[Federal Register Volume 75, Number 244 (Tuesday, December 21, 2010)]
[Rules and Regulations]
[Pages 80118-80172]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2010-30847]
[[Page 80117]]
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Part II
Environmental Protection Agency
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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]]
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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.
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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 http://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 http://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:
[email protected]. 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: [email protected].
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:
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Examples of regulated
Category NAICS \a\ entities
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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.
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\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 (http://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 http://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\
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\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.
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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,
[[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 http://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 http://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 http://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 http://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 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 [micro]m 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 [micro]m 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 [micro]m in size would generate
dried particles of 2 [micro]m or less and that water droplets up to 20
[micro]m would generate dried particles up to 4 [micro]m or less.
Based on wet scrubber operation and typical mist eliminator
performance, EPA has determined that the Method 5 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 [deg]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 [deg]F
(538 [deg]C) 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. If the
[[Page 80127]]
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
[deg]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 [deg]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 are
affected by the same influences and uncertainties that make particle
sizing in stacks with entrained water droplets a challenging technical
issue. Particle-sizing 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
source-specific 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 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
[[Page 80128]]
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
[Delta]pmin and [Delta]pmax 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 [Delta]pmin and
[Delta]pmax 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 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 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 [deg]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
[[Page 80129]]
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 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[deg]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
(http://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[supreg] liner
or whether another liner is acceptable.
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 performance-based 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[supreg]'' with ``Teflon[supreg],
fluoropolymer or chemically equivalent.'' Another commenter stated that
the final method should allow for alternatives to Teflon[supreg]
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 [mu]m 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.
[[Page 80130]]
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).
5. Glassware Baking Requirements
Comment: Several commenters stated that the proposed requirement in
Section 8.4 to bake glassware at 300[deg]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[deg]C for three
hours) was sufficient to achieve the blank allowance specified in the
method. One commenter stated that, based upon their experiments, no
benefit was obtained from baking glassware. Another commenter stated
that they had conducted numerous test runs on non-combustion 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[deg]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[deg]C for three hours after cleaning
is adequate. The commenter added that the baking requirements should be
revised because high-temperature 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 time-consuming. 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
[deg]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 [deg]C for six hours versus
lower glassware preparation temperatures. Otherwise, according to the
commenter, this requirement would require the stack tester to bring to
the testing site a large amount of pre-cleaned 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 [deg]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
[[Page 80131]]
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
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[supreg] 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[supreg] 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.
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[supreg] 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[supreg] 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[supreg] 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
[[Page 80132]]
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 high-temperature 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 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 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 [mu]m 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
[[Page 80133]]
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.
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 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 performance-
based requirement limiting the residual mass contribution. The
performance based approach 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. Regarding efficiency,
the CPM filter must have an efficiency of at least 99.95 percent (<
0.05 percent penetration) on 0.3 [mu]m 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
[[Page 80134]]
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.
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
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.
0
For the reasons stated in the preamble, title 40, chapter I of the Code
of Federal Regulations is amended as follows:
PART 51--[AMENDED]
0
1. The authority citation for part 51 continues to read as follows:
Authority: 23 U.S.C. 101; 42 U.S.C 7401-7671q.
0
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 [deg]C (85
[deg]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 [deg]C (85 [deg]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 the procedures in Method 202 of appendix M to this part
for measuring condensable PM. However, if the gas filtration
temperature never exceeds 30 [deg]C (85 [deg]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 [deg]C (400
[deg]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 [deg]C (248
[deg]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 in-stack 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
[[Page 80135]]
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 [deg]C (248 [deg]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.
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 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 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 (http://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 O-ring 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 [deg]C (85 [deg]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
[[Page 80136]]
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 [deg]C (350 [deg]F)
if it is being reused. You do not have to dry new silica gel if the
indicator shows the silica 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 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 in-
stack 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 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[deg] 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 in-stack 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 cross-sectional 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
[[Page 80137]]
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[deg]. (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 [deg]C
( 50 [deg]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 Impingers (ALT-008) to estimate the moisture content. You may
use a wet bulb-dry bulb measurement or hand-held hygrometer
measurement to estimate the moisture content of sources with gas
temperatures less than 71 [deg]C (160 [deg]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 size-specific
emissions, and controlled size-specific particulate emissions.
(http://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
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 [deg]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 [Delta]H. Use Equation 11 to calculate the meter
box orifice pressure drop ([Delta]H) 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 [Delta]H to maintain the correct
constant cut diameters. Therefore, use Equation 11 to recalculate
the [Delta]H values for 50 [deg]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
[[Page 80138]]
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,
[Delta]pmin. Use Equation 23 to convert vmax
to maximum velocity pressure, [Delta]pmax.
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 [Delta]pmin
and [Delta]pmax. 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
[Delta]pmin and [Delta]pmax. 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
[Delta]pmin and [Delta]pmax.
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 [deg]C (400 [deg]F). Use cyclones with
stainless steel sealing rings for stack temperatures above 205
[deg]C (400 [deg]F) up to 260 [deg]C (500 [deg]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 [deg]C (500 [deg]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 screw-together assemblies at temperatures
up to 538 [deg]C (1,000 [deg]F). You must use ``break-away'' 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 [deg]C (1,000 [deg]F). The
method can be used at temperatures up to 1,371 [deg]C (2,500 [deg]F)
using specially constructed high-temperature stainless steel alloys
(Hastelloy or Haynes 230) with bolt-together 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
[deg]C (68 10 [deg]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 [deg]C (220
[deg]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 [deg]C (85 [deg]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 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 [deg]C, 50 [deg]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 [deg]C (50 [deg]F) of the temperature used to calculate
[Delta]H. If stack temperatures vary by more than 28 [deg]C (50
[deg]F), use the appropriate [Delta]H 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 ([Delta]pavg).
You must use the velocity pressure
[[Page 80139]]
measured during the sampling run to determine the velocity pressure
at each point ([Delta]pn). 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 ([Delta]ps2) 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 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
[deg]C (50 [deg]F) of the temperature used to calculate [Delta]H. If
stack temperatures vary by more than 28 [deg]C (50 [deg]F), use the
appropriate [Delta]H 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
[deg]C ( 18 [deg]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 [Delta]H at the value
calculated in Section 8.5.3 for the stack 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 non-representative 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
[[Page 80140]]
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 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, prepare a data summary and
compile all the calculations and raw data sheets.
9.3 Conditions. You must document data and information on the
process unit tested, the particulate control system used to control
emissions, any non-particulate control system that may affect
particulate emissions, the sampling train conditions, and weather
conditions. Discontinue the test if the operating conditions may
cause non-representative particulate emissions.
9.4 Field 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 S-type 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
[[Page 80141]]
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 http://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 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 250-ml 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/K\0.5\) = 13.4622 (micropoise/
R\0.5\)
C3 = 1.19183 x 10\6\ (micropoise/K\2\) = 3.86153 x 10\6\
(micropoise/R\2\)
C4 = 0.591123 (micropoise)
C5 = 91.9723 (micropoise)
C6 = 4.91705 x 10-5 (micropoise/K\2\) =
1.51761 x 10-5 (micropoise/R\2\)
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.
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 -[deg]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, [deg]R.
tn = Sampling time at point n, min.
tr = Total projected run time, min.
Ts = Absolute stack gas temperature, [deg]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.
[[Page 80142]]
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.
[Delta]H = Meter box orifice pressure drop, inches W.C.
[Delta]H@ = 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.)
[([Delta]p)\0.5\]avg = Average of square roots of the
velocity pressures measured during the preliminary traverse, inches
W.C.
[Delta]pm = Observed velocity pressure using S-type pitot
tube in preliminary traverse, inches W.C.
[Delta]pavg = Average velocity pressure, inches W.C.
[Delta]pmax = Maximum velocity pressure, inches W.C.
[Delta]pmin = Minimum velocity pressure, inches W.C.
[Delta]pn = Velocity pressure measured at point n during
the test run, inches W.C.
[Delta]ps = Velocity pressure calculated in Equation 25,
inches W.C.
[Delta]ps1 = Velocity pressure adjusted for combined
cyclone pitot tube, inches W.C.
[Delta]ps2 = Velocity pressure corrected for blockage,
inches W.C.
[Delta]p1 = Velocity pressure measured at point 1, inches
W.C.
[gamma] = Dry gas meter gamma value, dimensionless.
[micro] = Gas viscosity, micropoise.
[thgr] = Total run time, min.
[rho]a = 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 re-established cyclone IV
D50-1 if the Reynolds number is less than 3,162.
(b) Use Equation 38 to calculate the re-established 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 re-established
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.
[GRAPHIC] [TIFF OMITTED] TR21DE10.000
Molecular Weight of Wet Gas. Calculate the molecular weight of
the stack gas on a wet basis using Equation 2.
[GRAPHIC] [TIFF OMITTED] TR21DE10.001
Gas Stream Viscosity. Calculate the gas stream viscosity using
Equation 3. This equation uses constants for gas temperatures in
[deg]R.
[[Page 80143]]
[GRAPHIC] [TIFF OMITTED] TR21DE10.002
Cunningham Correction Factor. The Cunningham correction factor
is calculated for a 2.25 micrometer diameter particle.
[GRAPHIC] [TIFF OMITTED] TR21DE10.003
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.
[GRAPHIC] [TIFF OMITTED] TR21DE10.004
Cut Diameter for Cyclone I for the Middle of the Overlap Zone.
[GRAPHIC] [TIFF OMITTED] TR21DE10.005
Sampling Rate Using Both PM10 and PM2.5 Cyclones.
[GRAPHIC] [TIFF OMITTED] TR21DE10.006
Sampling Rate Using Only PM2.5 Cyclone.
For Nre Less than 3,162:
[GRAPHIC] [TIFF OMITTED] TR21DE10.007
For Nre greater than or equal to 3,162:
[GRAPHIC] [TIFF OMITTED] TR21DE10.008
Reynolds Number.
[GRAPHIC] [TIFF OMITTED] TR21DE10.009
Meter Box Orifice Pressure Drop.
[[Page 80144]]
[GRAPHIC] [TIFF OMITTED] TR21DE10.010
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.
[GRAPHIC] [TIFF OMITTED] TR21DE10.011
Velocity of Stack Gas. Correct the mean preliminary velocity
pressure for Cp and blockage using Equations 25, 26, and
27.
[GRAPHIC] [TIFF OMITTED] TR21DE10.012
Calculated Nozzle Diameter for Acceptable Sampling Rate.
[GRAPHIC] [TIFF OMITTED] TR21DE10.013
Velocity of Gas in Nozzle.
[GRAPHIC] [TIFF OMITTED] TR21DE10.014
Minimum Nozzle/Stack Velocity Ratio Parameter.
[GRAPHIC] [TIFF OMITTED] TR21DE10.015
Maximum Nozzle/Stack Velocity Ratio Parameter.
[GRAPHIC] [TIFF OMITTED] TR21DE10.016
Minimum Gas Velocity for Rmin Less than 0.5.
[[Page 80145]]
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Minimum Gas Velocity for Rmin Greater than or Equal to 0.5.
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Maximum Gas Velocity for Rmax Less than to 1.5.
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Maximum Gas Velocity for Rmax Greater than or Equal to 1.5.
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Minimum Velocity Pressure.
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Maximum Velocity Pressure.
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Sampling Dwell Time at Each Point. Ntp is the total
number of traverse points. You must use the preliminary velocity
traverse data.
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Adjusted Velocity Pressure.
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Average Probe Blockage Factor.
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Velocity Pressure.
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Dry Gas Volume Sampled at Standard Conditions.
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Sample Flow Rate at Standard Conditions.
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Volume of Water Vapor.
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Moisture Content of Gas Stream.
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Sampling Rate.
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(Note: The viscosity and Reynolds Number must be recalculated
using the actual stack temperature, moisture, and oxygen content.)
Actual Particle Cut Diameter for Cyclone I. This is based on
actual temperatures and pressures measured during the test run.
[GRAPHIC] [TIFF OMITTED] TR21DE10.032
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.
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[[Page 80147]]
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.
[GRAPHIC] [TIFF OMITTED] TR21DE10.034
Re-estimated Cunningham Correction Factor. You must use the
actual test run Reynolds Number (Nre) value and select
the appropriate D50 from Equation 33 or 34 (or Equation
37 or 38 if reiterating).
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Re-calculated Particle Cut Diameter for Nre Less than 3,162.
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Re-calculated Particle Cut Diameter for N Greater than or Equal
to 3,162.
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Ratio (Z) Between D50 and D50 1 Values.
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Acceptance Criteria for Z Values. The number of iterative steps
is represented by N.
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Percent Isokinetic Sampling.
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Acetone Blank Concentration.
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Acetone Blank Correction Weight.
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Acetone Blank Weight.
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Concentration of Total Filterable PM.
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Concentration of Filterable PM10.
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Concentration of Filterable PM2.5.
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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 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).
14.0 Alternative Procedures
Alternative methods for estimating the moisture content (ALT-
008) and thermocouple calibration (ALT-011) can be found at http://www.epa.gov/ttn/emc/approalt.html.
15.0 Waste Management
[Reserved]
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.
(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.
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................... 0.015 gr/DSCF.
Less than or equal to 10 and greater than 2.5 40% of total collectable PM.
micrometers.
[[Page 80149]]
<= 2.5 micrometers.............................. 20% of total collectable PM.
----------------------------------------------------------------------------------------------------------------
Table 2--Required Cyclone Cut Diameters (D50)
------------------------------------------------------------------------
Min. cut Max. cut
Cyclone diameter diameter
(micrometer) (micrometer)
------------------------------------------------------------------------
PM10 Cyclone (Cyclone I from five 9 11
stage cyclone).......................
PM2.5 Cyclone (Cyclone IV from five 2.25 2.75
stage cyclone).......................
------------------------------------------------------------------------
Table 3--Test Calculations
------------------------------------------------------------------------
If you are using . . . To calculate . . . Then use . . .
------------------------------------------------------------------------
Preliminary data............ Dry gas molecular Equation 1.
weight, Md.
Dry gas molecular weight wet gas molecular Equation 2.\a\
(Md) and preliminary weight, MW.
moisture content of the gas
stream.
Stack gas temperature, and gas viscosity, [mu]. Equation 3.
oxygen and moisture content
of the gas stream.
Gas viscosity, [mu]......... Cunningham Equation 4.
correction factor
\b\, C.
Reynolds Number \c\ (Nre)... Preliminary lower Equation 5.
Nre less than 3,162......... limit cut diameter
for cyclone I,
D50LL.
D50LL from Equation 5....... Cut diameter for Equation 6.
cyclone I for
middle of the
overlap zone, D50T.
D50T from Equation 6........ Final sampling rate Equation 7.
for cyclone I,
QI(Qs).
D50 for PM2.5 cyclone and Final sampling rate Equation 8.
Nre less than 3,162. for cyclone IV, QIV.
D50 for PM2.5 cyclone and Final sampling rate Equation 9.
Nre greater than or equal for cyclone IV, QIV.
to 3,162.
QI(Qs) from Equation 7...... Verify the assumed Equation 10.
Reynolds number,
Nre.
------------------------------------------------------------------------
\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 [deg]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--[Delta]H Values Based on Preliminary Traverse Data
----------------------------------------------------------------------------------------------------------------
Stack Temperature ([deg]R) Ts--50[deg] Ts Ts + 50[deg]
----------------------------------------------------------------------------------------------------------------
[Delta]H, (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................. Calculate [Delta]H Assume original
for the meter box. D50LL is correct
Greater than or equal to 3,162.. Recalculate D50LL Substitute the
using Equation 12. ``new'' D50LL
into Equation 6
to recalculate
D50T.
------------------------------------------------------------------------
Table 6--Calculations for Recovery of PM10 and PM2.5
------------------------------------------------------------------------
Calculations Instructions and References
------------------------------------------------------------------------
Average dry gas meter temperature...... See field test data sheet.
Average orifice pressure drop.......... See field test data sheet.
Dry gas volume (Vms)................... Use Equation 28 to correct the
sample volume measured by the
dry gas meter to standard
conditions (20 [deg]C, 760 mm
Hg or 68 [deg]F, 29.92 inches
Hg).
Dry gas sampling rate (QsST)........... Must be calculated using
Equation 29.
Volume of water condensed (Vws)........ 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.
Moisture content of gas stream (Bws)... Calculate this using Equation
31.
Sampling rate (Qs)..................... Calculate this using Equation
32.
Test condition Reynolds number\a\...... Use Equation 10 to calculate
the actual Reynolds number
during test conditions.
[[Page 80150]]
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.
Stack gas velocity (vs)................ Calculate this using Equation
13.
Percent isokinetic rate (%I)........... Calculate this using Equation
41.
------------------------------------------------------------------------
\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.
BILLING CODE 6560-50-P
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BILLING CODE 6560-50-C
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 [deg]C (85
[deg]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 the procedures in
Method 201A of appendix M to this part for measuring filterable PM.
However, if the gas filtration temperature never exceeds 30 [deg]C
(85 [deg]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 in-stack 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:
(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 [deg]C (85 [deg]F) in conjunction with this method.
However, if the gas filtration temperature never exceeds 30 [deg]C
(85 [deg]F), then use of this method is not required to measure
total primary PM.
[[Page 80161]]
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 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 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 O-ring. 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
[[Page 80162]]
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 [deg]C (350 [deg]F) if it is
being reused. You do not have to dry new silica gel if the indicator
shows the silica gel is active for moisture collection.
7.1.3 Water. Use deionized, ultra-filtered water that contains
1.0 parts per million by weight (ppmw) (1 mg/L) residual mass or
less to recover and extract samples.
7.1.4 Crushed Ice. Obtain from the best readily available
source.
7.1.5 Nitrogen Gas. Use Ultra-High Purity compressed nitrogen or
equivalent to purge the sampling train. The compressed nitrogen you
use to purge the sampling train must contain no more than 1 parts
per million by volume (ppmv) oxygen, 1 ppmv total hydrocarbons as
carbon, and 2 ppmv moisture. The compressed nitrogen must not
contribute more than 0.1 mg of residual mass per purge.
7.2 Sample Recovery and Analytical Reagents. You will need
acetone, hexane, anhydrous calcium sulfate, ammonia hydroxide, and
deionized water for the sample recovery and analysis. Unless
otherwise indicated, all reagents must conform to the specifications
established by the Committee on Analytical Reagents of the American
Chemical Society. If such specifications are not available, then use
the best available grade. Additional information on each of these
items is in the following paragraphs:
7.2.1 Acetone. Use acetone that is stored in a glass bottle. Do
not use acetone from a metal container because it normally produces
a high residual mass in the laboratory and field reagent blanks. You
must use acetone that has a blank value less than 1.0 ppmw (0.1 mg/
100 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 in-
stack 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.
(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 [deg]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 [deg]C (85 [deg]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
[deg]C (less than or equal to 85 [deg]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.)
[[Page 80163]]
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 [deg]C
(68 [deg]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 leak-check 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 leak-check of the pitot tube assembly. Follow the
procedures outlined in Section 8.4.1 of Method 5.
8.5 Sampling Train Operation. Operate the sampling train as
described in the filterable particulate sampling method (i.e.,
Method 5 of appendix A-3 to part 60, Method 17 of appendix A-6 to
part 60, or Method 201A of appendix M to this part) with the
following additions or exceptions:
8.5.1 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 [deg]C
(greater than 65 [deg]F) but less than or equal to 30 [deg]C (less
than or equal to 85 [deg]F) during sample collection. (Note:
Maintain the temperature of the CPM filter assembly as close to 30
[deg]C (85 [deg]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, 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 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 [Delta]H@ 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
[Delta]H@ 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 [deg]C (greater than 65
[deg]F), but less than or equal to 30 [deg]C (less than or equal to
85 [deg]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
[deg]C (68 [deg]F). Continue the purge under these conditions for at
least one hour, checking the rotameter and [Delta]H@ 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,
[[Page 80164]]
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, 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 [deg]C (85 [deg]F) during shipping.
9.0 Quality Control
9.1 Daily Quality Checks. You must perform daily quality checks
of field log notebooks and data entries and calculations using data
quality indicators from this method and your site-specific test
plan. You must review and evaluate recorded and transferred raw
data, calculations, and documentation of testing procedures. You
must initial or sign log notebook pages and data entry forms that
were reviewed.
9.2 Calculation Verification. Verify the calculations by
independent, manual checks. You must flag any suspect data and
identify the nature of the problem and potential effect on data
quality. After you complete the test, prepare a data summary and
compile all the calculations and raw data sheets.
9.3 Conditions. You must document data and information on the
process unit tested, the particulate control system used to control
emissions, any non-particulate control system that may affect
particulate emissions, the sampling train conditions, and weather
conditions. Discontinue the test if the operating conditions may
cause non-representative particulate emissions.
9.4 Field 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
[[Page 80165]]
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.
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) (http://www.epa.gov/ttn/emc).
Calibrate each temperature sensor at a minimum of three points over
the anticipated range of use against a NIST-traceable thermometer.
Alternatively, a reference thermocouple and potentiometer calibrated
against NIST standards can be used.
10.2 Ammonium Hydroxide. The 0.1 N NH4OH used for
titrations in this method is made as follows: Add 7 ml of
concentrated (14.8 M) NH4OH to 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 http://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 [deg]C (85 [deg]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 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 [deg]C and allow to dry at room temperature (not to
exceed 30 [deg]C (85 [deg]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. 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 [deg]C, evaporate
the aqueous phase 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 [deg]C
(85 [deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least
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 [deg]C (85 [deg]F)) and pressure in a
laboratory hood to not less than 10 ml. Quantitatively transfer the
beaker contents to a clean 50-ml pre-tared weighing tin and
evaporate to dryness at room temperature (not to exceed 30 [deg]C
(85 [deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the organic fraction for 24 hours in a
desiccator containing anhydrous calcium sulfate. Weigh at intervals
of at least 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 250-ml beaker. Evaporate
the acetone at room temperature (not to exceed 30 [deg]C (85
[deg]F)) and pressure in a laboratory hood to approximately 10 ml.
Quantitatively transfer
[[Page 80166]]
the beaker contents to a clean 50-ml pre-tared weighing tin, and
evaporate to dryness at room temperature (not to exceed 30 [deg]C
(85 [deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least
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 [deg]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 [deg]C
(85 [deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least
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 [deg]C (85 [deg]F)) and
pressure in a laboratory hood to approximately 10 ml. Quantitatively
transfer the beaker contents to a clean 50-ml pre-tared weighing tin
and evaporate to dryness at room temperature (not to exceed 30
[deg]C (85 [deg]F)) and pressure in a laboratory hood. Following
evaporation, desiccate the residue for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh at intervals of at least
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.
12.0 Calculations and Data Analysis
12.1 Nomenclature. Report results in International System of
Units (SI units) unless the regulatory authority for testing
specifies English units. The following nomenclature is used.
[Delta]H@ = Pressure drop across orifice at flow rate
of 0.75 SCFM at standard conditions, inches of water column (Note:
Specific to each orifice and meter box).
17.03 = mg/milliequivalents for ammonium ion.
ACFM = Actual cubic feet per minute.
Ccpm = Concentration of the condensable PM in the stack
gas, dry basis, corrected to standard conditions, milligrams/dry
standard cubic foot.
mc = Mass of the NH4\+\ added to sample to
form ammonium sulfate, mg.
mcpm = Mass of the total condensable PM, mg.
mfb = Mass of total CPM in field train 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.
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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.
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12.2.3 Mass of Inorganic CPM (mg).
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12.2.4 Total Mass of CPM (mg).
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12.2.5 Concentration of CPM (mg/dscf).
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12.3 Emissions Test Report. You must prepare a test report
following the guidance in EPA 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 http://www.epa.gov/ttn/emc/approalt.html.
17.0 References
(1) Commonwealth of Pennsylvania, Department of Environmental
Resources. 1960. Chapter 139, Sampling and Testing (Title 25, Rules
and Regulations, part I, Department of Environmental Resources,
Subpart C, Protection of Natural Resources, Article III, Air
Resources). January 8, 1960.
(2) DeWees, W.D. and K.C. Steinsberger. 1989. ``Method
Development and Evaluation of Draft Protocol for Measurement of
Condensable Particulate Emissions.'' Draft Report. November 17,
1989.
(3) DeWees, W.D., K.C. Steinsberger, G.M. Plummer, L.T. Lay,
G.D. McAlister, and R.T. Shigehara. 1989. ``Laboratory and Field
Evaluation of EPA Method 5 Impinger Catch for Measuring Condensable
Matter from Stationary Sources.'' Paper presented at the 1989 EPA/
AWMA International Symposium on Measurement of Toxic and Related Air
Pollutants. Raleigh, North Carolina. May 1-5, 1989.
(4) Electric Power Research Institute (EPRI). 2008. ``Laboratory
Comparison of Methods to Sample and Analyze Condensable PM.'' EPRI
Agreement EP-P24373/C11811 Condensable Particulate Methods: EPRI
Collaboration with EPA, October 2008.
(5) Nothstein, Greg. Masters Thesis. University of Washington.
Department of Environmental Health. Seattle, Washington.
(6) Richards, J., T. Holder, and D. Goshaw. 2005. ``Optimized
Method 202 Sampling Train to Minimize the Biases Associated with
Method 202 Measurement of Condensable PM Emissions.'' Paper
presented at Air & Waste Management Association Hazardous Waste
Combustion Specialty Conference. St. Louis, Missouri. November 2-3,
2005.
(7) Texas Air Control Board, Laboratory Division. 1976.
``Determination of Particulate in Stack Gases Containing Sulfuric
Acid and/or Sulfur Dioxide.'' Laboratory Methods for Determination
of Air Pollutants. Modified December 3, 1976.
(8) Puget Sound Air Pollution Control Agency, Engineering
Division. 1983. ``Particulate Source Test Procedures Adopted by
Puget Sound Air Pollution Control Agency Board of Directors.''
Seattle, Washington. August 11, 1983.
(9) U.S. Environmental Protection Agency, Federal Reference
Methods 1 through 5 and Method 17, 40 CFR 60, appendix A-1 through
A-3 and A-6.
(10) U.S. Environmental Protection Agency. 2008. ``Evaluation
and Improvement of Condensable PM Measurement,'' EPA Contract No.
EP-D-07-097, Work Assignment 2-03, October 2008.
(11) U.S. Environmental Protection Agency. 2005. ``Laboratory
Evaluation of Method 202 to Determine Fate of SO2 in
Impinger Water,'' EPA Contract No. 68-D-02-061, Work Assignment 3-
14, September 30, 2005.
(12) U.S. Environmental Protection Agency. 2010. Field valuation
of an Improved Method for Sampling and Analysis of Filterable and
Condensable Particulate Matter. Office of Air Quality Planning and
Standards, Sector Policy and Program Division Monitoring Policy
Group. Research Triangle Park, NC 27711.
(13) Wisconsin Department of Natural Resources. 1988. Air
Management Operations Handbook, Revision 3. January 11, 1988.
18.0 Tables, Diagrams, Flowcharts, and Validation Data
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Figure 4--Field Train Recovery Blank Condensable Particulate
Calculations
------------------------------------------------------------------------
------------------------------------------------------------------------
Field Train Recovery Blank Condensable Particulate Calculations
------------------------------------------------------------------------
Plant .......................
------------------------------------------------------------------------
Date .......................
------------------------------------------------------------------------
Blank No. .......................
------------------------------------------------------------------------
CPM Filter No. .......................
------------------------------------------------------------------------
[[Page 80171]]
Water volume added to purge train (Vp)......... ml
------------------------------------------------------------------------
Field Reagent Blank Mass\a\ .......................
------------------------------------------------------------------------
Water (Section 11.2.7)......................... mg
------------------------------------------------------------------------
Acetone (Section 11.2.6)....................... mg
------------------------------------------------------------------------
Hexane (Section 11.2.8)........................ mg
------------------------------------------------------------------------
Field Train Recovery Blank Mass .......................
------------------------------------------------------------------------
Mass of Organic CPM (mob) (Section 11.2.3)..... mg
------------------------------------------------------------------------
Mass of Inorganic CPM (mib) (Equation 3)....... mg
------------------------------------------------------------------------
Mass of the Field Train Recovery Blank (not to mg
exceed 2.0 mg) (Equation 2).
------------------------------------------------------------------------
\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.
Figure 5--Other Field Train Sample Condensable Particulate Data
------------------------------------------------------------------------
------------------------------------------------------------------------
Other Field Train Sample Condensable Particulate Data
------------------------------------------------------------------------
Plant .......................
------------------------------------------------------------------------
Date .......................
------------------------------------------------------------------------
Run No. .......................
------------------------------------------------------------------------
CPM Filter No. .......................
------------------------------------------------------------------------
Water volume added to purge train (max 50 ml) ml
(Vp).
------------------------------------------------------------------------
Date .......................
------------------------------------------------------------------------
Run No. .......................
------------------------------------------------------------------------
CPM Filter No. .......................
------------------------------------------------------------------------
Water volume added to purge train (max 50 ml) ml
(Vp).
------------------------------------------------------------------------
Date .......................
------------------------------------------------------------------------
Run No. .......................
------------------------------------------------------------------------
CPM Filter No. .......................
------------------------------------------------------------------------
Water volume added to purge train (max 50 ml) ml
(Vp).
------------------------------------------------------------------------
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 .................. ml
transport
Plant
------------------------------------------------------------------------
Date
------------------------------------------------------------------------
Run No.
------------------------------------------------------------------------
Was significant volume of organic ..................
rinse lost during transport? Yes or
No
------------------------------------------------------------------------
If Yes, measure the volume received ..................
Estimate the volume lost during .................. ml
transport.
For Titration:
Normality of NH4OH (N) (Section .................. N
10.2)
Volume of titrant (Vt) (Section .................. ml
11.2.2.2)
Mass of NH4 added (mc) (Equation 1) .................. mg
For CPM Blank Weights:
Inorganic Field Train Recovery Blank .................. mg
Mass(mib) (Section 9.9)
Organic Field Train Recovery Blank .................. mg
Mass (mob) (Section 9.9)
Mass of Field Train Recovery Blank .................. mg
(Mfb) (max. 2 mg) (Equation 2)
For CPM Train Weights:
Mass of Organic CPM (mo) (Section .................. mg
11.2.3)
Mass of Inorganic CPM (mi) (Equation .................. mg
3)
Total CPM Mass (mcpm) (Equation 4) .................. mg
------------------------------------------------------------------------
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[FR Doc. 2010-30847 Filed 12-20-10; 8:45 am]
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