[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:

------------------------------------------------------------------------
                                                   Examples of regulated
           Category                 NAICS \a\             entities
------------------------------------------------------------------------
Industry......................  332410...........  Fossil fuel steam
                                                    generators.
                                332410...........  Industrial,
                                                    commercial,
                                                    institutional steam
                                                    generating units.
                                332410...........  Electricity
                                                    generating units.
                                324110...........  Petroleum refineries.
                                562213...........  Municipal waste
                                                    combustors.
                                322110...........  Pulp and paper mills.
                                325188...........  Sulfuric acid plants.
                                327310...........  Portland cement
                                                    plants.
                                327410...........  Lime manufacturing
                                                    plants.
                                211111, 212111,    Coal preparation
                                 212112, 212113.    plants.
                                331312, 331314...  Primary and secondary
                                                    aluminum plants.
                                331111, 331513...  Iron and steel
                                                    plants.
                                321219, 321211,    Plywood and
                                 321212.            reconstituted
                                                    products plants.
------------------------------------------------------------------------
\a\ North American Industrial Classification System.

B. Where can I obtain a copy of this action and other related 
information?

    In addition to being available in the docket, an electronic copy of 
these final rules are also available on the World Wide Web (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.
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    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.

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    Minimum Gas Velocity for Rmin Greater than or Equal to 0.5.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.018
    
    Maximum Gas Velocity for Rmax Less than to 1.5.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.019
    
    Maximum Gas Velocity for Rmax Greater than or Equal to 1.5.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.020
    
    Minimum Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.021
    
    Maximum Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.022
    
    Sampling Dwell Time at Each Point. Ntp is the total 
number of traverse points. You must use the preliminary velocity 
traverse data.
[GRAPHIC] [TIFF OMITTED] TR21DE10.023

    Adjusted Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.024
    
    Average Probe Blockage Factor.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.025
    

[[Page 80146]]


    Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.026
    
    Dry Gas Volume Sampled at Standard Conditions.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.027
    
    Sample Flow Rate at Standard Conditions.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.028
    
    Volume of Water Vapor.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.029
    
    Moisture Content of Gas Stream.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.030
    
    Sampling Rate.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.031
    
    (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.
[GRAPHIC] [TIFF OMITTED] TR21DE10.033


[[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).
[GRAPHIC] [TIFF OMITTED] TR21DE10.035

    Re-calculated Particle Cut Diameter for Nre Less than 3,162.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.036
    
    Re-calculated Particle Cut Diameter for N Greater than or Equal 
to 3,162.
[GRAPHIC] [TIFF OMITTED] TR21DE10.037

    Ratio (Z) Between D50 and D50	1 Values.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.038
    
    Acceptance Criteria for Z Values. The number of iterative steps 
is represented by N.
[GRAPHIC] [TIFF OMITTED] TR21DE10.039

    Percent Isokinetic Sampling.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.040
    
    Acetone Blank Concentration.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.041
    

[[Page 80148]]


    Acetone Blank Correction Weight.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.042
    
    Acetone Blank Weight.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.043
    
    Concentration of Total Filterable PM.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.044
    
    Concentration of Filterable PM10.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.045
    
    Concentration of Filterable PM2.5.
    [GRAPHIC] [TIFF OMITTED] TR21DE10.046
    
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).
    [GRAPHIC] [TIFF OMITTED] TR21DE10.062
    
    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]
BILLING CODE 6560-50-C