable weights at a mass
approximately equal to the weight of the
sample plus container you will weigh.
10.0 Calibration and Standardization
Maintain a log of all filterable particulate
sampling and analysis calibrations. Include
copies of the relevant portions of the
calibration and field logs in the final test
report.
10.1 Gas Flow Velocities. You must use
an S-type pitot tube that meets the required
EPA specifications (EPA Publication 600/4–
77–0217b) during these velocity
measurements. (Note: If, as specified in
Section 8.7.2.3, testing is performed in stacks
less than 26.5 inches in diameter, testers may
use a standard pitot tube according to the
requirements in Method 4A or 5 of appendix
A–3 to part 60.) You must also complete the
following:
(a) Visually inspect the S-type pitot tube
before sampling.
(b) Leak check both legs of the pitot tube
before and after sampling.
(c) Maintain proper orientation of the Stype pitot tube while making measurements.
10.1.1 S-type Pitot Tube Orientation. The
S-type pitot tube is properly oriented when
the yaw and the pitch axis are 90 degrees to
the air flow.
10.1.2 Average Velocity Pressure Record.
Instead of recording either high or low
values, record the average velocity pressure
at each point during flow measurements.
10.1.3 Pitot Tube Coefficient. Determine
the pitot tube coefficient based on physical
measurement techniques described in
Method 2 of appendix A–1 to part 60. (Note:
You must calibrate the pitot tube on the
sampling head because of potential
interferences from the cyclone body. Refer to
Section 8.7.2 for additional information.)
10.2 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). 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.
10.3 Nozzles. You may use stainless steel
(316 or equivalent), high-temperature steel
alloy, or fluoropolymer-coated nozzles for
isokinetic sampling. Make sure that all
nozzles are thoroughly cleaned, visually
inspected, and calibrated according to the
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procedure outlined in Section 10.1 of Method
5 of appendix A–3 to part 60.
10.4 Dry Gas Meter Calibration. Calibrate
your dry gas meter following the calibration
procedures in Section 16.1 of Method 5 of
appendix A–3 to part 60. Also, make sure
you fully calibrate the dry gas meter to
determine the volume correction factor prior
to field use. Post-test calibration checks must
be performed as soon as possible after the
equipment has been returned to the shop.
Your pre-test and post-test calibrations must
agree within ± 5 percent.
10.5 Glassware. Use class A volumetric
glassware for titrations, or calibrate your
equipment against NIST-traceable glassware.
11.0 Analytical Procedures
11.1 Analytical Data Sheet. Record all
data on the analytical data sheet. Obtain the
data sheet from Figure 5–6 of Method 5 of
appendix A–3 to part 60. Alternatively, data
may be recorded electronically using
software applications such as the Electronic
Reporting Tool located at https://
www.epa.gov/ttn/chief/ert/ert_tool.html.
11.2 Dry Weight of PM. Determine the
dry weight of particulate following
procedures outlined in this section.
11.2.1 Container #1, Less than or Equal to
PM2.5 Micrometer Filterable Particulate.
Transfer the filter and any loose particulate
from the sample container to a tared
weighing dish or pan that is inert to solvent
or mineral acids. Desiccate for 24 hours in a
dessicator containing anhydrous calcium
sulfate. Weigh to a constant weight and
report the results to the nearest 0.1 mg. (See
Section 3.0 for a definition of Constant
weight.) If constant weight requirements
cannot be met, the filter must be treated as
described in Section 11.2.1 of Method 202 of
appendix M to this part. Extracts resulting
from the use of this procedure must be
filtered to remove filter fragments before the
filter is processed and weighed.
11.2.2 Container #2, Greater than PM10
Micrometer Filterable Particulate Acetone
Rinse. Separately treat this container like
Container #4.
11.2.3 Container #3, Filterable Particulate
Less than or Equal to 10 Micrometer and
Greater than 2.5 Micrometers Acetone Rinse.
Separately treat this container like Container
#4.
11.2.4 Container #4, Less than or Equal to
PM2.5 Micrometers Acetone Rinse of the Exit
Tube of Cyclone IV and Front Half of the
Filter Holder. Note the level of liquid in the
container and confirm on the analysis sheet
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. Quantitatively
transfer the contents to a tared 250 ml beaker
or tared fluoropolymer beaker liner, and
evaporate to dryness at room temperature
and pressure in a laboratory hood. Desiccate
for 24 hours and weigh to a constant weight.
Report the results to the nearest 0.1 mg.
11.2.5 Container #5, Cold Impinger
Water. If the amount of water has not been
determined in the field, note the level of
liquid in the container and confirm on the
analysis sheet whether leakage occurred
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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.
Measure the liquid in this container either
volumetrically to ± 1 ml or gravimetrically to
± 0.5 g.
11.2.6 Container #6, Silica Gel Absorbent.
Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g using a balance.
This step may be conducted in the field.
11.2.7 Container #7, Acetone Field
Reagent Blank. Use 150 ml of acetone from
the blank container used for this analysis.
Transfer 150 ml of the acetone to a clean 250ml beaker or tared fluoropolymer beaker
liner. Evaporate the acetone to dryness at
room temperature and pressure in a
laboratory hood. Following evaporation,
desiccate the residue for 24 hours in a
desiccator containing anhydrous calcium
sulfate. Weigh and report the results to the
nearest 0.1 mg.
12.0
Calculations and Data Analysis
12.1 Nomenclature. Report results in
International System of Units (SI units)
unless the regulatory authority that
established the requirement to use this test
method specifies reporting in English units.
The following nomenclature is used.
A = Area of stack or duct at sampling
location, square inches.
An = Area of nozzle, square feet.
bf = Average blockage factor calculated in
Equation 26, dimensionless.
Bws = Moisture content of gas stream, fraction
(e.g., 10 percent H2O is Bws = 0.10).
C = Cunningham correction factor for particle
diameter, Dp, and calculated using the
actual stack gas temperature,
dimensionless.
%CO2 = Carbon Dioxide content of gas
stream, percent by volume.
Ca = Acetone blank concentration, mg/mg.
CfPM10 = Conc. of filterable PM10, gr/DSCF.
CfPM2.5 = Conc. of filterable PM2.5, gr/DSCF.
Cp = Pitot coefficient for the combined
cyclone pitot, dimensionless.
Cp′ = Coefficient for the pitot used in the
preliminary traverse, dimensionless.
Cr = Re-estimated Cunningham correction
factor for particle diameter equivalent to
the actual cut size diameter and
calculated using the actual stack gas
temperature, dimensionless.
Ctf = Conc. of total filterable PM, gr/DSCF.
C1 = -150.3162 (micropoise)
C2 = 18.0614 (micropoise/K0.5) = 13.4622
(micropoise/R0.5)
C3 = 1.19183 × 106 (micropoise/K2) = 3.86153
× 106 (micropoise/R2)
C4 = 0.591123 (micropoise)
C5 = 91.9723 (micropoise)
C6 = 4.91705 × 10¥5 (micropoise/K2) =
1.51761 × 10¥5 (micropoise/R2)
D = Inner diameter of sampling nozzle
mounted on Cyclone I, inches.
Dp = Physical particle size, micrometers.
D50 = Particle cut diameter, micrometers.
D50–1 = Re-calculated particle cut diameters
based on re-estimated Cr, micrometers.
D50LL = Cut diameter for cyclone I
corresponding to the 2.25 micrometer cut
diameter for cyclone IV, micrometers.
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80141
D50N = D50 value for cyclone IV calculated
during the Nth iterative step,
micrometers.
D50(N∂1) = D50 value for cyclone IV calculated
during the N+1 iterative step,
micrometers.
D50T = Cyclone I cut diameter corresponding
to the middle of the overlap zone shown
in Figure 10 of Section 17, micrometers.
I = Percent isokinetic sampling,
dimensionless.
Kp = 85.49, ((ft/sec)/(pounds/mole -°R)).
ma = Mass of residue of acetone after
evaporation, mg.
Md = Molecular weight of dry gas, pounds/
pound mole.
mg = Milligram.
mg/L = Milligram per liter.
Mw = Molecular weight of wet gas, pounds/
pound mole.
M1 = Milligrams of PM collected on the filter,
less than or equal to 2.5 micrometers.
M2 = Milligrams of PM recovered from
Container #2 (acetone blank corrected),
greater than 10 micrometers.
M3 = Milligrams of PM recovered from
Container #3 (acetone blank corrected),
less than or equal to 10 and greater than
2.5 micrometers.
M4 = Milligrams of PM recovered from
Container #4 (acetone blank corrected),
less than or equal to 2.5 micrometers.
Ntp = Number of iterative steps or total
traverse points.
Nre = Reynolds number, dimensionless.
%O2,wet = Oxygen content of gas stream, %
by volume of wet gas.
(Note: The oxygen percentage used in
Equation 3 is on a wet gas basis. That
means that since oxygen is typically
measured on a dry gas basis, the
measured percent O2 must be multiplied
by the quantity (1–Bws) to convert to the
actual volume fraction. Therefore,
%O2,wet = (1–Bws) * %O2, dry)
Pbar = Barometric pressure, inches Hg.
Ps = Absolute stack gas pressure, inches Hg.
Qs = Sampling rate for cyclone I to achieve
specified D50.
QsST = Dry gas sampling rate through the
sampling assembly, DSCFM.
QI = Sampling rate for cyclone I to achieve
specified D50.
Rmax = Nozzle/stack velocity ratio parameter,
dimensionless.
Rmin = Nozzle/stack velocity ratio parameter,
dimensionless.
Tm = Meter box and orifice gas temperature,
°R.
tn = Sampling time at point n, min.
tr = Total projected run time, min.
Ts = Absolute stack gas temperature, °R.
t1 = Sampling time at point 1, min.
vmax = Maximum gas velocity calculated from
Equations 18 or 19, ft/sec.
vmin = Minimum gas velocity calculated from
Equations 16 or 17, ft/sec.
vn = Sample gas velocity in the nozzle, ft/sec.
vs = Velocity of stack gas, ft/sec.
Va = Volume of acetone blank, ml.
Vaw = Volume of acetone used in sample
recovery wash, ml.
Vc = Quantity of water captured in impingers
and silica gel, ml.
Vm = Dry gas meter volume sampled, ACF.
Vms = Dry gas meter volume sampled,
corrected to standard conditions, DSCF.
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Vws = Volume of water vapor, SCF.
Vb = Volume of aliquot taken for IC analysis,
ml.
Vic = Volume of impinger contents sample,
ml.
Wa = Weight of blank residue in acetone used
to recover samples, mg.
W2,3,4 = Weight of PM recovered from
Containers #2, #3, and #4, mg.
Z = Ratio between estimated cyclone IV D50
values, dimensionless.
DH = Meter box orifice pressure drop, inches
W.C.
DH@ = Pressure drop across orifice at flow
rate of 0.75 SCFM at standard
conditions, inches W.C.
(Note: Specific to each orifice and meter box.)
[(Dp)0.5]avg = Average of square roots of the
velocity pressures measured during the
preliminary traverse, inches W.C.
Dpm = Observed velocity pressure using Stype pitot tube in preliminary traverse,
inches W.C.
Dpavg = Average velocity pressure, inches
W.C.
Dpmax = Maximum velocity pressure, inches
W.C.
Dpmin = Minimum velocity pressure, inches
W.C.
Dpn = Velocity pressure measured at point n
during the test run, inches W.C.
Dps = Velocity pressure calculated in
Equation 25, inches W.C.
Dps1 = Velocity pressure adjusted for
combined cyclone pitot tube, inches
W.C.
Dps2 = Velocity pressure corrected for
blockage, inches W.C.
Dp1 = Velocity pressure measured at point 1,
inches W.C.
g = Dry gas meter gamma value,
dimensionless.
μ = Gas viscosity, micropoise.
q = Total run time, min.
ra = Density of acetone, mg/ml (see label on
bottle).
12.0 = Constant calculated as 60 percent of
20.5 square inch cross-sectional area of
combined cyclone head, square inches.
12.2 Calculations. Perform all of the
calculations found in Table 6 of Section 17.
Table 6 of Section 17 also provides
instructions and references for the
calculations.
12.3 Analyses. Analyze D50 of cyclone IV
and the concentrations of the PM in the
various size ranges.
12.3.1 D50 of Cyclone IV. To determine
the actual D50 for cyclone IV, recalculate the
Cunningham correction factor and the
Reynolds number for the best estimate of
cyclone IV D50. The following sections
describe additional information on how to
recalculate the Cunningham correction factor
and determine which Reynolds number to
use.
12.3.1.1 Cunningham correction factor.
Recalculate the initial estimate of the
Cunningham correction factor using the
actual test data. Insert the actual test run data
and D50 of 2.5 micrometers into Equation 4.
This will give you a new Cunningham
correction factor based on actual data.
12.3.1.2 Initial D50 for cyclone IV.
Determine the initial estimate for cyclone IV
D50 using the test condition Reynolds number
calculated with Equation 10 as indicated in
Table 3 of Section 17. Refer to the following
instructions.
(a) If the Reynolds number is less than
3,162, calculate the D50 for cyclone IV with
Equation 34, using actual test data.
(b) If the Reynolds number is greater than
or equal to 3,162, calculate the D50 for
cyclone IV with Equation 35 using actual test
data.
(c) Insert the ‘‘new’’ D50 value calculated by
either Equation 34 or 35 into Equation 36 to
re-establish the Cunningham Correction
Factor (Cr). (Note: Use the test condition
calculated Reynolds number to determine the
most appropriate equation (Equation 34 or
35).)
12.3.1.3 Re-establish cyclone IV D50. Use
the re-established Cunningham correction
factor (calculated in the previous step) and
the calculated Reynolds number to determine
D50–1.
(a) Use Equation 37 to calculate the reestablished cyclone IV D50–1 if the Reynolds
number is less than 3,162.
(b) Use Equation 38 to calculate the reestablished cyclone IV D50–1 if the Reynolds
number is greater than or equal to 3,162.
12.3.1.4 Establish ‘‘Z’’ values. The ‘‘Z’’
value is the result of an analysis that you
must perform to determine if the Cr is
acceptable. Compare the calculated cyclone
IV D50 (either Equation 34 or 35) to the reestablished cyclone IV D50–1 (either Equation
36 or 37) values based upon the test
condition calculated Reynolds number
(Equation 39). Follow these procedures.
(a) Use Equation 39 to calculate the ‘‘Z’’
values. If the ‘‘Z’’ value is between 0.99 and
1.01, the D50–1 value is the best estimate of
the cyclone IV D50 cut diameter for your test
run.
(b) If the ‘‘Z’’ value is greater than 1.01 or
less than 0.99, re-establish a Cr based on the
D50–1 value determined in either Equations 36
or 37, depending upon the test condition
Reynolds number.
(c) Use the second revised Cr to re-calculate
the cyclone IV D50.
(d) Repeat this iterative process as many
times as necessary using the prescribed
equations until you achieve the criteria
documented in Equation 40.
12.3.2 Particulate Concentration. Use the
particulate catch weights in the combined
cyclone sampling train to calculate the
concentration of PM in the various size
ranges. You must correct the concentrations
for the acetone blank.
12.3.2.1 Acetone blank concentration.
Use Equation 42 to calculate the acetone
blank concentration (Ca).
12.3.2.2 Acetone blank residue weight.
Use Equation 44 to calculate the acetone
blank weight (Wa (2,3,4)). Subtract the weight
of the acetone blank from the particulate
weight catch in each size fraction.
12.3.2.3 Particulate weight catch per size
fraction. Correct each of the PM weights per
size fraction by subtracting the acetone blank
weight (i.e., M2,3,4–Wa). (Note: Do not subtract
a blank value of greater than 0.1 mg per 100
ml of the acetone used from the sample
recovery.) Use the following procedures.
(a) Use Equation 45 to calculate the PM
recovered from Containers #1, #2, #3, and #4.
This is the total collectable PM (Ctf).
(b) Use Equation 46 to determine the
quantitative recovery of PM10 (CfPM10) from
Containers #1, #3, and #4.
(c) Use Equation 47 to determine the
quantitative recovery of PM2.5 (CfPM2.5)
recovered from Containers #1 and #4.
12.4 Reporting. You must prepare a test
report following the guidance in EPA
Guidance Document 043, Preparation and
Review of Test Reports (December 1998).
12.5 Equations. Use the following
equations to complete the calculations
required in this test method.
Molecular Weight of Dry Gas. Calculate the
molecular weight of the dry gas using
Equation 1.
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Gas Stream Viscosity. Calculate the gas
stream viscosity using Equation 3. This
equation uses constants for gas temperatures
in °R.
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Molecular Weight of Wet Gas. Calculate the
molecular weight of the stack gas on a wet
basis using Equation 2.
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations
80143
Cunningham Correction Factor. The
Cunningham correction factor is calculated
for a 2.25 micrometer diameter particle.
Lower Limit Cut Diameter for Cyclone I for
Nre Less than 3,162. The Cunningham
correction factor is calculated for a 2.25
micrometer diameter particle.
Cut Diameter for Cyclone I for the Middle
of the Overlap Zone.
ER21DE10.009
Sampling Rate Using Both PM10 and PM2.5
Cyclones.
ER21DE10.008
For Nre Less than 3,162:
ER21DE10.007
Sampling Rate Using Only PM2.5 Cyclone.
ER21DE10.005
ER21DE10.006
For Nre greater than or equal to 3,162:
ER21DE10.004
ER21DE10.003
Meter Box Orifice Pressure Drop.
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Reynolds Number.
80144
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations
Lower Limit Cut Diameter for Cyclone I for
Nre Greater than or Equal to 3,162. The
Cunningham correction factor is calculated
for a 2.25 micrometer diameter particle.
Velocity of Stack Gas. Correct the mean
preliminary velocity pressure for Cp and
blockage using Equations 25, 26, and 27.
Calculated Nozzle Diameter for Acceptable
Sampling Rate.
ER21DE10.015
ER21DE10.016
Velocity of Gas in Nozzle.
ER21DE10.013
ER21DE10.014
Minimum Nozzle/Stack Velocity Ratio
Parameter.
ER21DE10.012
ER21DE10.011
Minimum Gas Velocity for Rmin Less than
0.5.
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Maximum Nozzle/Stack Velocity Ratio
Parameter.
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80145
Minimum Gas Velocity for Rmin Greater
than or Equal to 0.5.
Maximum Gas Velocity for Rmax Less than
to 1.5.
Maximum Gas Velocity for Rmax Greater
than or Equal to 1.5.
ER21DE10.025
Minimum Velocity Pressure.
ER21DE10.023
ER21DE10.024
Maximum Velocity Pressure.
ER21DE10.021
ER21DE10.022
Sampling Dwell Time at Each Point. Ntp is
the total number of traverse points. You must
use the preliminary velocity traverse data.
ER21DE10.019
ER21DE10.018
Average Probe Blockage Factor.
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Adjusted Velocity Pressure.
80146
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations
Velocity Pressure.
Dry Gas Volume Sampled at Standard
Conditions.
Sample Flow Rate at Standard Conditions.
Volume of Water Vapor.
ER21DE10.032
ER21DE10.033
Moisture Content of Gas Stream.
ER21DE10.031
Sampling Rate.
Particle Cut Diameter for Nre Less than
3,162 for Cyclone IV. C must be recalculated
using the actual test data and a D50 for 2.5
micrometer diameter particle size.
ER21DE10.030
Actual Particle Cut Diameter for Cyclone I.
This is based on actual temperatures and
pressures measured during the test run.
ER21DE10.028
ER21DE10.027
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ER21DE10.029
(Note: The viscosity and Reynolds Number
must be recalculated using the actual stack
temperature, moisture, and oxygen content.)
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations
Particle Cut Diameter for Nre Greater than
or Equal to 3,162 for Cyclone IV. C must be
recalculated using the actual test run data
and a D50 for 2.5 micrometer diameter
particle size.
Re-estimated Cunningham Correction
Factor. You must use the actual test run
Reynolds Number (Nre) value and select the
80147
appropriate D50 from Equation 33 or 34 (or
Equation 37 or 38 if reiterating).
Re-calculated Particle Cut Diameter for Nre
Less than 3,162.
ER21DE10.041
Re-calculated Particle Cut Diameter for N
Greater than or Equal to 3,162.
ER21DE10.039
ER21DE10.040
Ratio (Z) Between D50 and D50–1 Values.
ER21DE10.037
ER21DE10.038
Acceptance Criteria for Z Values. The
number of iterative steps is represented by N.
ER21DE10.036
ER21DE10.035
Acetone Blank Concentration.
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Percent Isokinetic Sampling.
80148
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Acetone Blank Correction Weight.
Acetone Blank Weight.
Concentration of Total Filterable PM.
Concentration of Filterable PM10.
16.0 References
(1) Dawes, S.S., and W.E. Farthing. 1990.
‘‘Application Guide for Measurement of PM2.5
at Stationary Sources,’’ U.S. Environmental
Protection Agency, Atmospheric Research
and Exposure Assessment Laboratory,
Research Triangle Park, NC, 27511, EPA–
600/3–90/057 (NTIS No.: PB 90–247198).
(2) Farthing, et al. 1988a. ‘‘PM10 Source
Measurement Methodology: Field Studies,’’
EPA 600/3–88/055, NTIS PB89–194278/AS,
U.S. Environmental Protection Agency,
Research Triangle Park, NC 27711.
17.0 Tables, Diagrams, Flowcharts, and
Validation Data
You must use the following tables,
diagrams, flowcharts, and data to complete
this test method successfully.
TABLE 1—TYPICAL PM CONCENTRATIONS
Particle size range
Concentration and % by weight
Total collectable particulate ..............................................................................................................................
Less than or equal to 10 and greater than 2.5 micrometers ............................................................................
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0.015 gr/DSCF.
40% of total collectable PM.
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14.0 Alternative Procedures
Alternative methods for estimating the
moisture content (ALT–008) and
thermocouple calibration (ALT–011) can be
found at https://www.epa.gov/ttn/emc/
approalt.html.
(3) Farthing, W.E., and S.S. Dawes. 1988b.
‘‘Application Guide for Source PM10
Measurement with Constant Sampling Rate,’’
EPA/600/3–88–057, U.S. Environmental
Protection Agency, Research Triangle Park,
NC 27711.
(4) Richards, J.R. 1996. ‘‘Test protocol: PCA
PM10/PM2.5 Emission Factor Chemical
Characterization Testing,’’ PCA R&D Serial
No. 2081, Portland Cement Association.
(5) U.S. Environmental Protection Agency,
Federal Reference Methods 1 through 5 and
Method 17, 40 CFR part 60, Appendix A–1
through A–3 and A–6.
(6) U.S. Environmental Protection Agency.
2010. ‘‘Field Evaluation 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.
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for the field evaluation was 6.7 percent
relative standard deviation. The field
evaluation also showed that the blank
expected from Method 201A was less than
0.9 mg (EPA, 2010).
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13.0 Method Performance
13.1 Field evaluation of PM10 and total
PM showed that the precision of constant
sampling rate method was the same
magnitude as Method 17 of appendix A–6 to
part 60 (approximately five percent).
Precision in PM10 and total PM between
multiple trains showed standard deviations
of four to five percent and total mass
compared to 4.7 percent observed for Method
17 in simultaneous test runs at a Portland
cement clinker cooler exhaust. The accuracy
of the constant sampling rate PM10 method
for total mass, referenced to Method 17, was
¥2 ± 4.4 percent (Farthing, 1988a).
13.2 Laboratory evaluation and guidance
for PM10 cyclones were designed to limit
error due to spatial variations to 10 percent.
The maximum allowable error due to an
isokinetic sampling was limited to ± 20
percent for 10 micrometer particles in
laboratory tests (Farthing, 1988b).
13.3 A field evaluation of the revised
Method 201A by EPA showed that the
detection limit was 2.54 mg for total filterable
PM, 1.44 mg for filterable PM10, and 1.35 mg
for PM2.5. The precision resulting from 10
quadruplicate tests (40 test runs) conducted
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Concentration of Filterable PM2.5.
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TABLE 1—TYPICAL PM CONCENTRATIONS—Continued
Particle size range
Concentration and % by weight
≤ 2.5 micrometers .............................................................................................................................................
20% of total collectable PM.
TABLE 2—REQUIRED CYCLONE CUT DIAMETERS (D50)
Min. cut
diameter
(micrometer)
Cyclone
PM10 Cyclone (Cyclone I from five stage cyclone) .............................................................................................
PM2.5 Cyclone (Cyclone IV from five stage cyclone) ..........................................................................................
Max. cut
diameter
(micrometer)
9
2.25
11
2.75
TABLE 3—TEST CALCULATIONS
If you are using . . .
To calculate . . .
Then use . . .
Preliminary data .........................................................................
Dry gas molecular weight (Md) and preliminary moisture content of the gas stream.
Stack gas temperature, and oxygen and moisture content of
the gas stream.
Gas viscosity, μ .........................................................................
Reynolds Number c (Nre) ...........................................................
Nre less than 3,162 ....................................................................
D50LL from Equation 5 ...............................................................
Dry gas molecular weight, Md ..................................................
wet gas molecular weight, MW .................................................
Equation 1.
Equation 2.a
gas viscosity, μ .........................................................................
Equation 3.
Cunningham correction factor b, C ...........................................
Preliminary lower limit cut diameter for cyclone I, D50LL .........
Equation 4.
Equation 5.
Cut diameter for cyclone I for middle of the overlap zone,
D50T.
Final sampling rate for cyclone I, QI(Qs) .................................
Final sampling rate for cyclone IV, QIV ....................................
Final sampling rate for cyclone IV, QIV ....................................
Verify the assumed Reynolds number, Nre .............................
Equation 6.
D50T from Equation 6 .................................................................
D50 for PM2.5 cyclone and Nre less than 3,162 .........................
D50 for PM2.5 cyclone and Nre greater than or equal to 3,162
QI(Qs) from Equation 7 ..............................................................
Equation
Equation
Equation
Equation
7.
8.
9.
10.
a Use Method 4 to determine the moisture content of the stack gas. Use a wet bulb-dry bulb measurement device or hand-held hygrometer to
estimate moisture content of sources with gas temperature less than 160 °F.
b For the lower cut diameter of cyclone IV, 2.25 micrometer.
c Verify the assumed Reynolds number, using the procedure in Section 8.5.1, before proceeding to Equation 11.
TABLE 4—DH VALUES BASED ON PRELIMINARY TRAVERSE DATA
Stack Temperature (°R)
Ts—50°
Ts
Ts + 50°
DH, (inches W.C.)
a
a
a
a These
values are to be filled in by the stack tester.
TABLE 5—VERIFICATION OF THE ASSUMED REYNOLDS NUMBER
If the Nre is . . .
Then . . .
And . . .
Less than 3,162 .......................................................................................
Greater than or equal to 3,162 ...............................................................
Calculate DH for the meter box .....
Recalculate D50LL using Equation
12.
Assume original D50LL is correct
Substitute the ‘‘new’’ D50LL into
Equation 6 to recalculate D50T.
TABLE 6—CALCULATIONS FOR RECOVERY OF PM10 AND PM2.5
Instructions and References
Average dry gas meter temperature ........................................................
Average orifice pressure drop ..................................................................
Dry gas volume (Vms) ...............................................................................
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Calculations
See field test data sheet.
See field test data sheet.
Use Equation 28 to correct the sample volume measured by the dry
gas meter to standard conditions (20 °C, 760 mm Hg or 68 °F, 29.92
inches Hg).
Must be calculated using Equation 29.
Use Equation 30 to determine the water condensed in the impingers
and silica gel combination. Determine the total moisture catch by
measuring the change in volume or weight in the impingers and
weighing the silica gel.
Calculate this using Equation 31.
Calculate this using Equation 32.
Use Equation 10 to calculate the actual Reynolds number during test
conditions.
Dry gas sampling rate (QsST) ...................................................................
Volume of water condensed (Vws) ...........................................................
Moisture content of gas stream (Bws) ......................................................
Sampling rate (Qs) ....................................................................................
Test condition Reynolds numbera ............................................................
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TABLE 6—CALCULATIONS FOR RECOVERY OF PM10 AND PM2.5—Continued
Calculations
Instructions and References
Actual D50 of cyclone I .............................................................................
Calculate this using Equation 33. This calculation is based on the average temperatures and pressures measured during the test run.
Calculate this using Equation 13.
Calculate this using Equation 41.
Stack gas velocity (vs) ..............................................................................
Percent isokinetic rate (%I) ......................................................................
a Calculate the Reynolds number at the cyclone IV inlet during the test based on: (1) The sampling rate for the combined cyclone head, (2) the
actual gas viscosity for the test, and (3) the dry and wet gas stream molecular weights.
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BILLING CODE 6560–50–C
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Method 202—Dry Impinger Method for
Determining Condensable Particulate
Emissions From Stationary Sources
1.0 Scope and Applicability
1.1 Scope. The U.S. Environmental
Protection Agency (U.S. EPA or ‘‘we’’)
developed this method to describe the
procedures that the stack tester (‘‘you’’) must
follow to measure condensable particulate
matter (CPM) emissions from stationary
sources. This method includes procedures for
measuring both organic and inorganic CPM.
1.2 Applicability. This method addresses
the equipment, preparation, and analysis
necessary to measure only CPM. You can use
this method only for stationary source
emission measurements. You can use this
method to measure CPM from stationary
source emissions after filterable particulate
matter (PM) has been removed. CPM is
measured in the emissions after removal from
the stack and after passing through a filter.
(a) If the gas filtration temperature exceeds
30 °C (85 °F) and you must measure both the
filterable and condensable (material that
condenses after passing through a filter)
components of total primary (direct) PM
emissions to the atmosphere, then you must
combine the procedures in this method with
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the procedures in Method 201A of appendix
M to this part for measuring filterable PM.
However, if the gas filtration temperature
never exceeds 30 °C (85 °F), then use of this
method is not required to measure total
primary PM.
(b) If Method 17 of appendix A–6 to part
60 is used in conjunction with this method
and constant weight requirements for the instack filter cannot be met, the Method 17
filter and sampling nozzle rinse must be
treated as described in Sections 8.5.4.4 and
11.2.1 of this method. (See Section 3.0 for a
definition of constant weight.) Extracts
resulting from the use of this procedure must
be filtered to remove filter fragments before
the filter is processed and weighed.
1.3 Responsibility. You are responsible
for obtaining the equipment and supplies you
will need to use 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:
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(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) You will need additional test methods
to measure filterable PM. You may use
Method 5 (including Method 5A, 5D and 5I
but not 5B, 5E, 5F, 5G, or 5H) of appendix
A–3 to part 60, or Method 17 of appendix
A–6 to part 60, or Method 201A of appendix
M to this part to collect filterable PM from
stationary sources with temperatures above
30 °C (85 °F) in conjunction with this
method. However, if the gas filtration
temperature never exceeds 30 °C (85 °F), then
use of this method is not required to measure
total primary PM.
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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 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. 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 fractions of the
impingers and an out-of-stack CPM filter are
then taken to dryness and weighed. The total
of 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 immediately 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. CPM 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 immediately after
sample collection to remove dissolved sulfur
dioxide (SO2) gases from the impinger. The
CPM filter is extracted with water and
hexane. The impinger solution is then
extracted with hexane. The organic and
aqueous fractions are dried 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 condenser and water dropout
impinger to separate CPM from reactive
gases. No water is added to the 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
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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 one percent of total
weight less tare weight, whichever is greater,
between two consecutive weighings, with no
less than six hours of desiccation time
between weighings.
3.3 Field Train Proof Blank. A field train
proof blank is recovered on site from a clean,
fully-assembled sampling train prior to
conducting the first emissions test.
3.4 Filterable PM means particles that are
emitted directly by a source as a solid or
liquid at stack or release conditions and
captured on the filter of a stack test train.
3.5 Primary PM (also known as direct
PM) means particles that enter the
atmosphere as a direct emission from a stack
or an open source. Primary PM comprises
two components: filterable PM and
condensable PM. These two PM components
have no upper particle size limit.
3.6 Primary PM2.5 (also known as direct
PM2.5, total PM2.5, PM2.5, or combined
filterable PM2.5 and condensable PM) means
PM with an aerodynamic diameter less than
or equal to 2.5 micrometers. These solid
particles are emitted directly from an air
emissions source or activity, or are the
gaseous emissions or liquid droplets from an
air emissions source or activity that condense
to form PM at ambient temperatures. Direct
PM2.5 emissions include elemental carbon,
directly emitted organic carbon, directly
emitted sulfate, directly emitted nitrate, and
other inorganic particles (including but not
limited to crustal material, metals, and sea
salt).
3.7 Primary PM10 (also known as direct
PM10, total PM10, PM10, or the combination
of filterable PM10 and condensable PM)
means PM with an aerodynamic diameter
equal to or less than 10 micrometers.
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
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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
Method 23 type condenser as described in
Section 2.1.2 of Method 23 of appendix A–
8 to part 60, 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 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 filters. Commercial size filter
holders contain a fluoropolymer O-ring,
stainless steel, ceramic or fluoropolymer
filter support and a final fluoropolymer Oring. A filter that meets the requirements
specified in Section 7.1.1 may be placed
behind the CPM filter to reduce the pressure
drop across the CPM filter. This support filter
is not part of the PM sample and is not
recovered with the CPM filter. At the exit of
the CPM filter, install a fluoropolymer-coated
or stainless steel encased thermocouple that
is in contact with the gas stream.
6.1.4 Long Stem Impinger Insert. You will
need a long stem modified Greenburg Smith
impinger insert for the water dropout
impinger to perform the nitrogen purge of the
sampling train.
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 L/
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
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least 14 L/min purge gas for one hour
through the sampling train.
(d) Amber glass bottles (500 ml).
6.2.2 Analysis Equipment. The following
equipment is necessary for CPM sample
analysis:
(a) Separatory Funnel. Glass, 1 liter.
(b) Weighing Tins. 50 ml. Glass
evaporation vials, fluoropolymer beaker
liners, or aluminum weighing tins can be
used.
(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 or Colormetric pH Indicator.
The pH meter or colormetric pH indicator
(e.g., phenolphthalein) must be capable of
determining the acidity of liquid within 0.1
pH units.
(i) Sonication Device. The device must
have a minimum sonication frequency of 20
kHz and be approximately four to six inches
deep to accommodate the sample extractor
tube.
(j) Leak-Proof Sample Containers.
Containers used for sample and blank
recovery must not contribute more than 0.05
mg of residual mass to the CPM
measurements.
(k) Wash bottles. Any container material is
acceptable, but wash bottles used for sample
and blank recovery must not contribute more
than 0.1 mg of residual mass to the CPM
measurements.
7.0 Reagents and Standards
7.1 Sample Collection. To collect a
sample, you will need a CPM filter, crushed
ice, and silica gel. You must also have water
and nitrogen gas to purge the sampling train.
You will find additional information on each
of these items in the following summaries.
7.1.1 CPM Filter. You must use a
nonreactive, nondisintegrating 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 six 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 two
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, 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.
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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 ml) residue.
7.2.2 Hexane, American Chemical Society
grade. You must use hexane that has a blank
residual mass value less than 1.0 ppmw (0.1
mg/100 ml) residue.
7.2.3 Water. Use deionized, ultra-filtered
water that contains 1 ppmw (1 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-traceable or equivalent (0.1 N)
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 instack filtration systems (such as, cyclones,
impactors, and thimbles) and impinger and
moisture train systems.
8.2 Preparations. You must 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. Analyze
laboratory reagent blanks (water, acetone,
and hexane) before field tests to verify low
blank concentrations. 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.
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(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 Methods 5, 17, or 201A, whichever
is applicable to your test requirements. 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 must be cleaned prior to the
test with soap and water, and rinsed using
tap water, deionized water, acetone, and
finally, hexane. It is important to completely
remove all silicone grease from areas that
will be exposed to the hexane rinse during
sample recovery. After cleaning, you must
bake glassware at 300 °C for six hours prior
to beginning tests at each source category
sampled at a facility. As an alternative to
baking glassware, a field train proof blank, as
specified in Section 8.5.4.10, can be
performed on the sampling train glassware
that is used to collect CPM samples. Prior to
each sampling run, the train glassware used
to collect condensable PM must be rinsed
thoroughly with deionized, ultra-filtered
water that that contains 1 ppmw (1 mg/L)
residual mass or less.
8.4.1 Condenser and Water Dropout
Impinger. Add a Method 23 type condenser
and a condensate 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.
The Method 23 type stack gas condenser is
described in Section 2.1.2 of Method 23. The
condenser must be capable of cooling the
stack gas to less than or equal to 30 °C (85
°F).
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 water
dropout and backup impingers must be
clean, without any water or reagent added.
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. (Note: A thermocouple well is not
sufficient for this purpose because the
fluoropolymer- or steel-encased
thermocouple must be in contact with the
sample gas.)
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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
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 Silica Gel Trap. Place 200 to 300 g
of silica gel in each of several air-tight
containers. Weigh each container, including
silica gel, to the nearest 0.5 g, and record this
weight on the filterable particulate data
sheet. As an alternative, the silica gel need
not be preweighed, but may be weighed
directly in its impinger or sampling holder
just prior to train assembly.
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 leakcheck at a vacuum equal to or greater than
the vacuum anticipated during the test run.
Enter the leak-check results on the field test
data sheet for the filterable particulate
method. (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 leakcheck 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 CPM Filter Assembly. On the field
data sheet for the filterable particulate
method, 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. (Note: Maintain the
temperature of the CPM filter assembly as
close to 30 °C (85 °F) as feasible.)
8.5.2 Leak-Check Probe/Sample Train
Assembly (Post-Test). Conduct the leak rate
check according to the filterable particulate
sampling method used during sampling. If
required, conduct the leak-check at a vacuum
equal to or greater than the maximum
vacuum achieved during the test run. If the
leak rate of the sampling train exceeds 0.02
actual cubic feet per minute or four 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 Post-Test Nitrogen Purge. As soon
as possible after the post-test leak-check,
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detach the probe, any cyclones, and in-stack
or hot filters from the condenser and
impinger train. If no water was collected
before the CPM filter, then you may skip the
remaining purge steps and proceed with
sample recovery (see Section 8.5.4). You may
purge the CPM sampling train using the
sampling system meter box and vacuum
pump or by passing nitrogen through the
train under pressure. For either type of purge,
you must first attach the nitrogen supply line
to a purged inline filter.
8.5.3.1 If you choose to conduct a
pressurized nitrogen purge on the complete
CPM sampling train, you must quantitatively
transfer the water collected in the condenser
and the water dropout impinger to the
backup impinger. You must measure the
water combined in the backup impinger and
record the volume or weight as part of the
moisture collected during sampling as
specified in Section 8.5.3.4.
(a) You must conduct the purge on the
condenser, backup impinger, and CPM filter.
If the tip of the backup impinger insert does
not extend below the water level (including
the water transferred from the first impinger),
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).
(b) To perform the nitrogen purge using
positive pressure nitrogen flow, you must
start with no flow of gas through the clean
purge line and fittings. Connect the filter
outlet to the input of the impinger train and
disconnect the vacuum line from the exit of
the silica moisture collection impinger (see
Figure 3 of Section 18). You may purge only
the CPM train by disconnecting the moisture
train components if you measure moisture in
the field prior to the nitrogen purge. You
must 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 for at least one hour.
At the conclusion of the purge, turn off the
nitrogen delivery system.
8.5.3.2 If you choose to conduct a
nitrogen purge on the complete CPM
sampling train using the sampling system
meter box and vacuum pump, replace the
short stem impinger insert with a modified
Greenberg Smith impinger insert. The
impinger tip length must extend below the
water level in the impinger catch.
(a) You must conduct the purge on the
complete CPM sampling train starting at the
inlet of the condenser. If insufficient water
was collected, 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
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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).
(b) You must start the purge using the
sampling train vacuum pump with no flow
of gas through the clean purge line and
fittings. Connect the filter outlet to the input
of the impinger train (see Figure 2 of Section
18). To avoid over- or under-pressurizing the
impinger array, slowly commence the
nitrogen gas flow through the line while
simultaneously opening the meter box pump
valve(s). Adjust the pump bypass and/or
nitrogen delivery rates to obtain the
following conditions: 14 liters/min or DH@
and a positive overflow rate through the
rotameter of less than 2 liters/min. The
presence of a positive overflow rate
guarantees that the nitrogen delivery system
is operating at greater than ambient pressure
and prevents the possibility of passing
ambient air (rather than nitrogen) through the
impingers. Continue the purge under these
conditions for at least one hour, checking the
rotameter and DH@ value(s) at least every 15
minutes. At the conclusion of the purge,
simultaneously turn off the delivery and
pumping systems.
8.5.3.3 During either purge procedure,
continue operation of the condenser
recirculation pump, and heat or cool the
water surrounding the first two impingers to
maintain the gas temperature measured at the
exit of 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). If the
volume of liquid collected in the moisture
traps has not been determined prior to
conducting the nitrogen purge, 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). Continue
the purge under these conditions for at least
one hour, checking the rotameter and DH@
value(s) periodically. At the conclusion of
the purge, simultaneously turn off the
delivery and pumping systems.
8.5.3.4 Weigh the liquid, or measure the
volume of the liquid collected in the dropout,
impingers, and silica trap if this has not been
done prior to purging the sampling train.
Measure the liquid in the water dropout
impinger to within 1 ml using a clean
graduated cylinder or by weighing it to
within 0.5 g using a balance. Record the
volume or weight of liquid present to be used
to calculate the moisture content of the
effluent gas in the field log notebook.
8.5.3.5 If a balance is available in the
field, weigh the silica impinger to within 0.5
g. Note the color of the indicating silica gel
in the last impinger to determine whether it
has been completely spent, and make a
notation of its condition in the field log
notebook.
8.5.4 Sample Recovery.
8.5.4.1 Recovery of filterable PM.
Recovery of filterable PM involves the
quantitative transfer of particles according to
the filterable particulate sampling method
(i.e., Method 5 of appendix A–3 to part 60,
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Method 17 of appendix A–6 to part 60, or
Method 201A of appendix M to this part).
8.5.4.2 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, 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.
8.5.4.3 CPM Container #2, Organic rinses.
Follow the water rinses of the probe
extension, 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
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 jar.
8.5.4.4 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.’’
8.5.4.5 CPM Container #4, Cold impinger
water. You must weigh or measure the
volume of the contents of CPM Container #4
either in the field or during sample analysis
(see Section 11.2.4). If the water from the
cold impinger has been weighed in the field,
it can be discarded. Otherwise, quantitatively
transfer liquid from the cold impinger that
follows the CPM filter into a clean, leak-proof
container labeled with test identification and
‘‘CPM Container #4, Cold Water Impinger.’’
Mark the liquid level on the container. CPM
Container #4 holds the remainder of the
liquid water from the emission gases.
8.5.4.6 CPM Container #5, Silica gel
absorbent. You must weigh the contents of
CPM Container #5 in the field or during
sample analysis (see Section 11.2.5). If the
silica gel has been weighed in the field to
measure water content, then it can be
discarded or recovered for reuse. Otherwise,
transfer the silica gel to its original container
labeled with test identification and ‘‘CPM
Container #5, Silica Gel Absorbent’’ and seal.
You may use a funnel to make it easier to
pour the silica gel without spilling. You may
also use a rubber policeman as an aid in
removing the silica gel from the impinger. It
is not necessary to remove the small amount
of silica gel dust particles that may adhere to
the impinger wall and are difficult to remove.
Since the gain in weight is to be used for
moisture calculations, do not use any water
or other liquids to transfer the silica gel.
8.5.4.7 CPM Container #6, Acetone field
reagent blank. Take approximately 200 ml of
the acetone 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 #6,
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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 the lot(s) of solvent used
for the test.
8.5.4.8 CPM Container #7, Water field
reagent blank. Take approximately 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 #7, 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 the lot(s) of water used for the
test.
8.5.4.9 CPM Container #8, Hexane field
reagent blank. Take approximately 200 ml of
the hexane 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 #8,
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 the lot(s) of solvent used
for the test.
8.5.4.10 Field train proof blank. If you
did not bake the sampling train glassware as
specified in Section 8.4, you must conduct a
field train proof blank as specified in
Sections 8.5.4.11 and 8.5.4.12 to demonstrate
the cleanliness of sampling train glassware.
8.5.4.11 CPM Container #9, Field train
proof blank, inorganic rinses. Prior to
conducting the emission test, 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 #9, Field
Train Proof Blank, Inorganic Rinses.’’ Mark
the liquid level on the container.
8.5.4.12 CPM Container #10, 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
#10, Field Train Proof Blank, 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 #10).
Mark the liquid level on the container.
8.5.5 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 must 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.
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9.2 Calculation Verification. Verify the
calculations by independent, manual checks.
You must flag any suspect data and identify
the nature of the problem and potential effect
on data quality. After you complete the test,
prepare a data summary and compile all the
calculations and raw data sheets.
9.3 Conditions. You must document data
and information on the process unit tested,
the particulate control system used to control
emissions, any non-particulate control
system that may affect particulate emissions,
the sampling train conditions, and weather
conditions. Discontinue the test if the
operating conditions may cause nonrepresentative particulate emissions.
9.4 Field Analytical Balance Calibration
Check. Perform calibration check procedures
on field analytical balances each day that
they are used. You must use National
Institute of Standards and Technology
(NIST)-traceable weights at a mass
approximately equal to the weight of the
sample plus container you will weigh.
9.5 Glassware. Use class A volumetric
glassware for titrations, or calibrate your
equipment against NIST-traceable glassware.
9.6 Laboratory Analytical Balance
Calibration Check. Check the calibration of
your laboratory analytical balance each day
that you weigh CPM samples. You must use
NIST Class S weights at a mass
approximately equal to the weight of the
sample plus container you will weigh.
9.7 Laboratory Reagent Blanks. You
should run blanks of water, acetone, and
hexane used for field recovery and sample
analysis. Analyze at least one sample (150 ml
minimum) of each lot of reagents that you
plan to use for sample recovery and analysis
before you begin testing. These blanks are not
required by the test method, but running
blanks before field use is advisable to verify
low blank concentrations, thereby reducing
the potential for a high field blank on test
samples.
9.8 Field Reagent Blanks. You should run
at least one field reagent blank of water,
acetone, and hexane you use for field
recovery. These blanks are not required by
the test method, but running independent
field reagent blanks is advisable to verify that
low blank concentrations were maintained
during field solvent use and demonstrate that
reagents have not been contaminated during
field tests.
9.9 Field Train Proof Blank. If you are not
baking glassware as specified in Section 8.4,
you must recover a minimum of one field
train proof blank for the sampling train used
for testing each new source category at a
single facility. You must assemble the
sampling train as it will be used for testing.
You must recover the field train proof blank
samples as described in Section 8.5.4.11 and
8.5.4.12.
9.10 Field Train Recovery Blank. You
must recover a minimum of one field train
blank for each source category tested at the
facility. You must recover the field train
blank after the first or second run of the test.
You must assemble the sampling train as it
will be used for testing. Prior to the purge,
you must add 100 ml of water to the first
impinger and record this data on Figure 4.
You must purge the assembled train as
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described in Sections 8.5.3.2 and 8.5.3.3. You
must recover field train blank samples as
described in Section 8.5.4. From the field
sample weight, you will subtract the
condensable particulate mass you determine
with this blank train or 0.002 g (2.0 mg),
whichever is less.
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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/
ttn/emc). Calibrate each temperature sensor
at a minimum of three points over the
anticipated range of use against a NISTtraceable 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 l liter of water.
Standardize against standardized 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).
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. Alternatively, data
may be recorded electronically using
software applications such as the Electronic
Reporting Tool available at https://
www.epa.gov/ttn/chief/ert/ert_tool.html.
Record the condensable particulate data on
the CPM Work Table (see Figure 6 of Section
18).
(b) Measure the liquid in all containers
either volumetrically to ± 1 ml or
gravimetrically to ± 0.5 g. Confirm on the
filterable particulate analytical data sheet
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 7 of Section 18 for the
steps to process and combine fractions from
the CPM train.
11.2.1 Container #3, CPM Filter Sample.
If the sample was collected by Method 17 or
Method 201A with a stack temperature below
30 °C (85 °F) and the filter can be brought
to a constant weight, transfer the filter and
any loose PM from the sample container to
a tared glass weighing dish. (See Section 3.0
for a definition of constant weight.) Desiccate
the sample for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh
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to a constant weigh and report the results to
the nearest 0.1 mg. If the filter cannot be
brought to constant weight using this
procedure, you must follow the extraction
and weighing procedures in this section. (See
Section 3.0 for a definition of constant
weight.) Extract the filter recovered from the
low-temperature portion of the train, and
combine the extracts with the organic and
inorganic fractions resulting from the
aqueous impinger sample recovery in
Containers 1 and 2, respectively. Extract the
CPM filter as follows:
11.2.1.1 Extract the water soluble
(aqueous or inorganic) CPM from the CPM
filter by folding the filter in quarters and
placing it into a 50-ml extraction tube. Add
sufficient deionized, ultra-filtered water to
cover the filter (e.g., 10 ml of water). Place
the extractor tube into a sonication bath and
extract the water-soluble material for a
minimum of two 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 drain off the lower organic
phase. Repeat this procedure twice with 30
ml of hexane each time combining the
organic phase from each extraction. Each
time, leave a small amount of the organic/
hexane phase in the separatory funnel,
ensuring that no water is collected in the
organic phase. This extraction should yield
about 90 ml of organic extract. Combine the
organic extract from Container #1 with the
organic train rinse in Container 2.
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)). You must ensure that
water and volatile acids have completely
evaporated before neutralizing nonvolatile
acids in the sample. Following evaporation,
desiccate the residue for 24 hours in a
desiccator containing anhydrous calcium
sulfate. Weigh at intervals of at least six
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 can not be weighed to constant
weight, redissolve 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 Use titration to neutralize acid in
the sample and remove water of hydration.
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If used, calibrate the pH meter with the
neutral and acid buffer solutions. Then titrate
the sample with 0.1N NH4OH to a pH of 7.0,
as indicated by the pH meter or colorimetric
indicator. 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 pretared weighing tin 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 six 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 °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 pre-tared weighing tin 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 six
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 CPM Container #4, Cold Impinger
Water. If the amount of water has not been
determined in the field, note the level of
liquid in the container, and confirm on the
filterable particulate analytical data sheet
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. Measure the liquid
in Container #4 either volumetrically to ± 1
ml or gravimetrically to ± 0.5 g, and record
the volume or weight on the filterable
particulate analytical data sheet of the
filterable PM test method.
11.2.5 CPM Container #5, Silica Gel
Absorbent. Weigh the spent silica gel (or
silica gel plus impinger) to the nearest 0.5 g
using a balance. This step may be conducted
in the field. Record the weight on the
filterable particulate analytical data sheet of
the filterable PM test method.
11.2.6 Container #6, Acetone Field
Reagent Blank. Use 150 ml of acetone from
the blank container used for this analysis.
Transfer 150 ml of the acetone to a clean 250ml 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
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pressure in a laboratory hood to
approximately 10 ml. Quantitatively transfer
the beaker contents to a clean 50-ml pre-tared
weighing tin 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 six 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 4 of
Section 18.
the beaker contents to a clean 50-ml pre-tared
weighing tin, 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 six 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 4 of
Section 19.
11.2.7 Water Field Reagent Blank,
Container #7. Use 150 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 pre-tared
weighing tin 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 six 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 4 of
Section 18.
11.2.8 Hexane Field Reagent Blank,
Container #8. Use 150 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 °C (85 °F)) and
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.
12.2.2 Mass of the Field Train Recovery
Blank (mg). Per Section 9.10, the mass of the
field train recovery blank, mfb, shall not
exceed 2.0 mg.
Calculations and Data Analysis
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Mass of Inorganic CPM (mg).
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12.2.3
12.0
mfb = Mass of total CPM in field train
recovery blank, mg.
mg = Milligrams.
mg/L = Milligrams per liter.
mi = Mass of inorganic CPM, mg.
mib = Mass of inorganic CPM in field train
recovery 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 6 of
Section 18).
12.2.1 Mass of ammonia correction.
Correction for ammonia added during
titration of 100 ml aqueous CPM sample.
This calculation assumes no waters of
hydration.
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations
12.2.4
Total Mass of CPM (mg).
12.2.5
Concentration of CPM (mg/dscf).
12.3 Emissions Test Report. You must
prepare a test report following the guidance
in EPA Guidance Document 043 (Preparation
and Review of Test Reports. December 1998).
13.0 Method Performance
An EPA field evaluation of the revised
Method 202 showed the following precision
in the results: approximately 4 mg for total
CPM, approximately 0.5 mg for organic CPM,
and approximately 3.5 mg for inorganic CPM.
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
RCRA organic waste.
16.0 Alternative Procedures
Alternative Method 2, Thermocouple
Calibration (ALT–011) for the thermocouple
calibration can be found at https://
www.epa.gov/ttn/emc/approalt.html.
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.
18.0 Tables, Diagrams, Flowcharts, and
Validation Data
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ER21DE10.061
ER21DE10.062
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
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FIGURE 4—FIELD TRAIN RECOVERY
BLANK CONDENSABLE PARTICULATE
CALCULATIONS
Field Train Recovery Blank Condensable
Particulate Calculations
Plant
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FIGURE 4—FIELD TRAIN RECOVERY
BLANK CONDENSABLE PARTICULATE
CALCULATIONS—Continued
Date
Blank No.
CPM Filter No.
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FIGURE 4—FIELD TRAIN RECOVERY
BLANK CONDENSABLE PARTICULATE
CALCULATIONS—Continued
Water volume added to purge train (Vp)
ml
Field Reagent Blank Massa
Water (Section 11.2.7) ............................
mg
Acetone (Section 11.2.6) ........................
mg
Hexane (Section 11.2.8) .........................
mg
FIGURE 4—FIELD TRAIN RECOVERY
BLANK CONDENSABLE PARTICULATE
CALCULATIONS—Continued
Mass of the Field Train Recovery Blank
(not to exceed 2.0 mg) (Equation 2).
mg
a Field reagent blanks are optional and intended to provide the testing contractor with
information they can use to implement corrective actions, if necessary, to reduce the residual mass contribution from reagents used in
the field. Field reagent blanks are not used to
correct the CPM measurement results.
80171
FIGURE 5—OTHER FIELD TRAIN SAMPLE CONDENSABLE PARTICULATE
DATA—Continued
CPM Filter No.
Water volume added to purge train (max
50 ml) (Vp).
ml
Date
Run No.
CPM Filter No.
Field Train Recovery Blank Mass
Mass of Organic CPM (mob) (Section
11.2.3).
mg
Mass of Inorganic CPM (mib) (Equation
3).
mg
FIGURE 5—OTHER FIELD TRAIN SAMPLE CONDENSABLE PARTICULATE
DATA
Other Field Train Sample Condensable
Particulate Data
Water volume added to purge train (max
50 ml) (Vp).
ml
Date
Run No.
Plant
CPM Filter No.
Date
Water volume added to purge train (max
50 ml) (Vp).
Run No.
ml
FIGURE 6—CPM WORK TABLE
Calculations for Recovery of Condensable PM (CPM)
Plant
Date
Run No.
Sample Preparation—CPM Containers No. 1 and 2 (Section 11.1):
Was significant volume of water lost during transport? Yes or No
..............................
If Yes, measure the volume received
Estimate the volume lost during transport
Plant
..............................
..............................
ml
Date
Run No.
Was significant volume of organic rinse lost during transport? Yes or No
..............................
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If Yes, measure the volume received
Estimate the volume lost during transport.
For Titration:
Normality of NH4OH (N) (Section 10.2)
Volume of titrant (Vt) (Section 11.2.2.2)
Mass of NH4 added (mc) (Equation 1)
For CPM Blank Weights:
Inorganic Field Train Recovery Blank Mass(mib) (Section 9.9)
Organic Field Train Recovery Blank Mass (mob) (Section 9.9)
Mass of Field Train Recovery Blank (Mfb) (max. 2 mg) (Equation 2)
For CPM Train Weights:
Mass of Organic CPM (mo) (Section 11.2.3)
Mass of Inorganic CPM (mi) (Equation 3)
Total CPM Mass (mcpm) (Equation 4)
..............................
..............................
.............................. N
.............................. ml
.............................. mg
.............................. mg
.............................. mg
.............................. mg
.............................. mg
.............................. mg
.............................. mg
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Agencies
[Federal Register Volume 75, Number 244 (Tuesday, December 21, 2010)]
[Rules and Regulations]
[Pages 80118-80172]
From the Federal Register Online via the Government Printing Office [www.gpo.gov]
[FR Doc No: 2010-30847]
[[Page 80117]]
-----------------------------------------------------------------------
Part II
Environmental Protection Agency
-----------------------------------------------------------------------
40 CFR Part 51
Methods for Measurement of Filterable PM10 and
PM2.5 and Measurement of Condensable PM Emissions From
Stationary Sources; Final Rule
Federal Register / Vol. 75 , No. 244 / Tuesday, December 21, 2010 /
Rules and Regulations
[[Page 80118]]
-----------------------------------------------------------------------
ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 51
[EPA-HQ-OAR-2008-0348; FRL-9236-2]
RIN 2060-AO58
Methods for Measurement of Filterable PM10 and
PM2.5 and Measurement of Condensable PM Emissions From
Stationary Sources
AGENCY: Environmental Protection Agency (EPA).
ACTION: Final rule.
-----------------------------------------------------------------------
SUMMARY: This action promulgates amendments to Methods 201A and 202.
The final amendments to Method 201A add a particle-sizing device to
allow for sampling of particulate matter with mean aerodynamic
diameters less than or equal to 2.5 micrometers (PM2.5 or
fine particulate matter). The final amendments to Method 202 revise the
sample collection and recovery procedures of the method to reduce the
formation of reaction artifacts that could lead to inaccurate
measurements of condensable particulate matter. Additionally, the final
amendments to Method 202 eliminate most of the hardware and analytical
options in the existing method, thereby increasing the precision of the
method and improving the consistency in the measurements obtained
between source tests performed under different regulatory authorities.
This action also announces that EPA is taking no action to affect
the already established January 1, 2011 sunset date for the New Source
Review (NSR) transition period, during which EPA is not requiring that
State NSR programs address condensable particulate matter emissions.
DATES: This final action is effective on January 1, 2011.
ADDRESSES: EPA has established a docket for this action under Docket ID
No. EPA-HQ-OAR-2008-0348. All documents are listed in the https://www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., confidential business
information (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 form. Publicly available docket
materials are available either electronically at https://www.regulations.gov or in hard copy at the EPA Docket Center EPA/DC,
EPA West, Room 3334, 1301 Constitution Ave., NW., Washington, DC. The
Public Reading Room 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 Center is (202) 566-1742.
FOR FURTHER INFORMATION CONTACT: For general information, contact Ms.
Candace Sorrell, U.S. EPA, Office of Air Quality Planning and
Standards, Air Quality Assessment Division, Measurement Technology
Group (E143-02), Research Triangle Park, NC 27711; telephone number:
(919) 541-1064; fax number; (919) 541-0516; e-mail address:
sorrell.candace@epa.gov. For technical questions, contact Mr. Ron
Myers, U.S. EPA, Office of Air Quality Planning and Standards, Sector
Policies and Programs Division, Measurement Policy Group (D243-05),
Research Triangle Park, NC 27711; telephone number: (919) 541-5407; fax
number: (919) 541-1039; e-mail address: myers.ron@epa.gov.
SUPPLEMENTARY INFORMATION:
Acronyms and Abbreviations. The following acronyms and
abbreviations are used in this document.
[Delta]pmax maximum velocity pressure
[Delta]pmin minimum velocity pressure
[mu]m micrometers
ASTM American Society for Testing and Materials
AWMA Air and Waste Management Association
CAA Clean Air Act
CBI confidential business information
CCM Controlled Condensation Method
CPM condensable PM
DOP dioctyl phthalate
DOT Department of Transportation
DQO data quality objective
MSHA Mine Safety and Health Administration
NAAQS National Ambient Air Quality Standards
NSR New Source Review
NTTAA National Technology Transfer and Advancement Act of 1995
OSHA Occupational Safety and Health Administration
PCB polychlorinated biphenyl
PM particulate matter
PM10 particulate matter less than or equal to 10
micrometers
PM2.5 particulate matter less than or equal to 2.5
micrometers
ppmw parts per million by weight
PTFE polytetrafluoropolymer
RCRA Resource Conservation and Recovery Act
RFA Regulatory Flexibility Act
SBA Small Business Administration
SIP State Implementation Plan
SO2 sulfur dioxide
TDS total dissolved solids
TTN Technology Transfer Network
UMRA Unfunded Mandates Reform Act
www World Wide Web
The information in this preamble is organized as follows:
I. General Information
A. Does this action apply to me?
B. Where can I obtain a copy of this action and other related
information?
C. What is the effective date?
D. Judicial Review
II. Background
A. Why is EPA issuing this final action?
B. Particulate Matter National Ambient Air Quality Standards
C. Measuring PM Emissions
1. Method 201A
2. Method 202
III. Summary of Changes Since Proposal
A. Method 201A
B. Method 202
C. How will the final amendments to methods 201A and 202 affect
existing emission inventories, emission standards, and permit
programs?
IV. Summary of Final Methods
A. Method 201A
B. Method 202
V. Summary of Public Comments and Responses
A. Method 201A
B. Method 202
C. Conditional Test Method 039 (Dilution Method)
VI. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act
D. Unfunded Mandates Reform Act
E. Executive Order 13132: Federalism
F. Executive Order 13175: Consultation and Coordination With
Indian Tribal Governments
G. Executive Order 13045: Protection of Children From
Environmental Health and Safety Risks
H. Executive Order 13211: Actions Concerning Regulations That
Significantly Affect Energy Supply, Distribution, or Use
I. National Technology Transfer and Advancement Act
J. Executive Order 12898: Federal Actions To Address
Environmental Justice in Minority Populations and Low-Income
Populations
K. Congressional Review Act
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 total
particulate matter (PM), total PM with mean aerodynamic diameters less
than or equal to 10 micrometers ([mu]m) (PM10), or total
PM2.5, where EPA Method 202 is incorporated as a component
of the applicable test method.
In addition, this action applies to you if federal, State, or local
agencies take certain additional independent actions. For example, this
action applies to sources through actions by State and local agencies
that implement condensable PM (CPM) control measures to attain the
National Ambient
[[Page 80119]]
Air Quality Standards (NAAQS) for PM2.5 and specify the use
of Method 202 to demonstrate compliance with the control measures.
State and local agencies that specify the use of Method 201A or 202
would have to implement the following: (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 Method 201A or 202 (or an incorporated method
based upon Method 201A or 202). This action also applies to stationary
sources that are required to meet new applicable CPM requirements
established through federal or State permits or rules, such as New
Source Performance Standards and New Source Review (NSR), which specify
the use of Method 201A or 202 to demonstrate compliance with the
control measures.
The source categories and entities potentially affected include,
but are not limited to, the following:
------------------------------------------------------------------------
Examples of regulated
Category NAICS \a\ 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, 212111, Coal preparation
212112, 212113. plants.
331312, 331314... Primary and secondary
aluminum plants.
331111, 331513... Iron and steel
plants.
321219, 321211, Plywood and
321212. reconstituted
products plants.
------------------------------------------------------------------------
\a\ North American Industrial Classification System.
B. Where can I obtain a copy of this action and other related
information?
In addition to being available in the docket, an electronic copy of
these final rules are also available on the World Wide Web (https://www.epa.gov/ttn/) through the Technology Transfer Network (TTN).
Following the Administrator's signature, a copy of these final rules
will be posted on the TTN's policy and guidance page for newly proposed
or promulgated rules at https://www.epa.gov/ttn/oarpg. The TTN provides
information and technology exchange in various areas of air pollution
control.
C. What is the effective date?
The final rule amendments are effective on January 1, 2011. Section
553(d) of the Administrative Procedure Act (APA), 5 U.S.C. Chapter 5,
generally provides that rules may not take effect earlier than 30 days
after they are published in the Federal Register. EPA is issuing this
final rule under section 307(d)(1) of the Clean Air Act, which states:
``The provisions of section 553 through 557 * * * of Title 5 shall not,
except as expressly provided in this section, apply to actions to which
this subsection applies.'' Thus, section 553(d) of the APA does not
apply to this rule. EPA is nevertheless acting consistently with the
purposes underlying APA section 553(d) in making this rule effective on
January 1, 2011. Section 5 U.S.C. 553(d)(3) allows an effective date
less than 30 days after publication ``as otherwise provided by the
agency for good cause found and published with the rule.'' As explained
below, EPA finds that there is good cause for these rules to become
effective on or before January 1, 2011, even if this date is not 30
days from date of publication in the Federal Register.
While this action is being signed prior to December 1, 2010, there
may be a delay in the publication of this rule as it contains many
complex diagrams, equations, and charts, and is relatively long in
length. The purpose of the 30-day waiting period prescribed in 5 U.S.C.
553(d) is to give affected parties a reasonable time to adjust their
behavior and prepare before the final rule takes effect. Where, as
here, the final rule will be signed and made available on the EPA
website more than 30 days before the effective date, but where the
publication may be delayed due to the complexity and length of the
rule, that purpose is still met. Moreover, since permitting authorities
and regulated entities may need to rely on the methods described in
these rules to carry out requirements of the SIP and NSR implementation
rules that become effective on January 1, 2011 (see section III.C,
infra), there would be unnecessary regulatory confusion if a
publication delay caused this rule to become effective after January 1,
2011. Accordingly, we find good cause exists to make this rule
effective on or before January 1, 2011, consistent with the purposes of
5 U.S.C. 553(d)(3).\1\
---------------------------------------------------------------------------
\1\ We recognize that this rule could be published at least 30
days before January 1, 2011, which would negate the need for this
good cause finding, and we plan to request expedited publication of
this rule in order to decrease the likelihood of a publication
delay. However, as we cannot know the date of publication in advance
of signing this rule, we are proceeding with this good cause finding
for an effective date on or before January 1, 2011, in an abundance
of caution in order to avoid the unnecessary regulatory confusion
noted above.
---------------------------------------------------------------------------
D. Judicial Review
Under section 307(b)(1) of the Clean Air Act (CAA), judicial review
of this final action is available only by filing a petition for review
in the United States Court of Appeals for the District of Columbia
Circuit by February 22, 2011. Under CAA section 307(b)(2), the
requirements established by this action may not be challenged
separately in any civil or criminal proceedings brought by EPA to
enforce these requirements.
Section 307(d)(7)(B) of the CAA further provides that ``[o]nly an
objection to a rule or procedure which was raised with reasonable
specificity during the period for public comment (including any public
hearing) may be raised during judicial review.'' This section also
provides a mechanism for EPA to convene a proceeding for
reconsideration, ``[i]f the person raising an objection can demonstrate
to EPA that it was impracticable to raise such objection within [the
period for public comment] or if the grounds for such objection arose
after the period for public comment (but within the time specified for
judicial review) and if such objection is of central relevance to the
outcome of the rule.'' Any person seeking to make such a demonstration
to us should submit a Petition for Reconsideration to the Office of the
Administrator, U.S. EPA, Room 3000,
[[Page 80120]]
Ariel Rios Building, 1200 Pennsylvania Ave., NW., Washington, DC 20460,
with a copy to both the person(s) listed in the preceding FOR FURTHER
INFORMATION CONTACT section, and the Associate General Counsel for the
Air and Radiation Law Office, Office of General Counsel (Mail Code
2344A), U.S. EPA, 1200 Pennsylvania Ave., NW., Washington, DC 20460.
II. Background
A. Why is EPA issuing this final action?
Section 110 of the CAA, 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 (SIP) 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 inventories and analyses used in the State's attainment
demonstrations must consider PM10 and PM2.5
emissions from stationary sources that are significant contributors of
primary PM10 and PM2.5 emissions. Primary or
direct 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.
Appendix A to subpart A of 40 CFR part 51 (Requirements for
Preparation, Adoption, and Submittal of Implementation Plans) defines
primary PM10 and PM2.5 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 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, EPA previously developed and promulgated Method
201A (Determination of PM10 Emissions (Constant Sampling
Rate Procedure)) and Method 202 (Determination of Condensable
Particulate Emissions from Stationary Sources) in 40 CFR part 51,
appendix M (Recommended Test Methods for State Implementation Plans).
On April 17, 1990 (56 FR 65433), EPA promulgated Method 201A in
appendix M of 40 CFR part 51 to provide a test method for measuring
filterable PM10 emissions from stationary sources. In EPA
Method 201A, a gas sample is extracted at a constant flow rate through
an in-stack sizing device that directs particles with aerodynamic
diameters less than or equal to 10 [mu]m to a filter. The particulate
mass collected on the filter is determined gravimetrically after
removal of uncombined water.
On December 17, 1991 (56 FR 65433), EPA promulgated Method 202 in
appendix M of 40 CFR part 51 to provide a test method for measuring CPM
from stationary sources. Method 202 uses 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
used by State and local regulatory entities at the time Method 202 was
being developed.
In this action, we are finalizing amendments to Methods 201A and
202 to improve the measurement of fine PM emissions. For Method 201A,
the final amendments add a particle-sizing device to allow for sampling
of PM2.5 emissions. For Method 202, the final amendments
will (1) revise the sample collection and recovery procedures of the
method to reduce the potential for formation of reaction artifacts that
are not related to the primary emission of CPM from the source but may
be counted erroneously as CPM when using Method 202, and (2) eliminate
most of the hardware and analytical options in the existing method.
These changes increase the precision of Method 202 and improve the
consistency in the measurements obtained between source tests performed
under different regulatory authorities.
B. Particulate Matter National Ambient Air Quality Standards
Section 108 and 109 of the CAA govern the establishment and
revision of the NAAQS. Section 108 of the CAA (42 U.S.C. 7408) directs
the Administrator to identify and list ``air pollutants'' that ``in his
judgment, may reasonably be anticipated to endanger public health and
welfare'' and whose ``presence * * * in the ambient air results from
numerous or diverse mobile or stationary sources'' and to issue air
quality criteria for those that are listed. Air quality criteria are
intended to ``accurately reflect the latest scientific knowledge useful
in indicating the kind and extent of identifiable effects on public
health or welfare which may be expected from the presence of [a]
pollutant in ambient air * * *.'' Section 109 of the CAA (42 U.S.C.
7409) directs the Administrator to propose and promulgate primary and
secondary NAAQS for pollutants listed under CAA section 108 to protect
public health and welfare, respectively. Section 109 of the CAA also
requires review of the NAAQS at 5-year intervals and that an
independent scientific review committee ``shall complete a review of
the criteria * * * and the national primary and secondary ambient air
quality standards * * * and shall recommend to the Administrator any
new * * * standards and revisions of existing criteria and standards as
may be appropriate * * *.'' Since the early 1980s, this independent
review function has been performed by the Clean Air Scientific Advisory
Committee.
Initially, EPA established the PM NAAQS on April 30, 1971 (36 FR
8186), based on the original criteria document (Department of Health,
Education, and Welfare, 1969). The reference method specified for
determining attainment of the original standards was the high-volume
sampler, which collects PM up to a nominal size of 25 to 45 [mu]m
(referred to as total suspended particulates or TSP). On October 2,
1979 (44 FR 56730), EPA announced the first periodic review of the air
quality criteria and PM NAAQS, and significant revisions to the
original standards were promulgated on July 1, 1987 (52 FR 24634). In
that decision, EPA changed the indicator for particles from TSP to
PM10. When that rule was challenged, the court upheld
revised standards in all respects. Natural Resources Defense Council v.
Administrator, 902 F. 2d 962 (D.C. Cir. 1990, cert. denied, 498 U.S.
1082 (1991).
In April 1994, EPA announced its plans for the second periodic
review of the air quality criteria and PM NAAQS, and the Agency
promulgated significant revisions to the NAAQS on July 18, 1997 (62 FR
38652). In that decision, EPA revised the PM NAAQS in several respects.
While EPA determined that the PM NAAQS should continue to focus on
particles less than or equal to 10 [mu]m in diameter (PM10),
EPA also determined that the fine and coarse fractions of
PM10 should be considered separately. EPA added new
standards, using PM2.5 as the indicator for fine particles
(with PM2.5 referring to particles with a nominal mean
aerodynamic diameter less than or equal to 2.5 [mu]m), and using
PM10 as the indicator for purposes of regulating the coarse
fraction of PM10.
Following promulgation of the 1997 PM NAAQS, petitions for review
were filed by a large number of parties
[[Page 80121]]
addressing a broad range of issues. In May 1999, a three-judge panel of
the U.S. Court of Appeals for the District of Columbia Circuit issued
an initial decision that upheld EPA's decision to establish fine
particle standards. American Trucking Associations v. EPA, 175 F.3d
1027, 1055 (D.C. Cir. 1999), reversed in part on other grounds in
Whitman v. American Trucking Associations, 531 U.S. 457 (2001). The
panel also found ``ample support'' for EPA's decision to regulate
coarse particle pollution, but vacated the 1997 PM10
standards concluding that EPA had not provided a reasonable explanation
justifying use of PM10 as an indicator for coarse particles.
(Id. at 1054-55.) Pursuant to the court's decision, EPA removed the
vacated 1997 PM10 standards but retained the pre-existing
1987 PM10 standards (65 FR 80776, December 22, 2000).
On October 23, 1997, EPA published its plans for the third periodic
review of the air quality criteria and PM NAAQS (62 FR 55201),
including the 1997 PM2.5 standards and the 1987
PM10 standards. On October 17, 2006, EPA issued its final
decision to revise the primary and secondary PM NAAQS to provide
increased protection of public health and welfare respectively (71 FR
61144). With regard to the primary and secondary standards for fine
particles, EPA revised the level of the 24-hour PM2.5
standard to 35 [mu]g per cubic meter ([mu]g/m\3\), retained the level
of the annual PM2.5 annual standard at 15 [mu]g/m\3\, and
revised the form of the annual PM2.5 standard by narrowing
the constraints on the optional use of spatial averaging. With regard
to the primary and secondary standards for PM10, EPA
retained the 24-hour PM10 standard (150 [mu]g/m\3\) and
revoked the annual standard because available evidence generally did
not suggest a link between long-term exposure to current ambient levels
of coarse particles and health or welfare effects.
C. Measuring PM Emissions
Section 110 of the CAA, as amended (42 U.S.C. 7410), requires State
and local air pollution control agencies to develop and submit plans
(SIP) for EPA approval that provide for the attainment, maintenance,
and enforcement of the NAAQS in each air quality control region (or
portion thereof) within such State. 40 CFR part 51 (Requirements for
Preparation, Adoption, and Submittal of Implementation Plans) specifies
the requirements for SIP. Appendix A to subpart A of 40 CFR part 51,
defines primary PM10 and PM2.5 as including both
the filterable and condensable fractions of PM. Filterable PM consists
of those particles 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 train. Condensable PM is the material that is in vapor
phase at stack conditions but which condenses and/or reacts upon
cooling and dilution in the ambient air to form solid or liquid PM
immediately after discharge from the stack.
Promulgation of the 1987 NAAQS created the need for methods to
quantify PM10 emissions from stationary sources. In
response, EPA developed and promulgated the following test methods:
Method 201A--Determination of PM10 Emissions
(Constant Sampling Rate Procedure), and
Method 202--Determination of Condensable Particulate
Emissions from Stationary Sources.
1. Method 201A
Method 201A is a test method for measuring filterable
PM10 emissions from stationary sources. With the exception
of the PM10-sizing device, the current Method 201A sampling
train is the same as the sampling train used for EPA Method 17 of
appendix A-3 to 40 CFR part 60.
Method 201A cannot be used to measure emissions from stacks that
have entrained moisture droplets (e.g., from a wet scrubber stack)
since these stacks may have water droplets that are larger than the cut
size of the PM10 sizing device. The presence of moisture
would prevent an accurate measurement of total PM10 since
any PM10 dissolved in larger water droplets would not be
collected by the sizing device and would consequently be excluded in
determining total PM10 mass. To measure PM10 in
stacks where water droplets are known to exist, EPA's Technical
Information Document 09 (Methods 201 and 201A in Presence of Water
Droplets) recommends use of Method 5 of appendix A-3 to 40 CFR part 60
(or a comparable method) and consideration of the total particulate
catch as PM10 emissions.
Method 201A is also not applicable for stacks with small diameters
(i.e., 18 inches or less). The presence of the in-stack nozzle/cyclones
and filter assembly in a small duct will cause significant cross-
sectional area interference and blockage leading to incorrect flow
calculation and particle size separation. Additionally, the type of
metal used to construct the Method 201A cyclone may limit the
applicability of the method when sampling at high stack temperatures
(e.g., stainless steel cyclones are reported to gall and seize at
temperatures greater than 260 [deg]C).
2. Method 202
Method 202 measures CPM from stationary sources. Method 202
contains several optional procedures that were intended to accommodate
the various test methods used by State and local regulatory entities at
the time Method 202 was being developed.
When conducted consistently and carefully, Method 202 provides
acceptable precision for most emission sources. Method 202 has been
used successfully in regulatory programs where the emission limits and
compliance demonstrations are established based on a consistent
application of the method and its associated options. However, when the
same emission source is tested using different combinations of the
optional procedures, there appears to be large variations in the
measured CPM emissions. Additionally, during validation of the
promulgated 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. We consistently
maintain that the artifact formation can be reduced by at least 90
percent if a one-hour nitrogen purge of the impinger water is used to
remove SO2 before it can form sulfuric acid (this is our
preferred application of the Method 202 optional procedures).
Inappropriate use or omission of the preferred or optional procedures
in Method 202 can increase the potential for artifact formation.
Considering the potential for variations in measured CPM emissions,
we believe that further verification and refinement of Method 202 is
appropriate to minimize the potential for artifact formation. We
performed several studies to assess artifact formation when using
Method 202. The results of our 1998 laboratory study and field
evaluation commissioned to evaluate the impinger approach can be found
in ``Laboratory and Field Evaluation of EPA's Method 5 Impinger Catch
for Measuring Condensible Matter from Stationary Sources'' at https://www.epa.gov/ttn/emc/methods/m202doc1.pdf.
The 1998 study verified the need for a nitrogen purge when
SO2 is present in stack gas and provided guidance for
analyzing the collected samples. In 2005, an EPA contractor conducted a
[[Page 80122]]
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 at https://www.epa.gov/ttn/emc/methods/m202doc2.pdf. This report also verified the need for a nitrogen purge
and identified the primary factors that affect artifact formation.
Also in 2005, a private testing contractor presented a possible
minor modification to Method 202 at the Air and Waste Management
Association (AWMA) specialty conference. The proposed modification, as
described in their presentation titled ``Optimized Method 202 Sampling
Train to Minimize the Biases Associated with Method 202 Measurement of
Condensable Particulate Matter Emissions,'' involved the elimination of
water from the first impingers. The presentation (available at https://www.epa.gov/ttn/emc/methods/m202doc3.pdf) concluded that modification
of the promulgated method to use dry impingers resulted in a
significant additional reduction in the sulfate artifact.
In 2006, we began to conduct laboratory studies in collaboration
with several stakeholders to characterize the artifact formation and
other uncertainties associated with conducting Method 202 and to
identify procedures that would minimize uncertainties when using Method
202. Since August 2006, we conducted two workshops in Research Triangle
Park, NC to present and request comments on our plan for evaluating
potential modifications to Method 202 that would reduce artifact
formation, and also to discuss (1) Our progress in characterizing the
performance of the modified method, (2) issues that require additional
investigation, (3) the results of our laboratory studies, and (4) our
commitments to extend the investigation through stakeholders external
to EPA. Another meeting was held with experienced stack testers and
vendors of emissions monitoring equipment to discuss hardware issues
associated with modifications of the sampling equipment and the
glassware for the proposed CPM test method. Summaries of the method
evaluations, as well as meeting minutes from our workshops, can be
found at https://www.epa.gov/ttn/emc/methods/method202.html.
The laboratory studies that were performed fulfill a commitment in
the preamble to the Clean Air Fine Particle Implementation Rule (72 FR
20586, April 25, 2007) to examine the relationship between several
critical CPM sampling and analysis parameters and, to the extent
necessary, promulgate revisions to incorporate improvements in the
method. While these improvements in the stationary source test method
for CPM will provide for more accurate and precise measurement of all
PM, the addition of PM2.5 as an indicator of health and
welfare effects by the 1997 NAAQS revisions generates the need to
quantify PM2.5 emissions from stationary sources. To respond
to this need, we are promulgating revisions to incorporate this
capability into the test method for filterable PM10.
III. Summary of Changes Since Proposal
The methods in this final action contain several changes that were
made as a result of public comments. The following sections present a
summary of the changes to the methods. We explain the reasons for these
changes in detail in the Summary of Public Comments and Responses
section of this preamble.
A. Method 201A
Method 201A contains the following changes and clarifications:
Revised Section 1.5 to clarify that Method 201A cannot be
used to measure emissions from stacks that have entrained moisture
droplets (e.g., from a wet scrubber stack).
Removed the language in proposed Section 1.5 regarding
ambient air contributions to PM. The decision to correct results for
ambient air contributions is up to the permitting or regulatory
authority.
Added definitions of Primary PM, Filterable PM, Primary
PM2.5, Primary PM10, and CPM to Section 3.0.
Added a requirement to Sections 6.1.3 and 8.6.3 stating
that the filter must not be compressed between the gasket and the
filter housing.
Clarified the sample recovery and analysis equipment in
Section 6.2, including acceptable materials of construction, analytical
balance, and fluoropolymer (polytetrafluoroethylene) beaker liners.
Revised Section 6.2 to add performance-based, residual
mass contribution specifications for containers rather than specifying
the type of container that must be used (storage containers must not
contribute more than 0.1 mg of residual mass to the CPM measurements).
Revised Section 8.3.1 (regarding sampling ports) to state
that a 4-inch port should be adequate for the single PM2.5
(or single PM10) sampling apparatus. However, testers will
not be able to use conventional 4-inch ports if the combined dimension
of the PM10 cyclone and the nozzle extending from the
cyclone exceeds the internal diameter of the port.
Clarified the sampling procedures in Section 8.3.1 for
cases where the PM2.5 cyclone is used without the
PM10 cyclone. In these cases, samples are collected using
the procedures specified in Section 11.3.2.2 of EPA Method 1, and the
sampling time is extended at the replacement sampling point to include
the duration of the unreachable traverse points.
Revised Section 8.3.2.2 to clarify that Method 201A is not
applicable for stack diameters less than 26.5 inches when the combined
PM10/PM2.5 cyclone is used. The in-stack nozzle/
cyclones and filter assembly in stacks less than 26.5 inches in
diameter would cause significant cross-sectional area interference and
blockage, leading to incorrect flow calculation and particle size
separation.
Revised Section 8.5.5 to express the maximum failure rate
of values outside the minimum-maximum velocity pressure range in terms
of percent of values outside the range instead of the number of
traverse points outside the range.
Revised section 8.6.1 to clarify that alternative designs
are acceptable for fastening caps or covers to cyclones to avoid
galling of the cyclone component threads in hot stacks. The method may
be used at temperatures up to 1,000[deg]F using stainless steel
cyclones that are bolted together, rather than screwed together. Using
``break-away'' stainless steel bolts facilitates disassembly and
circumvents the problem of thread galling.
Clarified sampling procedures in Section 8.7.3.3 to
maintain the temperature of the cyclone sampling head within 10 [deg]C of the stack temperature and to maintain flow until
after removing and before inserting the sampling head.
Revised Section 11.2.7 to allow the use of tared
fluoropolymer beaker liners for the acetone field reagent blank.
B. Method 202
Method 202 contains the following changes and clarifications:
Clarified the terminology used to refer to laboratory and
field blanks throughout the method.
For health and safety reasons, replaced the use of
methylene chloride with hexane throughout the method.
Clarified Section 1.2 by moving the discussion of
filterable PM methods used in conjunction with Method 202 to Section
1.5.
[[Page 80123]]
Clarified Section 1.6 to specify that Method 202 can be
used for measuring CPM in stacks that contain entrained moisture if the
sampling temperature is sufficiently high to keep the moisture in the
vapor phase.
Moved the recommendation to develop a health and safety
plan from Section 9.4 to Section 5.0.
Added amber glass bottles to the list of sample recovery
equipment in Section 6.2.
Added alternatives (fluoropolymer beaker liners or
fluoropolymer baggies) to weighing tins to the list of analytical
equipment in Section 6.2.2 (Section 6.3 of the proposed method).
Added specifications for sample drying equipment in
Section 6.2.2 (Section 6.3 of the proposed method).
Clarified Section 6.3.7 regarding the use of an analytical
balance with sensitivity to 0.00001 g (0.01 milligram).
Added an option to use a colorimetric pH indicator instead
of a pH meter in Section 6.2.2 (Section 6.3 of the proposed method).
Added a sonication device to the list of analytical
equipment in Section 6.2.2 (Section 6.3 of the proposed method).
Added performance-based, residual mass contribution
specifications for containers and wash bottles in Section 6.2.2
(Section 6.3 of the proposed method) rather than specifying the type of
container that must be used.
Replaced the prescriptive language regarding filter
materials in Section 7.1.1 with performance-based requirements limiting
the residual mass contribution.
Replaced the prescriptive language regarding water quality
in Section 7.1.3 with performance-based requirements for residual mass
content.
Clarified Section 8.2 to specify that cleaned glassware
must be used at the start of each new source category tested at a
single facility.
Added a performance-based option to Section 8.4 to conduct
a field train proof blank rather than meeting the glassware baking
requirements in Section 8.2.
Clarified the sampling train configuration for the
nitrogen purge procedures in Section 8.5.3.2 regarding pressurized
purges.
C. How will the final amendments to methods 201A and 202 affect
existing emission inventories, emission standards, and permit programs?
We anticipate that over time the changes in the test methods
finalized in this action will result in, among other positive outcomes,
more accurate emissions inventories of direct PM emissions and
emissions standards that are more indicative of the actual impact of
the source on the ambient air quality.
Accurate emission inventories are critical for regulatory agencies
to develop the control strategies and demonstrations necessary to
attain air quality standards. When implemented, the test method
revisions should improve our understanding of PM emissions due to the
increased availability of more accurate emission tests and eventually
through the incorporation of less biased test data into existing
emissions factors. For CPM, the use of the revised method could reveal
a reduced level of CPM emissions from a source compared to the
emissions that would have been measured using Method 202 as typically
performed. However, there may be some cases where the revised test
method would reveal an increased level of CPM emissions from a source,
depending on the relative emissions of filterable and CPM emissions
from the source. For example, the existing Method 202 allows complete
evaporation of the water containing inorganic PM at 105 [deg]C (221
[deg]F), where the revised method requires the last 10 ml of the water
to be evaporated at room temperature (not to exceed 30 [deg]C (85
[deg]F)), thereby retaining the CPM that would evaporate at the
increased temperature.
Prior to our adoption of the 1997 PM2.5 NAAQS, several
State and local air pollution control agencies had developed emission
inventories that included CPM. Additionally, some agencies established
enforceable CPM emissions limits or otherwise required that PM
emissions testing include measurement of CPM. While this approach was
viable in cases where the same test method was used to develop the CPM
regulatory limits and to demonstrate facility compliance, there are
substantial inconsistencies within and between States regarding the
completeness and accuracy of CPM emission inventories and the test
methods used to measure CPM emissions and demonstrate facility
compliance.
These amendments would serve to mitigate the potential difficulties
that can arise when EPA and other regulatory entities attempt to use
the test data from State and local agencies with inconsistent CPM test
methods to develop emission factors, determine program applicability,
or to establish emissions limits for CPM emission sources within a
particular jurisdiction. For example, problems can arise when the test
method used to develop a CPM emission limit is not the same as the test
method specified in the rule for demonstrating compliance because the
different test methods may quantify different components of PM (e.g.,
filterable versus condensable). Also, when emissions from State
inventories are modeled to assess compliance with the NAAQS, the
determination of direct PM emissions may be biased high or low,
depending on the test methods used to estimate PM emissions, and the
atmospheric conversion of SO2 to sulfates (or sulfur
trioxide, SO3) may be inaccurate or double-counted.
Additionally, some State and local regulatory authorities have assumed
that EPA Method 5 of appendix A-3 to 40 CFR part 60 (Determination of
Particulate Matter Emissions from Stationary Sources) provides a
reasonable estimate of PM10 emissions. This assumption is
incorrect because Method 5 does not provide particle sizing of the
filterable component and does not quantify particulate caught in the
impinger portion of the sampling train. Similar assumptions for
measurements of PM2.5 will result in greater inaccuracies.
With regard to State permitting programs, we recognize that, in
some cases, existing best available control technology, lowest
achievable emission rate, or reasonably available control technology
limits have been based on an identified control technology, and that
the data used to determine the performance of that technology and to
establish the limits may have focused on filterable PM and, thus, did
not completely characterize PM emissions to the ambient air. While the
source test methods used by State programs that developed the
applicable permit limit may not have fully characterized the PM
emissions, we have no information that would indicate that the test
methods are inappropriate indicators of the control technologies'
performance for the portion of PM emissions that was addressed by the
applicable requirement. As promulgated in the Clean Air Fine Particle
Implementation Rule, after January 1, 2011, States are required to
consider inclusion of CPM emissions in new or revised emissions limits
that they establish. We will defer to the individual State's judgment
as to whether, and at what time it is appropriate to revise existing
facility emission limits or operating permits to incorporate
information from the revised CPM test method when it is promulgated.
With regard to operating permits, the title V permit program does
not generally impose new substantive air quality control requirements.
In general, after emissions limits are established as CAA requirements
under the SIP or a
[[Page 80124]]
SIP-approved pre-construction review permit, they are included in the
title V permits. Obviously, title V permits should be updated to
reflect any revision of existing emission limits or new emission limits
created in the context of the underlying applicable requirements. Also,
if a permit contains previously promulgated test methods, it is not a
given that the permit would always have to be revised should these test
method changes be finalized (e.g., where test methods are incorporated
into existing permits through incorporation by reference, no permit
terms or conditions would necessarily have to change to reflect changes
to those test methods). In any event, the need for action related to
emissions source permitting, due to these changes to the test methods,
would be determined based upon several factors such as the exact
wording of the existing operating permit, the requirements of the EPA-
approved SIP, and any changes that may need to be made to pre-
construction review permits with respect to CPM measurement (e.g.,
emissions estimates may be based upon a source test method that did not
measure CPM or upon a set of Method 202 procedures that underestimated
CPM emissions).
In recognition of these issues, the Clean Air Fine Particle
Implementation Rule contains provisions establishing a transition
period for developing emission limits for condensable direct
PM2.5 that are needed to demonstrate attainment of the
PM2.5 NAAQS. The transition period for CPM is the time
period during which the new rules and NSR permits issued to stationary
sources are not required to address the condensable fraction of the
sources' PM emissions. The end date of the transition period (January
1, 2011) was adopted in the final Clean Air Fine Particle
Implementation Rule (72 FR 20586, April 25, 2007) and in the final
Implementation of the New Source Review Program for Particulate Matter
Less Than 2.5 Micrometers (PM2.5) rule (73 FR 28321, May 16,
2008). As discussed in these two rules, the intent of the transition
period (which ends January 1, 2011) was to allow time for EPA to issue
a CPM test method through notice and comment rulemaking, and for
sources and States to collect additional total primary (filterable and
condensable) PM2.5 emissions data to improve emissions
information to the extent possible. In the PM2.5 NSR
Implementation Rule, we stated that as part of this test methods
rulemaking, we would ``take comment on an earlier closing date for the
transition period in the NSR program if we are on track to meet our
expectation to complete the test method rule much earlier than January
1, 2011'' (73 FR 28344). In the notice of proposed rulemaking for this
final rule on amendments to Method 201A and 202, EPA sought comment on
whether to end the NSR transition period for CPM early (74 FR 12976).
In this final rule, EPA is taking no action to affect the already
established January 1, 2011 sunset date for the NSR transition period.
Source test data collected with the use of this updated test method
will be incorporated into the tools (e.g., emission factors, emission
inventories, air quality modeling) used to demonstrate the attainment
of air quality standards. Areas that are designated nonattainment for
the 1997 PM2.5 NAAQS, and that have approved attainment
dates of 2014 or 2015, are required to develop a mid-course review in
2011. If it is determined that additional control measures are needed
to ensure the area will be on track to attain the standard by the
attainment date, any new direct PM2.5 emission limits
adopted by the State must address the condensable fraction and the
filterable fraction of PM2.5. Additionally, the new test
data could be used to improve the applicability and performance
evaluations of various control technologies.
IV. Summary of Final Methods
A. Method 201A
Method 201A measures PM emissions from stationary sources. The
amendments to Method 201A add a PM2.5 measurement device
(PM2.5 cyclone) that allows the method to measure filterable
PM2.5, filterable PM10, or both filterable
PM2.5 and filterable PM10. The method can also be
used to measure coarse particles (i.e., the difference between measured
PM10 concentration and the measured PM2.5
concentration).
The amendments also add a PM2.5 cyclone to create a
sampling train that includes a total of two cyclones (one cyclone to
segregate particles with aerodynamic diameters greater than 10 [mu]m
and one cyclone to segregate particles with aerodynamic diameters
greater than 2.5 [mu]m) and a final filter to collect particles with
aerodynamic diameters less than or equal to 2.5 [mu]m. The
PM2.5 cyclone is inserted between the PM10
cyclone and the filter of the Method 201A sampling train.
The revised method has several limitations. The method cannot be
used to measure emissions from stacks that have entrained moisture
droplets (e.g., from a wet scrubber stack) because size separation of
the water droplets is not representative of the dry particle size
released into the air. In addition, the method is not applicable for
stacks with diameters less than 25.7 inches when the combined
PM10/PM2.5 cyclone is used. Also, the method may
not be suitable for sources with stack gas temperatures exceeding 260
[deg]C (500 [deg]F) when cyclones with screw-together caps are used
because the threads of the cyclone components may gall or seize, thus
preventing the recovery of the collected PM. However, the method may be
used at temperatures up to 1,000 [deg]F when using stainless steel
cyclones that are bolted together rather than screwed together. Using
``break-away'' stainless steel bolts facilitates disassembly and
circumvents the problem of thread galling. The method may also be used
at temperatures up to 2,500 [deg]F when using specialty high-
temperature alloys.
B. Method 202
Method 202 measures concentrations of CPM in stationary source
sample gas after the filterable PM has been removed using another test
method such as Method 5, 17, or 201A. The CPM sampling train begins at
the back half of the filterable PM filter holder and consists of a
condenser, two dry impingers (temperatures maintained to less than 30
[deg]C (85 [deg]F)), and a CPM filter (temperature maintained between
20 [deg]C (65 [deg]F) and 30 [deg]C (85 [deg]F)). During the test,
sample gases are cooled and CPM is collected in the dry impingers and
on the CPM filter. As soon as possible after the post-test leak check
has been conducted, any water collected in the dry impingers is purged
with nitrogen gas for at least one hour to remove dissolved
SO2 gas.
After the nitrogen purge, the sampling train components downstream
of the filterable PM filter (i.e., the probe extension (if any),
condenser, impingers, front half of CPM filter holder, and the CPM
filter) are rinsed with water to recover the inorganic CPM. The water
rinse is followed by an acetone rinse and a hexane rinse to recover the
organic CPM. The CPM filter is extracted using water to recover the
inorganic components and hexane to recover the organic portion. The
inorganic and organic fractions are then dried and the residues
weighed. The sum of both fractions represents the total CPM collected
by Method 202.
V. Summary of Public Comments and Responses
In response to the March 25, 2009 proposed revisions to EPA Methods
201A and 202, EPA received public
[[Page 80125]]
comment letters from industry representatives, trade associations,
State agencies, and environmental organizations. The public comments
submitted to EPA addressed the proposed revisions to Methods 201A and
202 and our request for comments on whether to end the transition
period for CPM in the NSR program on a date earlier than the current
end date of January 1, 2011.
This section provides responses to the more significant public
comments received on the proposed revisions to Methods 201A and 202.
Summaries and responses for all comments related to the proposed
revisions to Methods 201A and 202, including those addressed in this
preamble, are contained in the response to comments document located in
the docket for this final action (Docket ID No. EPA-HQ-OAR-2008-0348).
A. Method 201A
1. Speciation
Comment: One commenter stated that EPA should include guidance in
Method 201A concerning speciation of the constituents present in the
PM10, PM10-PM2.5, and PM2.5
size fractions. The commenter believes this information should be
provided to support the use of speciated PM10,
PM10-PM2.5, and PM2.5 data in source
apportionment studies.
Response: EPA did not revise the method to provide guidance for
speciation of various particle fractions for source apportionment
because Method 201A is not a speciation method. However, with judicious
selection of filter media, sources may use this method for speciating
the less volatile metals and use these data in source apportionment
studies. Including details to adapt this method for speciation analysis
would unduly increase the complexity of the method without increasing
the precision of the mass measurements.
2. Catch Weight and Sampling Times
Comment: Several commenters requested that EPA specify the minimum
solids catch weights needed in the PM10 and PM2.5
size fractions to help testing organizations determine the necessary
sampling times, especially for sources with low PM concentrations.
Other commenters expressed concern about extended sampling times that
would be necessary to obtain enough sample to weigh accurately. One
commenter stated that a reasonable limit must be put on sampling volume
to limit potentially unnecessary sampling time and exorbitant stack
testing costs that could quickly escalate with such a requirement.
Response: We agree with the commenters that collecting sufficient
weighable mass is important for the method to be precise. We also
understand that the sampling rate used to attain the cyclone cut-points
is typically less than the rate used during Method 5 sampling. However,
EPA did not revise the method to dictate a minimum sampling volume or
minimum catch weight that would be necessary to obtain a valid sample.
One reason for not specifying a minimum sampling volume or minimum
catch weight is that different regulatory authorities and testing
programs have differing measurement goals. For example, some regulatory
authorities will accept less precision if results are well below
compliance limits. State agencies or individual regulated facilities
may develop data quality objectives (DQO) for the test program, which
may specify minimum detection limits, and/or minimum sample volume,
and/or catch weight that would demonstrate that DQO can be met. Stack
samplers should take into consideration the compliance limits set by
their regulatory authority and determine the minimum amount of stack
gas needed to show compliance if the mass of particulate is below the
detection limit.
Stack testers can use the minimum detection limit to determine the
minimum stack gas volume. The stack tester may be able to estimate the
necessary stack gas volume based on how much PM the source or source
category is expected to emit (which could be determined from a previous
test or from knowledge of the emissions for that source category).
Alternatively, the minimum detection limit for a source can be
determined by calculating the percent relative standard deviation for a
series of field train recovery blanks. You will not be able to measure
below the average train recovery blank level, and EPA recommends
calculating a tester-specific detection limit by multiplying the
standard deviation of field recovery train blanks by the appropriate
``Student's t value'' (e.g., for seven field train recovery blanks, the
standard deviation of the results would be multiplied by three). Short
of having Method 201A field recovery train blanks for cyclone and
filter components of the sampling train, you may use the detection
limit determined from EPA field tests.
An estimated detection limit was determined from an EPA field
evaluation of proposed Method 201A (see ``Field Evaluation of an
Improved Method for Sampling and Analysis of Filterable and Condensable
PM,'' Docket ID No. EPA-HQ-OAR-2008-0348). The estimated detection
limit was calculated from the standard deviation of the differences
from 10 quadruplicate sampling runs multiplied by the appropriate
``Student's t value'' (n-1 = 9). Detection limits determined in this
manner were (1) Total filterable PM: 2.54 mg; (2) PM10: 1.44
mg; and (3) PM2.5: 1.35. These test runs showed more
filterable particulate in the PM2.5 fraction, and total
filterable particulate detection limits may be biased high due to the
small particulate mass collected in the fraction greater than
PM10.
Comment: Two commenters questioned the use of reference methods to
correct for ambient air in Section 1.5 of the proposed Method 201A. One
commenter believed that the statement would be used as a means to blame
non-compliance on ambient contributions and would result in legal
challenges and disputes of test results. The other commenter questioned
whether it was the intent of EPA to not allow the use of the CPM test
method for low-temperature sources.
Response: We agree with the commenters that Section 1.5 of the
proposed method was unclear. Thus, Section 1.5 (Additional Methods) has
been removed from the final method. For sources that have very low PM
emissions, such as processes that burn clean fuels (e.g., natural gas)
and/or use large volumes of dilution air (e.g., gas turbines and
thermal oxidizers), any ambient air particulate introduced into the
process operation could be a large component of total outlet PM
emissions. However, the decision to correct results for fine PM
measurements to account for ambient air contributions is up to the
permitting or regulatory authority. It is likely that these adjustments
would be limited to gas turbines and possibly sources fired with clean
natural gas.
Comment: Commenters expressed concern about the lack of a test
method to measure PM2.5 in stacks with entrained moisture.
Another commenter urged EPA to continue work to identify or develop a
method for measuring filterable (or total) PM at sources with entrained
moisture droplets in the stack (e.g., units with wet stacks due to wet
flue gas desulfurization or wet scrubbers). Commenters requested that
EPA provide guidance or identify a viable alternative for high-moisture
stacks as soon as possible. One commenter stated that when conducting
emission testing at facilities with similar wet stack conditions as
described in the proposal preamble (74 FR 12973), that they support
EPA's position on the
[[Page 80126]]
limitations of the proposed Method 201A.
One commenter was not satisfied with the use of Method 5 as the
only acceptable method for sources with entrained water droplets. To
provide more accurate emissions data for sources with ``wet'' stacks,
the commenter is sponsoring the development of an advanced manual
sampling technique that can accurately measure filterable
PM2.5 in stacks with entrained water droplets. The commenter
expects to complete field tests of this method in the near future. The
commenter will share laboratory and field test evaluations of this new
method. The commenter believes that this new method for filterable
PM2.5 emissions in ``wet'' stacks will be highly compatible
with proposed Method 201A for filterable PM2.5 emission
testing in ``dry'' stacks.
Response: We are currently developing a method to measure PM in
stacks with saturated water vapors and laboratory testing is ongoing.
EPA has committed a significant budget and personnel to developing an
acceptable method for sources with wet stacks and we plan to offer the
method and protocol as soon as possible. EPA's method development and
evaluation is focused on the ``Dried Particle Method'' (See ``Lab Work
to Evaluate PM2.5 Collection with a Dilution Monitoring
Device for Data Gathering for Emission Factor Development (Final
Report)'' in Docket ID No. EPA-HQ-OAR-2008-0348) that directly measures
the mass emission rate of particles with specified aerodynamic size. In
the meantime, the promulgated amendments to Methods 201A and 202
improve their performance and reduce known artifacts. Testers should
use these final, amended methods until a PM2.5 method for
stack gases containing water droplets is promulgated.
Regarding the advanced manual sampling technique that the commenter
is currently developing for use in ``wet'' stacks, EPA acknowledges the
sampling evaluations being conducted by the commenter. When the data
become available, we will review the data to determine if the
consistency and performance achieved by the advanced manual sampling
technique referenced by the commenter are comparable to EPA's wet-stack
sampling method currently under development. If the data are
comparable, we will consider whether the commenter's sampling technique
should be addressed (e.g., as an alternative method) when we propose an
EPA wet-stack, particle-sizing method in the future.
Comment: Several commenters disagreed with EPA's recommendation to
use Method 5 on stacks with entrained moisture and to consider all the
collected mass to be PM2.5. Commenters stated that the
categorization of all PM measured by Method 5 as PM2.5
overstates the true emissions. One commenter supported EPA's
recommendation to use Method 5 to determine PM10/
PM2.5 filterable mass when measuring emissions following a
wet scrubber. Another commenter stated that when conducting emissions
testing at facilities with similar wet stack conditions, as described
in the proposal preamble (74 FR 12973), they