[Federal Register Volume 74, Number 56 (Wednesday, March 25, 2009)]
[Proposed Rules]
[Pages 12970-13012]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: E9-6178]



[[Page 12969]]

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Part III





Environmental Protection Agency





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40 CFR Part 51



Methods for Measurement of Filterable PM<INF>10</INF> and 
PM<INF>2.5</INF> and Measurement of Condensable Particulate Matter 
Emissions from Stationary Sources; Proposed Rule

Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / 
Proposed Rules

[[Page 12970]]


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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 51

[EPA-HQ-OAR-2008-0348; FRL-8784-5]
RIN 2060-AO58


Methods for Measurement of Filterable PM<INF>10</INF> and 
PM<INF>2.5</INF> and Measurement of Condensable Particulate Matter 
Emissions From Stationary Sources

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule.

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SUMMARY: This action proposes amendments to Methods 201A and 202. The 
proposed amendments to Method 201A would add a particle-sizing device 
to allow for sampling of particulate matter (PM) with mean aerodynamic 
diameters less than or equal to 2.5 micrometers ([mu]m) 
(PM<INF>2.5</INF> or fine PM). The proposed amendments to Method 202 
would 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 (CPM). 
Additionally, the proposed amendments to Method 202 would 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. Finally, in this notice we are 
soliciting comments on whether to end the transition period for CPM in 
the New Source Review (NSR) program on a date earlier than the current 
end date of January 1, 2011. The proposed amendments would improve the 
measurement of fine particulates and would help State and local 
agencies in implementing CPM control measures to attain the 
PM<INF>2.5</INF> National Ambient Air Quality Standards (NAAQS) which 
were established to protect public health and welfare.

DATES: Comments. Comments must be received on or before May 26, 2009.

ADDRESSES: Submit your comments, identified by Docket ID Number EPA-HQ-
OAR-2008-0348, by one of the following methods:
    <bullet> http://www.regulations.gov. Follow the on-line 
instructions for submitting comments.
    <bullet> E-mail: Send your comments via electronic mail to <a href="/cdn-cgi/l/email-protection#a7c68ac6c9c38ad58ac3c8c4ccc2d3e7c2d7c689c0c8d1"><span class="__cf_email__" data-cfemail="c6a7eba7a8a2ebb4eba2a9a5ada3b286a3b6a7e8a1a9b0">[email protected]</span></a>.
    <bullet> Fax: (202) 566-9744.
    <bullet> Mail: Methods for Measurement of Filterable 
PM<INF>10</INF> and PM<INF>2.5</INF> and Measurement of Condensable 
Particulate Matter Emissions from Stationary Sources, Environmental 
Protection Agency, Mailcode 2822T, 1200 Pennsylvania Ave., NW., 
Washington, DC 20460. Please include a total of two copies.
    <bullet> Hand Delivery: EPA Docket Center EPA Headquarter Library, 
Room 3334, EPA West Building, 1301 Constitution Ave., NW., Washington, 
DC, 20460. Such deliveries are accepted only during the Docket's normal 
hours of operation, and special arrangements should be made for 
deliveries of boxed information.
    Instructions: Direct your comments to Docket ID No. EPA-HQ-OAR-
2008-0348. EPA's policy is that all comments received will be included 
in the public docket without change and may be made available online at 
http://www.regulations.gov, including any personal information 
provided, unless the comment includes information claimed to be 
Confidential Business Information (CBI) or other information whose 
disclosure is restricted by statute. Do not submit information that you 
consider to be CBI or otherwise protected through http://www.regulations.gov or e-mail. The http://www.regulation.gov Web site 
is an ``anonymous access'' system, which means EPA will not know your 
identity or contact information unless you provide it in the body of 
your comment. If you send an e-mail comment directly to EPA without 
going through http://www.regulations.gov, your e-mail address will be 
automatically captured and included as part of the comment that is 
placed in the public docket and made available on the Internet. If you 
submit an electronic comment, EPA recommends that you include your name 
and other contact information in the body of your comment and with any 
disk or CD-ROM you submit. If EPA cannot read your comment due to 
technical difficulties and cannot contact you for clarification, EPA 
may not be able to consider your comment. Electronic files should avoid 
the use of special characters, any form of encryption, and be free of 
any defects or viruses. For additional information about EPA's public 
docket, visit the EPA Docket Center homepage at http://www.epa.gov/epahome/dockets.htm.
    Docket: All documents in the docket are listed in the http://www.regulations.gov index. Although listed in the index, some 
information is not publicly available, e.g. , CBI or other information 
whose disclosure is restricted by statute. Certain other material, such 
as copyrighted material, will be publicly available only in hard copy. 
Publicly available docket materials are available either electronically 
in http://www.regulations.gov or in hard copy at the Methods for 
Measurement of Filterable PM<INF>10</INF> and PM<INF>2.5</INF> and 
Measurement of Condensable Particulate Matter Emissions from Stationary 
Sources Docket, EPA/DC, EPA West Building, Room 3334, 1301 Constitution 
Ave., NW., Washington, DC. The Public Reading Room/Docket Center 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.
    Public Hearing: If anyone contacts EPA requesting to speak at a 
public hearing concerning our proposal to revise the PM test methods by 
April 14, 2009, we will hold a public hearing on or about April 24, 
2009. Persons interested in presenting oral testimony should contact 
Ms. Kristal Mozingo, Measurement Policy Group (D243-05), Sector 
Policies and Programs Division, EPA, Research Triangle Park, NC 27711, 
telephone number: (919) 541-9767, e-mail address: 
<a href="/cdn-cgi/l/email-protection#036e6c796a6d646c2d68716a7077626f436673622d646c75"><span class="__cf_email__" data-cfemail="adc0c2d7c4c3cac283c6dfc4ded9ccc1edc8ddcc83cac2db">[email protected]</span></a>. Persons interested in attending the public 
hearing should also call Ms. Mozingo to verify the time, date, and 
location of the hearing. A public hearing will provide interested 
parties the opportunity to present data, views, or arguments concerning 
the proposed test method revisions.
    If a public hearing is held, it will be held at 10 a.m. at the 
Conference Facilities at EPA's Main Campus, Research Triangle Park, NC, 
or an alternate site nearby.

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: 
<a href="/cdn-cgi/l/email-protection#9ceff3eeeef9f0f0b2fffdf2f8fdfff9dcf9ecfdb2fbf3ea"><span class="__cf_email__" data-cfemail="92e1fde0e0f7fefebcf1f3fcf6f3f1f7d2f7e2f3bcf5fde4">[email protected]</span></a>. 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: <a href="/cdn-cgi/l/email-protection#91fce8f4e3e2bfe3feffd1f4e1f0bff6fee7"><span class="__cf_email__" data-cfemail="dab7a3bfa8a9f4a8b5b49abfaabbf4bdb5ac">[email protected]</span></a>.

SUPPLEMENTARY INFORMATION:

[[Page 12971]]

I. General Information

A. Does This Action Apply to Me?

    This action would apply to you if you operate a stationary source 
that is subject to applicable requirements for total PM or total 
PM<INF>10</INF> where EPA Method 202 is incorporated as a component of 
the applicable compliance method.
    In addition, this action would apply to you if Federal, State, or 
local agencies take certain additional independent actions. For 
example, this action would apply to sources through actions by State 
and local agencies which implement CPM control measures to attain the 
PM<INF>2.5</INF> NAAQS and specify the use of this test method to 
demonstrate compliance with the control measure. Actions that State and 
local agencies would have to implement include: (1) Adopting this 
method in rules or permits (either by incorporation by reference or by 
duplicating the method in its entirety), and (2) promulgating an 
emissions limit requiring the use of this method (or an incorporated 
method based upon this method). This action would also apply 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, which 
specify the use of this test method to demonstrate compliance with the 
control measure.
    The source categories and entities potentially affected include, 
but are not limited to, the following:

------------------------------------------------------------------------
                                                          Examples of
            Category              SIC \1\  NAICS \2\      potentially
                                    code      code    regulated entities
------------------------------------------------------------------------
Industry........................     3569     332410  Fossil fuel steam
                                                       generators.
                                     3569     332410  Industrial,
                                                       commercial,
                                                       institutional
                                                       steam generating
                                                       units.
                                     3569     332410  Electricity
                                                       generating units.
                                     2911     324110  Petroleum
                                                       refineries.
                                     4953     562213  Municipal waste
                                                       combustors.
                                     2621     322110  Pulp and paper
                                                       mills.
                                     2819     325188  Sulfuric acid
                                                       plants.
                                     3241     327310  Portland Cement
                                                       Plants.
                                     3274     327410  Lime Manufacturing
                                                       Plants.
                                     1222     211111  Coal Preparation
                                                       Plants.
                                     1231     212111
                                              212112
                                              212113
                                     3334     331312  Primary and
                                                       Secondary
                                                       Aluminum Plants.
                                     3341     331314
                                     3312     331111  Iron and Steel
                                                       Plants.
                                     3325     331513
                                     2493     321219  Plywood and
                                                       Reconstituted
                                                       Products Plants.
                                     2435     321211
                                     2436     321212
------------------------------------------------------------------------
\1\ Standard Industrial Classification.
\2\ North American Industrial Classification System.

B. What Should I Consider as I Prepare My Comments for EPA?

    Do not submit information containing CBI to EPA through http://www.regulations.gov or e-mail. Send or deliver information identified 
as CBI only to the following address: Roberto Morales, OAQPS Document 
Control Officer (C404-02), U.S. EPA, Office of Air Quality Planning and 
Standards, Research Triangle Park, NC 27711, Attention Docket ID No. 
EPA-HQ-OAR-2008-0348. Clearly mark the part or all of the information 
that you claim to be CBI. For CBI information on a disk or CD-ROM that 
you mail to EPA, mark the outside of the disk or CD-ROM as CBI, and 
then identify electronically within the disk or CD-ROM the specific 
information that is claimed as CBI. In addition to one complete version 
of the comment that includes information claimed as CBI, a copy of the 
comment that does not contain the information claimed as CBI must be 
submitted for inclusion in the public docket. Information so marked 
will not be disclosed except in accordance with procedures set forth in 
40 CFR part 2.

C. 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 
today's proposed amendments is also available on the Worldwide Web 
(http://www.epa.gov/ttn/) through the Technology Transfer Network 
(TTN). Following the Administrator's signature, a copy of the proposed 
amendment 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.

D. How Is This Document Organized?

    The information in this preamble is organized as follows:

I. General Information
    A. Does This Action Apply to Me?
    B. What Should I Consider as I Prepare My Comments for EPA?
C. Where Can I Obtain a Copy of This Action and Other Related 
Information?
D. How Is This Document Organized?
II. Background
    A. Why Is EPA Issuing This Proposed Rule?
    B. Particulate Matter National Ambient Air Quality Standards
    C. Measuring PM Emissions
    1. Method 201A
    2. Method 202
III. This Action
    A. What Are the Proposed Amendments to Method 201A?
    B. What Are the Proposed Amendments to Method 202?
    C. How Will the Proposed Amendments to Methods 201A and 202 
Affect Existing Emission Inventories, Emission Standards, and Permit 
Programs?
    D. Request for Comments
    1. Items Associated With Both Test Methods
    2. Items Associated With Method 201A
    2. Items Associated With Method 202
IV. 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

[[Page 12972]]

    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

II. Background

A. Why Is EPA Issuing This Proposed Rule?

    On April 25, 2007 (70 FR 20586), we promulgated the Clean Air Fine 
Particle Implementation Rule regarding the Clean Air Act (CAA) 
requirements for State and Tribal plans to implement the 1997 PM2.5 
NAAQS. These rules require that each State having a PM2.5 nonattainment 
area must submit, by April 5, 2008, an attainment demonstration and 
adopt regulations to ensure the area will attain the standards as 
expeditiously as practicable, but even those areas for which the 
Administrator determines an extension from the 2010 attainment date is 
appropriate may not receive an extension later than a 2015 attainment 
date. The emissions inventories and analyses used in the attainment 
demonstrations must consider filterable and condensable fractions of 
PM2.5 emissions from stationary sources that are significant 
contributors of direct PM2.5 emissions. Direct PM2.5 emissions means 
the solid particles or liquid droplets emitted directly from an air 
emissions source or activity, or the gaseous emissions or liquid 
droplets from an air emissions source or activity that condense to form 
PM or liquid droplets at ambient temperatures.
    The preamble to the April 25, 2007, rule acknowledged that there 
remain questions whether the available test methods provide the most 
accurate representation of primary PM emissions even though some States 
have established emissions limits for CPM. As a result, the final rule 
established a transitional period for developing emissions limits and 
regulations for condensable PM2.5. During this transitional period, EPA 
has committed to devote resources to assessing and improving the 
available test methods for CPM.
    In response to this commitment and to address the need for improved 
measurement of fine PM, EPA is proposing amendments to the following 
test methods in 40 CFR Part 51, Appendix M (Recommended Test Methods 
for State Implementation Plans (SIPs)):
    <bullet> Method 201A--Determination of PM10 Emissions (Constant 
Sampling Rate Procedure), and
    <bullet> Method 202--Determination of Condensable Particulate 
Emissions from Stationary Sources.
    These amendments to Method 201A add a particle-sizing device to 
allow for sampling of PM2.5, PM10, or both PM10 and PM2.5. With regard 
to Method 202, we are aware that the method and the various hardware 
and analytic options described therein are sometimes applied 
inappropriately, which can lead to inaccurate and imprecise CPM 
measurements. We are also aware that Method 202 can produce inaccurate 
CPM measurements when sampling certain types of emissions sources, due 
to formation of reaction artifacts. The amendments to Method 202 revise 
the sample collection and recovery procedures of the method to provide 
for more accurate and precise measurement of CPM.

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 (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 (42 U.S.C. 7409) directs 
the Administrator to propose and promulgate primary and secondary NAAQS 
for pollutants listed under section 108 to protect public health and 
welfare, respectively. Section 109 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 (CASAC).
    Initially EPA established the NAAQS for PM 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 NAAQS for PM, 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 NAAQS for PM, 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. The 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, 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

[[Page 12973]]

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 NAAQS for PM (62 FR 55201), 
including the 1997 PM2.5 standards and the 1987 PM10 standards. On 
October 17, 2006, EPA issued its final decisions to revise the primary 
and secondary NAAQS for PM 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 that 
State and local air pollution control agencies develop and submit plans 
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. These plans are known as SIPs. 40 CFR part 
51 (Requirements for Preparation, Adoption, and Submittal of 
Implementation Plans) specifies the requirements for SIPs. 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 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 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:
    <bullet> Method 201A--Determination of PM10 Emissions (Constant 
Sampling Rate Procedure), and
    <bullet> Method 202--Determination of Condensable Particulate 
Emissions from Stationary Sources.
1. Method 201A
    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 which 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. 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 the total PM10 mass. To 
measure PM10 in stacks where water droplets are known to exist, EPA's 
Technical Information Document (TID) 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
    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, 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, and the method has been 
used successfully in regulatory programs where the emission limits and 
compliance demonstrations are established based on a consistent 
application of Method 202 and its associated options. However, when the 
same emission source is tested using different combinations of the 
optional procedures, there may appear 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. As we have 
maintained consistently, 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 SO<INF>2</INF> 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 have 
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 the EPA Method 5 Impinger Catch 
for Measuring Condensible Matter from Stationary Sources'' at the 
following Internet address: http://www.epa.gov/ttn/emc/methods/m202doc1.pdf. Essentially, the 1998 study verified the need for a 
nitrogen purge when SO2 is

[[Page 12974]]

present in stack gas and also provided guidance for analyzing the 
collected samples. In 2005, an EPA contractor conducted a second study 
(``Laboratory Evaluation of Method 202 to Determine Fate of 
SO<INF>2</INF> in Impinger Water'') that replicated some of the earlier 
EPA work and addressed some additional issues. The report of that work 
is available at the following Internet address: 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, 
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 (which is available at 
the following Internet address: 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 have held two workshops in Research Triangle 
Park, North Carolina. These meetings were held to present and seek 
comments on our plan for evaluating potential modifications to Method 
202 that would reduce artifact formation. Also, these meetings were 
held to discuss our progress in characterizing the performance of the 
modified method, issues that require additional investigation, the 
results of our laboratory studies, and our commitments to extend the 
investigation through stakeholders external to EPA. We held another 
meeting 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 the following 
Internet address: 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, propose 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 PM<INF>2.5</INF> as an indicator of health and welfare 
effects by the 1997 NAAQS revisions generates the need to quantify 
PM<INF>2.5</INF> emissions from stationary sources. To respond to this 
need, we are proposing revisions to incorporate this capability into 
the test method for filterable PM<INF>10</INF>.

III. This Action

    This action proposes to provide the capability of measuring 
PM<INF>2.5</INF> using Method 201A and to provide for more accurate 
measurement of the filterable and condensable components of fine PM 
(particles with mean aerodynamic diameters less than or equal to 2.5 m) 
and coarse PM (particles with mean aerodynamic diameters less than or 
equal to 10 m) when using Method 202. Method 201A proposed amendments 
would add a particle-sizing cyclone to the sampling train. Method 202 
proposed amendments would reduce the formation of sulfuric acid 
artifact by at least an additional 90 percent (compared to our 
recommended procedures for the existing Method 202), provide for 
greater consistency between testing contractors in method application, 
improve the precision of the method, and provide for more accurate 
quantification of direct (i.e., primary) PM emissions to the ambient 
air (the method will not measure secondarily-formed PM). The proposed 
amendments would also affect the measurement of total PM, 
PM<INF>10</INF>, and PM<INF>2.5</INF>. Additionally, we are proposing 
to revise the format of Methods 201A and 202 to be consistent with the 
format developed by EPA's Environmental Monitoring Management Council 
(EMMC). A guidance document describing the EMMC format can be found at 
the following Internet address: http://www.epa.gov/ttn/emc/guidlnd/gd-045.pdf.

A. What Are the Proposed Amendments to Method 201A?

    On July 18, 1997 (62 FR 38652), we revised the NAAQS for PM to add 
new standards for fine particles, using PM<INF>2.5</INF> as the 
indicator. This action will modify the current Method 201A sampling 
train configuration to allow for measurement of filterable 
PM<INF>10</INF>, filterable PM<INF>2.5</INF>, or both filterable 
PM<INF>10</INF> and filterable PM<INF>2.5</INF> from stationary 
sources. These amendments combine the existing method with the 
PM<INF>2.5</INF> cyclone to create a sampling train that includes a 
total of two cyclones (one cyclone to size particles with aerodynamic 
diameters greater than 10 m and one cyclone to size particles with 
aerodynamic diameters greater than 2.5 m) and a final filter to collect 
particles with aerodynamic diameters less than or equal to 2.5 m. The 
PM<INF>2.5</INF> cyclone would be inserted between the PM<INF>10</INF> 
cyclone and the filter of the Method 201A sampling train.
    We are not proposing any amendments to address the use of this 
method when the stack gas has entrained moisture or when the method is 
used for stack gases with high temperatures. In July 1979, we published 
a research document (EPA-600/7-79-166) to report the preliminary 
development of a method for measuring and characterizing the particles 
in the vent stream from a wet scrubber used to control sulfur oxide 
emissions. The method was based on the use of a heated, electrified 
wire placed in the vent stream. When a water droplet impacted the wire, 
the electric current flowing through the wire was attenuated in 
proportion to the size of the water droplet. We decided it was not 
appropriate to promulgate the preliminary method and, at this time, we 
are not aware of any commercially-available equipment that can 
determine the aerodynamic size of PM contained in, or dissolved in, 
liquid water droplets as they would exist in the ambient air following 
release and evaporation in the ambient air. While we are aware of 
several optical aerosol droplet spectrometers for measuring the size 
distribution of liquid droplets in exhaust gases, we are not aware of 
any commercial instruments that can measure size distributions of 
particles emitted from stationary sources. We also lack knowledge on 
the relative effects of solids concentration in the liquid droplets and 
the possible presence of dry particles in addition to the liquid 
droplets. Consequently, we recommend the use of EPA Method 5 (40 CFR 
Part 60, Appendix A-3--Determination of Particulate Matter Emissions 
from Stationary Sources) when measuring PM in stacks with saturated 
water vapors containing entrained water droplets. With this application 
of EPA Method 5,

[[Page 12975]]

all of the collected material would be considered PM<INF>2.5</INF>.

B. What Are the Proposed Amendments to Method 202?

    This action proposes amendments incorporating modifications that 
would reduce the formation of artifacts at both low and high 
concentrations of SO<INF>2</INF> in the sample gas stream. The 
modifications were developed based on the method evaluations discussed 
in Section II.C.2 of this preamble.
    Method 202, as promulgated in 1991, is a set of sampling procedures 
for collecting PM in water-filled impingers and a set of sample 
recovery procedures that are performed on the water following its 
collection. The water-filled impingers are nearly identical to the four 
chilled impingers used in standard stationary source sampling trains 
for PM (e.g., Method 5 and Method 17 of Appendix A-3 and A-6, 40 CFR 
Part 60). In principle, CPM is collected in the impinger portion of a 
Method 17-type sampling train. Our preferred operation of the 
promulgated method requires that the impinger contents be purged with 
nitrogen after the test run to remove dissolved SO<INF>2</INF> gas from 
the impinger contents. The impinger solution is then extracted with 
methylene chloride to separate the organic CPM from the inorganic CPM. 
The organic and aqueous fractions are then dried and the residues 
weighed. The sum of both fractions represents the total CPM.
    These proposed amendments to Method 202 sampling train and sample 
recovery procedures would achieve at least an additional 90 percent 
reduction in sulfuric acid artifact formation compared to the current 
Method 202 using the nitrogen purge option, provide testing contractors 
with a more standardized application of the method, improve the 
precision of the method, and quantify more accurately direct PM 
emission to the ambient air.
    The proposed changes to the sampling train of this method include:
    <bullet> Installing a condenser between the filter in the front-
half of the sample train and the first impinger to cool the sample 
gases to ambient temperature (less than 30 [deg]C);
    <bullet> Installing a recirculation pump in the ambient water bath 
to supply cooling water to the condenser;
    <bullet> Changing the first two impingers from wet to dry, and 
placing these two dry impingers in a water bath at ambient temperature 
(less than 30 [deg]C) (the first dry impinger will use a short-stem 
insert, and the second dry impinger will use a long-stem insert);
    <bullet> Requiring the use of an out-of-stack, low-temperature 
filter (i.e., the CPM filter), as described in EPA Method 8, between 
the second and third impingers (a Teflon filter is used in place of the 
fiberglass filter described in EPA Method 8); and
    <bullet> Requiring that the temperature of the sample gas drawn 
through the CPM filter be maintained at ambient temperature (less than 
30 [deg]C).

It should be noted that under Method 202, the use of a CPM filter is an 
optional procedure that is used typically if the collection efficiency 
of the impinger is suspected to be low. These proposed amendments would 
make the use of a CPM filter a required procedure.
    The proposed changes to Method 202 include:
    <bullet> Extracting the CPM filter with water and organic solvent;
    <bullet> Evaporating the liquid collected in the impingers in an 
oven or on a hot plate down to a minimum volume of 10 milliliters, 
instead of all the way to dryness;
    <bullet> Evaporating the remaining liquid to dryness at ambient 
temperature prior to neutralization with ammonium hydroxide;
    <bullet> Titrating the reconstituted residue with 0.1 normal 
ammonium hydroxide and a pH meter;
    <bullet> Evaporating the neutralized liquid to a minimum volume of 
10 milliliters in an oven or hot plate;
    <bullet> Evaporating the final volume to dryness at ambient 
temperature; and
    <bullet> Weighing the CPM sample residue to constant weight after 
allowing a minimum of 24 hours for equilibration in a desiccator.

Note that the requirements to evaporate liquids at ambient temperature 
and to titrate the reconstituted liquid exist already as options under 
this method. These optional steps are typically performed to retain CPM 
that might be lost at higher evaporation temperatures. Under these 
proposed amendments, these options would be required procedures.

C. How Will the Proposed 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 
proposed 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. If implemented, the proposed test method 
revisions would have the potential to 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 proposed 
method would likely 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 proposed 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 proposed revision 
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 PM<INF>2.5</INF> 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 to demonstrate facility 
compliance.
    These amendments would serve to mitigate the potential difficulties 
that can arise when we and other regulatory entities attempt to use the 
test data from State and local agencies whose CPM test methods are 
inconsistent 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

[[Page 12976]]

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 SO<INF>2</INF> to sulfates (or 
SO<INF>3</INF>) 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 
PM<INF>10</INF> 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 PM<INF>2.5</INF> will 
result in greater inaccuracies.
    With regard to State permitting programs, we recognize that, in 
some cases, existing Best Available Control Technology (BACT), Lowest 
Achievable Emission Rate (LAER), or Reasonably Available Control 
Technology (RACT) limits have been based on an identified control 
technology, and that the data used to determine the performance of that 
technology and 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 
which 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, once emissions limits are established as CAA requirements 
under the SIP or a SIP-approved pre-construction review permit, they 
are included in the Title V permits. Obviously, Title V permits may 
have to 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 the previously 
promulgated test methods, it is not a given that the permit would 
always have to be revised should these test methods 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 in the permitting 
context due to these proposed changes to the test methods would be 
controlled by several factors, such as the exact wording of the 
existing operating permit, the requirements of the EPA-approved SIP, 
and any changes that may be made to pre-construction review permits 
with respect to a particular source test method that did not include 
CPM or on a set of procedures in Method 202 which underestimated 
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 
PM<INF>2.5</INF> that are needed to demonstrate attainment of the 
PM<INF>2.5</INF> NAAQS. As discussed in the April 25, 2007, Clean Air 
Fine Particle Implementation Rule (72 FR 20586) and in the May 16, 
2008, promulgation of the New Source Review Program Implementation for 
fine particulate matter (73 FR 28321), the transition period, which 
ends January 1, 2011, allows time to resolve and adopt appropriate 
testing procedures for CPM emissions and to collect total primary 
(filterable and condensable) PM<INF>2.5</INF> emissions data that are 
more representative of the emissions of each source in their areas. In 
the PM<INF>2.5</INF> 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.'' See 73 FR at 28344. Accordingly, we are 
hereby soliciting comments on ending the NSR transition period for CPM 
on a date 60 to 90 days after the promulgation date of this test 
methods rulemaking.
    During the transition period, we are available to provide technical 
support to States, as requested, in establishing emissions testing 
requirements. We will also solicit the involvement of interested 
stakeholders to collect new direct filterable and CPM emissions data 
using methodologies that provide more representative data of a source's 
direct PM<INF>2.5</INF> emissions. These data will be used by us, 
States, and others to improve emissions factors and to help establish 
or revise source emissions limits in implementation plans. The 
transition period will also provide time for additional method 
evaluations. During the transition period, we expect that some States 
will continue to develop more complete inventories of direct 
PM<INF>2.5</INF> emissions, particularly for CPM. As needed to 
demonstrate attainment of the PM NAAQS, we also expect States to 
address the control of direct PM<INF>2.5</INF> emissions, including 
CPM, with any new actions taken after January 1, 2011 and to address 
CPM emissions in any direct PM<INF>2.5</INF> regulations or limits 
developed under any new PM NAAQS.
    As with other methods, any new procedures approved by us will 
produce data that will be incorporated into the tools (e.g., emission 
factors, emission inventories, air quality modeling) used to assess the 
attainment of air quality standards. However, we do not believe that it 
is necessary to update continually the assessment tools or revise 
previous air quality analyses until evidence is presented that a mid-
course corrective action is needed to achieve the air quality standards 
(a mid-course review is required by April 2011 for each area with an 
approved attainment date in 2014 or 2015). At that time, updated 
inventories and air quality models may be needed to identify and 
characterize the emission sources that are impeding adequate progress 
towards attaining the air quality standards. Additionally, the new test 
data could be used to improve the applicability and performance 
evaluations of various control technologies.

D. Request for Comments

    We encourage stakeholders to continue to participate in the process 
to refine Methods 201A and 202. We are requesting public comments on 
all aspects of the proposed test methods. EPA has already engaged 
several stakeholder groups as described in Section II.C of this 
preamble. Stakeholders and other members of the public who have not yet 
participated are encouraged to submit comments. EPA is soliciting as 
many constructive comments as possible in order to make the most 
appropriate changes to the methods.
    We are specifically interested in recommended alternatives to 
replace what we have proposed. When submitting comments on alternative 
approaches, please submit supporting information to substantiate the 
improvements that are achieved with your recommendation. For

[[Page 12977]]

recommended changes to the procedures, include supporting technical 
data and any associated cost information. For example, if you are 
proposing an alternative procedure, include data or information that 
would demonstrate how the alternative procedure would equal or improve 
the bias and precision of the proposed methods. In addition, provide 
data or cost information that would show the cost implications to 
testing companies and analytical laboratories of implementing the 
alternative procedure. Although our request for comments is not limited 
to these items, the following are examples of items for which we are 
specifically requesting comment.
1. Items Associated With Both Test Methods
    The proposed test methods are based upon EPA's assessment of 
comments made on the Clean Air Fine Particle Implementation Rule (April 
25, 2007, 70 FR 20586). Commenters expressed that there is an 
overarching need for test methods that are unbiased with respect to 
primary particulate matter emissions to the atmosphere and that the 
test methods must provide a high degree of consistency (precision) in 
these measurements. As a result, we reduced the numerous options and 
alternative procedures in the existing methods to a single set of 
prescriptive procedures that already existed within the methods. In 
addition, we made a few minor changes to reduce further the bias caused 
by sulfate artifacts. We are requesting comments on the specific set of 
procedures we have proposed and any replacement procedures that would 
be less demanding but that would achieve or improve bias and precision. 
We are also requesting comments on our decision to eliminate options or 
alternatives within the existing methods that may not achieve 
comparable results. If we were to consider alternative procedures that 
may not achieve comparable results, then what level of difference would 
be acceptable?
2. Items Associated With Method 201A
    Regarding this proposed method, stakeholders have commented on the 
sample duration that would be required to collect a weighable mass. EPA 
is requesting comments on alternative methodologies or hardware that 
would reduce the sample duration in order to reach a reasonable 
detection limit or to demonstrate that emissions are below the 
regulatory limit. Commenters should provide information or data, 
including cost information, which supports their recommendation.
    Stakeholders have expressed concern about the configuration and 
size of the proposed sampling train. Specifically, commenters have 
expressed concern that the size and length of the combined 
PM<INF>10</INF> cyclone and the PM<INF>2.5</INF> cyclone and filter 
require larger port opening(s) and a very large stack cross section to 
minimize blockage. In addition, stakeholders have stated that it is 
difficult to maintain stack temperature in the sampling train. 
Therefore, EPA requests comments on alternatives to the proposed 
procedures or hardware. EPA requests comments on alternative procedures 
or configurations that would reduce the blockage. EPA also requests 
comments on alternative configurations that would allow testers to 
maintain stack temperature in the sampling train, thus reducing or 
eliminating condensation in the primary or filterable particulate 
portions of the method. Recommendations to revise the sampling train 
size or configuration should include an assessment of the impacts of 
the recommended revisions on the sample size, required sample duration, 
and ability to collect a representative sample. Commenters should 
provide information or data, including cost information that supports 
their recommendation.
3. Items Associated With Method 202
    Stakeholders originally expressed concern about the formation of 
artifacts in Method 202 when sulfur dioxide was present in the stack 
gas. Based on laboratory experiments, the proposed revision to Method 
202 eliminates at least an additional 90 percent of the artifact over 
the best practices procedures of the existing Method 202. In addition, 
the laboratory experiments show that the proposed revision to Method 
202 reduces artifact at or below the detection limits of the method. 
EPA requests comments on any further concerns with the formation of 
artifacts in the proposed method.
    Stakeholders have expressed concern about glassware cleaning. 
Specifically, stakeholders have questioned the requirement to bake 
glassware at 300 [deg]C for 6 hours prior to use in order to reduce the 
background level of CPM. Stakeholders have stated that many stack 
testing firms and some analytical laboratories may not have ovens that 
can achieve this temperature. EPA requests information on the 
performance of a lower temperature oven in effectively reducing the 
blank level of CPM.
    Another stakeholder concern is whether glassware needs to be 
completely cleaned between sampling runs. The proposed method requires 
clean glassware at the start of each new source category test. EPA 
requests comments on alternatives that would minimize the cost of 
glassware preparation and reduce bias due to carryover from tests at 
the same source category and between source categories. Commenters 
should submit data or information to demonstrate that their alternative 
procedure would reduce or minimize the carryover or blank and would 
minimize the cost to prepare glassware.
    Stakeholders expressed concern about the need for Method 202 
following filtration at less than 30 [deg]C (85 [deg]F). EPA requests 
comments on how to clarify when Method 202 is or is not required.
    Stakeholders have expressed concern about the appropriate type of 
CPM filter required by the proposed method. EPA requests comments on 
the construction material and porosity of the filter. Commenters should 
address the capture efficiency required by the method (i.e., the filter 
must have an efficiency of at least 99.95 percent (<0.05 percent 
penetration) on 0.3 micron particles). Commenters should include how 
their alternative would minimize the blank contribution from the 
filters.
    Commenters have expressed concern about the additional analytical 
steps required to process the CPM filter. The proposed method requires 
extraction and combination of the filter extract with the appropriate 
impinger samples to accurately collect and measure sulfuric acid and 
other condensable material. Commenters should address alternative 
procedures for CPM filter analysis that would generate precise and 
unbiased analysis of CPM collected on the CPM filter.
    Stakeholders have expressed concern about maintaining the stack gas 
flow through the Teflon[supreg] membrane filter. Stakeholders have 
commented on their need to use a supplementary support filter to 
maintain flow through the sample filter. EPA requests comments 
regarding the use of a support filter that would help maintain stack 
gas flow while minimizing or eliminating the support filter's 
contribution to the sample mass. EPA requests comments on the use of 
this alternative and its potential impact on bias and precision, as 
well as its potential impact on cost.

IV. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review

    Under Executive Order (EO) 12866 (58 FR 51735, October 4, 1993), 
this proposed action is a ``significant regulatory action'' since it 
raises novel

[[Page 12978]]

legal or policy issues arising out of legal mandates, the President's 
priorities, or the principles set forth in this Executive Order. 
Accordingly, EPA submitted this proposed action to the Office of 
Management and Budget (OMB) for review under Executive Order 12866 and 
any changes made in response to OMB recommendations have been 
documented in the docket for this action.

B. Paperwork Reduction Act

    This proposed 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 proposed 
amendments do not contain any reporting or recordkeeping requirements. 
The proposed amendments revise two existing source test methods to 
allow one method to perform additional particle sizing at 2.5 
micrometers 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 proposed rule on 
small entities, I certify that this action will not have a significant 
economic impact on a substantial number of small entities. We do not 
anticipate that the proposed changes to Methods 201A and 202 will 
result in a significant economic impact 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 proposed rule will not have a significant economic 
impact on a substantial number of small entities, EPA nonetheless has 
tried to reduce the impact of this rule on small entities. In this 
preamble, we explained that this rule does not require any entities to 
use these proposed test methods. Such a requirement would be mandated 
by a separate independent regulatory action. We indicated that upon 
promulgation of this rule, some entities may be required to use these 
test methods as a result of existing permits or regulations. Since the 
cost to use the proposed 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 
revised test methods which are proposed. We also indicated that 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 proposal to modify the existing test 
methods. Consequently, we believe that this rule imposes little if any 
adverse economic impact to small entities. However, we continue to be 
interested in the potential impacts of the proposed rule on small 
entities and welcome comments on issues related to such impacts.

D. Unfunded Mandates Reform Act

    This rule does not contain a Federal mandate that may result in 
expenditures of $100 million or more for State, local, and tribal 
governments, in the aggregate, or the private sector in any one year. 
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 rule 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

    Executive Order 13132, entitled ``Federalism'' (64 FR 43255, August 
10, 1999), requires EPA to develop an accountable process to ensure 
``meaningful and timely input by State and local officials in the 
development of regulatory policies that have federalism implications.'' 
``Policies that have federalism implications'' is defined in the 
Executive Order to include regulations that 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.''
    This proposed rule 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 
PM<INF>2.5</INF> emissions is owned by a State or local government, 
those governments may incur a minimal compliance costs associated with 
conducting tests to quantify PM<INF>2.5</INF> 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. Thus, Executive Order 13132 does not apply to this 
rule.
    In the spirit of Executive Order 13132, and consistent with EPA 
policy to promote communications between EPA and State and local 
governments, EPA specifically solicits comment on this proposed rule 
from State and local officials.

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 PM<INF>2.5</INF> emissions is owned by a tribal government, 
those governments may incur minimal compliance costs associated with 
conducting tests to quantify PM<INF>2.5</INF> 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.

[[Page 12979]]

    EPA specifically solicits additional comment on this proposed rule 
from tribal officials.

G. Executive Order 13045: Protection of Children From Environmental 
Health and Safety Risks

    EPA interprets EO 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 EO has the 
potential to influence the regulation. This action is not subject to EO 
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 a ``significant energy action'' as defined in 
Executive Order 13211 (66 FR 28355 (May 22, 2001)), because it is not 
likely to have a significant adverse effect on the supply, 
distribution, or use of energy. This rule revises existing EPA test 
methods and does not affect energy supply, distribution, or use.

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 (15 U.S.C. 272 note) 
directs EPA to use voluntary consensus standards (VCS) 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.
    The rulemaking involves technical standards. Therefore, the Agency 
conducted a search to identify potentially applicable voluntary 
consensus standards. However, we identified no such standards, and none 
were brought to our attention in comments. Therefore, EPA has decided 
to amend portions of existing EPA test methods. While no comprehensive 
source test methods were identified, EPA identified two VCS which were 
applicable for use within the amended test methods. The first VCS cited 
in this proposal is American Society for Testing and Materials (ASTM) 
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. The second VCS cited in 
this proposed rule is ASTM D1193-06, ``Standard Specification for 
Reagent Water,'' for the proper selection of distilled ultra-filtered 
water. These VCS are available from the American Society for Testing 
and Materials, 100 Barr Harbor Drive, Post Office Box C700, West 
Conshohocken, PA 19428-2959.
    EPA welcomes comments on this aspect of the proposed rulemaking 
and, specifically, invites the public to identify potentially 
applicable VCS and to explain why such standards should be used in this 
regulation.

J. Executive Order 12898: Federal Actions To Address Environmental 
Justice in Minority Populations and Low-Income Populations

    Executive Order (EO) 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 proposed rule will not have 
disproportionately high and adverse human health or environmental 
effects on minority or low-income populations because it does not 
affect the level of protection provided to human health or the 
environment. The proposed amendments revise existing test methods to 
improve the accuracies of the measurements which are expected to 
improve environmental quality and reduce health risks for areas that 
may be designated as nonattainment.

List of Subjects in 40 CFR Part 51

    Administrative practice and procedure, Air pollution control, 
Carbon monoxide, Incorporation by reference, Intergovernmental 
relations, Lead, Nitrogen oxide, Ozone, Particulate matter, Reporting 
and recordkeeping requirements, Sulfur compounds, Volatile organic 
compounds.

    Dated: March 16, 2009.
Lisa P. Jackson,
Administrator.
    For the reasons set out in the preamble, title 40, chapter I of the 
Code of Federal Regulations is proposed to be amended as follows:

PART 51--[AMENDED]

    1. The authority citation for part 51 continues to read as follows:

    Authority: 23 U.S.C. 101; 42 U.S.C 7401-7671q.

    2. Amend Appendix M by revising Methods 201A and 202 to read as 
follows:

Appendix M to Part 51--Recommended Test Methods for State 
Implementation Plans

* * * * *

METHOD 201A--DETERMINATION OF PM10 AND PM2.5 EMISSIONS FROM STATIONARY 
SOURCES (Constant Sampling Rate Procedure)

1.0 Scope and Applicability

    1.1 Scope. The U.S. Environmental Protection Agency (U.S. EPA or 
``we'') developed this method to describe the procedures that the 
stack tester (``you'') must follow to measure particulate matter 
emissions equal to or less than a nominal aerodynamic diameter of 10 
micrometer (PM<INF>10</INF>) and 2.5 micrometer (PM<INF>2.5</INF>). 
If the gas filtration temperature exceeds 30 [deg]C (85 [deg]F), 
this method includes procedures to measure only filterable 
particulate matter (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 total primary 
(direct) particulate matter emissions to the atmosphere, both the 
filterable and condensable (material that condenses after passing 
through a filter) components, then you must combine the procedures 
in this method with the procedures in Method 202 for measuring 
condensable particulate matter. However, if the gas filtration 
temperature never exceeds 30 [deg]C (85 [deg]F), then use of Method 
202 is not required to measure total primary particulate matter.
    1.2 Applicability. You can use this method to measure filterable 
particulate matter from stationary sources only. Filterable 
particulate matter is collected in-stack with this method (i.e., the 
method measures materials that are solid or liquid at stack 
conditions).
    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 Results. To obtain results, you must have a thorough 
knowledge of the following test methods that are found in Appendices 
A-1 through A-3 of 40 CFR Part 60.
    (a) Method 1--Sample and Velocity Traverses for Stationary 
Sources.

[[Page 12980]]

    (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 Additional Methods. We do not anticipate that you will need 
additional test methods to measure ambient contributions of 
particulate matter to source emissions because ambient contributions 
are insignificant for most of the sources that are expected to be 
measured using this test method. However, when an adjustment for the 
ambient air particulate matter is needed, use the ambient air 
reference methods to quantify the ambient air contribution. If the 
source gas filtration temperature never exceeds 30 [deg]C (85 
[deg]F) and condensable particulate is not measured by Method 202, 
then the correction for ambient particulate matter must be adjusted 
for condensable material that vaporizes at the process temperature.
    1.6 Limitations. You cannot use this method to measure emissions 
following a wet scrubber because this method is not applicable for 
in-stack gases containing water droplets. To measure PM<INF>10</INF> 
and PM<INF>2.5</INF> in emissions where water droplets are known to 
exist, we recommend that you use Method 5. This method may not be 
suitable for sources with stack gas temperatures exceeding 260 
[deg]C (500 [deg]F). You may need to take extraordinary measures--
including the use of specialty metals (e.g., Inconel) to achieve 
reliable particulate mass since the threads of the cyclones may gall 
or seize, thus preventing the recovery of the collected particulate 
matter and rendering the cyclone unusable for subsequent use.
    1.7 Conditions. You can use this method to obtain both particle 
sizing and total filterable particulate if the isokinetics are 
within 90-110 percent, the number of sampling points is the same as 
Method 5 or 17, and the in-stack filter temperature is within the 
acceptable range. The acceptable range for the in-stack filter 
temperature is generally defined as the typical range of temperature 
for emission gases. The acceptable range varies depending on the 
source and control technology. 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 PM<INF>2.5</INF> 
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 
PM<INF>10</INF> and PM<INF>2.5</INF> 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 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 on each portion of this sampling train. Also, 
if you are using this method as an alternative to a required 
performance test, then you must receive approval from the 
appropriate authorities prior to conducting the test.

2.0 Summary of Method

    2.1 Summary. To measure PM<INF>10</INF> and PM<INF>2.5</INF>, 
extract a sample of gas at a predetermined constant flow rate 
through an in-stack sizing device. The sizing device separates 
particles with nominal aerodynamic diameters of 10 microns and 2.5 
microns. To minimize variations in the isokinetic sampling 
conditions, you must establish well-defined limits. Once a sample is 
obtained, remove uncombined water from the particulate, then use 
gravimetric analysis to determine the particulate mass for each size 
fraction. Changes in the original Method 201A of Appendix M to 40 
CFR part 51, supplement the filterable particulate procedures with 
the PM<INF>2.5</INF> cyclone from a conventional five-stage cascade 
cyclone train. The addition of a PM<INF>2.5</INF> cyclone between 
the PM<INF>10</INF> cyclone and the stack temperature filter in the 
sampling train supplements the measurement of PM<INF>10</INF> with 
the measurement of fine particulate matter. Without the addition of 
the PM<INF>2.5</INF> cyclone, the filterable particulate portion of 
the sampling train may be used to measure total and PM<INF>10</INF> 
emissions. Likewise, with the exclusion of the PM<INF>10</INF> 
cyclone, the filterable particulate portion of the sampling train 
may be used to measure total and PM<INF>2.5</INF> emissions. Figure 
1 of Section 17 presents the schematic of the sampling train 
configured with these changes.

3.0 Definitions

    [Reserved]

4.0 Interferences

    You cannot use this method to measure emissions following a wet 
scrubber because this method is not applicable for in-stack gases 
containing water droplets. 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 PM<INF>10</INF> and PM<INF>2.5</INF> following 
evaporation of the water.

5.0 Safety

    Disclaimer: You may have to use hazardous materials, operations, 
and equipment while using this method. We do not provide information 
on appropriate safety and health practices. You are responsible for 
determining the applicability of regulatory limitations and 
establishing appropriate safety and health practices. Handle 
materials and equipment properly.

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 
PM<INF>10</INF> and PM<INF>2.5</INF> 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 Teflon[supreg]-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 
PM<INF>10</INF> 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 PM<INF>2.5</INF> cyclones are used 
without PM<INF>10</INF> cyclones as part of the sampling train.
    6.1.2 PM<INF>10</INF> and PM<INF>2.5</INF> Sizing Device. Use a 
stainless steel (316 or equivalent) PM<INF>10</INF> and 
PM<INF>2.5</INF> sizing devices. The sizing devices must be cyclones 
that meet the design specifications shown in Figures 3, 4, 5, and 6 
of Section 17. Use a caliper to verify the dimensions of the 
PM<INF>10</INF> and PM<INF>2.5</INF> sizing devices to within <plus-
minus>0.02 cm of the design specifications. Example suppliers of 
PM<INF>10</INF> and PM<INF>2.5</INF> sizing devices include the 
following:

(a) Environmental Supply Company, Inc., 2142 Geer Street, Durham, 
North Carolina 27704, (919) 956-9688 (phone), (919) 682-0333 (fax).
(b) Apex Instruments, P.O. Box 727, 125 Quantum Street, Holly 
Springs, North Carolina 27540, (919) 557-7300 (phone), (919) 557-
7110 (fax).
(c) Andersen Instruments Inc., 500 Technology Court, Smyrna, Georgia 
30082, (770) 319-9999 (phone), (770) 319-0336 (fax).

    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 (incorporated by reference) 
and are approved by the Administrator. The Director of the Federal 
Register approves this incorporation by reference in accordance with 
5 U.S.C. 552(a) and 1 CFR part 51. You may obtain a copy from 
National Technical Information Service, http://www.ntis.gov or (800) 
553-6847. You may inspect a copy at the Office of Federal Register, 
800 North Capitol Street, NW., Suite 700, Washington, DC.
    6.1.3 Filter Holder. Use a filter holder that is either 
stainless steel (316 or equivalent) or Teflon[supreg]-coated 
stainless steel. 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 filter holders to support 25-, 
47-, and 63-mm diameter filters. Commercial size filter holders 
contain a Teflon[supreg] O-ring, a stainless steel screen that 
supports the filter, and a final Teflon[supreg] O-ring. Screw the 
assembly together and attach to the outlet of cyclone IV.
    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

[[Page 12981]]

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.
    6.1.5 Probe Liner. The probe extension must be glass-lined or 
Teflon[supreg]. Follow the specifications in Section 6.1.1.2 of 
Method 5.
    6.1.6 Differential Pressure Gauge, Condensers, Metering Systems, 
Barometer, and Gas Density Determination Equipment. Follow the 
requirements in Sections 6.1.1.4 through 6.1.3 of Method 5, as 
applicable.
    6.2 Sample Recovery Equipment.
    6.2.1 Filterable Particulate Recovery. Use the following 
equipment to quantitatively determine the amount of filterable 
particulate matter recovered from the sampling train. Follow the 
requirements specified in Sections 6.2.1 through 6.2.8 of Method 5, 
respectively.
(a) Filter holder brushes
(b) Wash bottles
(c) Glass sample storage containers
(d) Petri dishes
(e) Graduated cylinders and balance
(f) Plastic storage containers
(g) Funnel
(h) Rubber policeman

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. 
Additional information on these items is in the following 
paragraphs.
    7.1.1 Filter. Use a glass fiber, quartz, or Teflon[supreg] 
filter that does not a have an organic binder. The filter must also 
have an efficiency of at least 99.95 percent (<0.05 percent 
penetration) on 0.3 micron dioctyl phthalate smoke particles. 
Conduct the filter efficiency test in accordance with ASTM Method 
D2986-95a--Standard Method for Evaluation of Air, Assay Media by the 
Monodisperse DOP (Dioctyl Phthalate) Smoke Test (incorporated by 
reference). The Director of the Federal Register approves this 
incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 
CFR part 51. You may obtain a copy from American Society for Testing 
and Materials (ASTM), 100 Barr Harbor Drive, Post Office Box C700, 
West Conshohocken, PA 19428-2959. You may inspect a copy at the 
Office of Federal Register, 800 North Capitol Street, NW., Suite 
700, Washington, DC. Alternatively, you may use test data from the 
supplier's quality control program. If the source you are sampling 
has sulfur dioxide (SO<INF>2</INF>) or sulfite (SO<INF>3</INF>) 
emissions, you must use a filter that will not react with 
SO<INF>2</INF> or SO<INF>3</INF>. Depending on your application and 
project data quality objectives (DQOs), filters are commercially 
available in 25-, 47-, 83-, and 110-mm sizes.
    7.1.2 Silica Gel. Use an indicating-type silica gel of 6 to 16 
mesh. We must approve other types of desiccants (equivalent or 
better) before you use them. Allow the silica gel to dry for 2 hours 
at 175 [deg]C (350 [deg]F) if it is being reused. You do not have to 
dry new silica gel.
    7.1.3 Crushed ice. Obtain from the best readily available 
source.
    7.2 Sample Recovery and Analysis Reagents. You will need acetone 
and anhydrous sodium sulfate for the sample 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 residue blank. You must use acetone with blank values <1 ppm, 
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 1E-06 of the weight of acetone used in sample recovery be 
subtracted from the sample weight (i.e., the maximum blank 
correction is 0.079 mg per 100 mL of acetone used to recover 
samples).
    7.2.2 Particulate Sample Desiccant. Use indicating-type 
anhydrous sodium 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 must be trained and experienced with in-stack 
filtration systems (such as cyclones, impactors, and thimbles) and 
their operations.
    8.2 Preparations. Follow the pretest preparation instructions in 
Section 8.1 of Method 5.
    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.
    8.3.1 Sampling Site Location and Traverse Point Determination. 
Follow the standard procedures in Method 1 to select the appropriate 
sampling site. Then do all of the following:
    (a) Sampling site. Choose a location that maximizes the distance 
from upstream and downstream flow disturbances.
    (b) Traverse points. The recommended maximum number of total 
traverse points at any location is 12 as shown in Figure 7 of 
Section 17. Prevent the disturbance and capture of any solids 
accumulated on the inner wall surfaces by maintaining a 1-inch 
distance from the stack wall (\1/2\ inch for sampling locations less 
than 24 inches in diameter).
    (c) Round or rectangular duct or stack. If a duct or stack is 
round with two ports located 90 degrees apart, use six sampling 
points on each diameter. Use a 3 x 4 sampling point layout for 
rectangular ducts or stacks. Consult with the Administrator to 
receive approval for other layouts before you use them.
    (d) Sampling ports. To accommodate the in-stack cyclones for 
this method, you may need larger diameter sampling ports than those 
used by Method 5 or Method 17 for total filterable particulate 
sampling. When you must use nozzles smaller than 0.16 inch in 
diameter, the sampling port diameter must be 6 inches. Do not use 
the conventional 4-inch diameter port because the combined dimension 
of the PM<INF>10</INF> 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 24 inches.
    Minimize the blockage effects of the combination of the in-stack 
nozzle/cyclones and filter assembly for ducts with diameters greater 
than 24 inches by keeping the cross-sectional area of the assembly 
at 3 percent or less of the cross-sectional area of the duct.
    8.3.2.2 Ducts with diameters between 18 and 24 inches. Ducts 
with diameters between 18 and 24 inches have blockage effects 
ranging from 3 to 6 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 3 
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).
    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 to determine the presence or absence 
of cyclonic flow and then perform the following calculations.
    (a) As per Section 11.4 of Method 1, find and record the angle 
that has a null velocity pressure for each traverse point using a 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 008. You may need to 
obtain an alternate method approval prior to using a modified 
sampling approach.]

    8.3.4 Preliminary Velocity Profile. Conduct a preliminary 
velocity traverse by following Method 2 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.
    (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

[[Page 12982]]

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 <plus-minus>20 percent and/or gas temperature 
variations of approximately <plus-minus>10 [deg]C (<plus-minus>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. 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 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 Particulate matter concentration in the gas stream. 
Determine the particulate matter concentration for the 
PM<INF>2.5</INF> and the PM<INF>2.5</INF> to PM<INF>10</INF> 
components of the gas stream through qualitative measurements or 
estimates. 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 particulate matter 
weight for better accuracy at the source emission level. The 
collectable particulate matter 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 particulate matter concentrations in the >10 micrometer, 
<=10 and >2.5 micrometers, and <=2.5 micrometer size ranges. Typical 
particulate matter concentrations are listed in Table 1 of Section 
17. Additionally, relevant sections of AP-42 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 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.
    8.4 Pre-test Calculations. You must perform pre-test 
calculations to help select the appropriate gas sampling rate 
through cyclone I (PM<INF>10</INF>) and cyclone IV 
(PM<INF>2.5</INF>). 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 9 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 9 
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 9 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 
PM<INF>10</INF> and PM<INF>2.5</INF> separately in order to meet the 
necessary particle size criteria shown in Table 2 of Section 17.0.]

    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 The Assumed Reynolds Number. Verify the assumed Reynolds 
number (N<INF>re</INF>) by substituting the sampling rate 
(Q<INF>s</INF>) calculated in Equation 7 into Equation 8. Then use 
Table 5 of Section 17 to determine if the N<INF>re</INF> used in 
Equation 5 was correct.
    8.5.2 Final Sampling Rate. Recalculate the final sampling rate 
(Q<INF>s</INF>) if the assumed Reynolds number used in your initial 
calculation is not correct. Use Equation 7 to recalculate the 
optimum sampling rate (Q<INF>s</INF>).
    8.5.3 Meter Box [Delta]H. Use Equation 9 to calculate the meter 
box [Delta]H after you calculate the optimum sampling rate and 
confirm the Reynolds number.

    [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 
9 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 (that is, 80 
percent to 120 percent). This will also minimize an isokinetic 
sampling error for the particles at each point. First calculate the 
mean stack gas velocity, v<INF>s</INF>, using Equation 11. See 
Section 8.7.2 for information on correcting for blockage and use of 
different pitot tube coefficients. Then use Equation 12 to calculate 
the diameter of a nozzle that provides for isokinetic sampling at 
the mean stack gas velocity at flow Q<INF>s</INF>. From the 
available nozzles just smaller and just larger of this diameter, D, 
select the most promising nozzle. Perform the following steps for 
the selected nozzle.
    8.5.4.1 Minimum/maximum nozzle/stack velocity ratio. Use 
Equation 14 to calculate the minimum nozzle/stack velocity ratio, 
R<INF>min</INF>. Use Equation 15 to calculate the maximum nozzle/
stack velocity ratio, R<INF>max</INF>.
    8.5.4.2 Minimum gas velocity. Use Equation 16 to calculate the 
minimum gas velocity (v<INF>min</INF>) if R<INF>min</INF> is an 
imaginary number (negative value under the square root function) or 
if R<INF>min</INF> is less than 0.5. Use Equation 17 to calculate 
v<INF>min</INF> if R<INF>min</INF> is greater than or equal to 0.5.
    8.5.4.3 Maximum stack velocity. Use Equation 18 to calculate the 
maximum stack velocity (v<INF>max</INF>) if R<INF>max</INF> is less 
than 1.5. Use Equation 19 to calculate the stack velocity if 
R<INF>max</INF> is greater than or equal to 1.5.
    8.5.4.4 Conversion of gas velocities to velocity pressure. Use 
Equation 20 to convert v<INF>min</INF> to minimum velocity pressure, 
[Delta]p<INF>min</INF>. Use Equation 21 to convert v<INF>max</INF> 
to maximum velocity pressure, [Delta]p<INF>max</INF>.
    8.5.4.5 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]p<INF>min</INF> 
and [Delta]p<INF>max</INF>. 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 PM<INF>2.5</INF> only, you may have only 
two traverse points out of 12 that are outside the range of the 
[Delta]p<INF>min</INF> and [Delta]p<INF>max</INF> (i.e., 16 percent 
failure rate rounded to the nearest whole number). If the coarse 
fraction for PM<INF>10</INF> determination is included, only one 
traverse point out of 12 can fall outside the minimum-maximum 
velocity pressure range (i.e., 8 percent failure rate rounded to the 
nearest whole number).
    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 Teflon[supreg] 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

[[Page 12983]]

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 when stack temperatures exceed 205 
[deg]C (400 [deg]F). This method may not be suitable for sources 
with stack gas temperatures exceeding 260 [deg]C (500 [deg]F). You 
may need to take extraordinary measures including the use of 
specialty metals (e.g., Inconel) to achieve reliable particulate 
mass since the threads of the cyclones may gall or seize, thus 
preventing the recovery of the collected particulate matter and 
rendering the cyclone unusable for subsequent use. You must also 
keep the nozzle covered to protect it from nicks and scratches.
    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.]

    Weld 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.

    [Note: Calibrate the pitot tube on the sampling head because the 
cyclone body is a potential source flow disturbance.]

    8.6.3 Filter. You must number and tare the filters before use. 
To tare the filters, desiccate each filter at 20 <plus-minus> 5.6 
[deg]C (68 <plus-minus> 10 [deg]F) and ambient pressure for at least 
24 hours and weigh at intervals of at least 6 hours to a constant 
weight, i.e., <0.5 mg change from previous weighing; record results 
to the nearest 0.1 mg. During each weighing, the filter must not be 
exposed to the laboratory atmosphere for longer than 2 minutes and a 
relative humidity above 50 percent. Alternatively, the filters may 
be oven-dried at 104 [deg]C (220 [deg]F) for 2 to 3 hours, 
desiccated for 2 hours, and weighed. Use tweezers or clean 
disposable surgical gloves to place a labeled (identified) and pre-
weighed filter in both filterable and condensable particulate filter 
holders. You must center the filter and properly place the gasket so 
that the sample gas stream will not circumvent the filter. Check the 
filter for tears after the assembly is completed. Then screw the 
filter housing together to prevent the seal from leaking.
    8.6.7 Moisture Trap. If you are measuring only filterable 
particulate (or you are sure that the 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 may also be used 
to collect moisture that passes through the ambient filter. If you 
are measuring condensable particulate matter in combination with 
this method, then follow the procedures in Method 202 for moisture 
collection.
    8.6.8 Leak Check. Use the procedures outlined in Section 8.4 of 
Method 5 to leak check the entire sampling system. Specifically 
perform the following procedures:
    8.6.8.1 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 ACFM 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 (see Section 11.1) for the specific test.

    [Note: Do not conduct a leak check during port changes.]

    8.6.8.2 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.
    8.6.9 Sampling Head. You must preheat the combined sampling head 
to the stack temperature of the gas stream at the test location 
(<plus-minus>10 [deg]C, <plus-minus>50 [deg]F). This will heat the 
sampling head and prevent moisture from condensing from the sample 
gas stream. Record the site barometric pressure and stack pressure 
on the field test data sheet.
    8.6.9.1 Unsaturated stacks. You must complete a passive warmup 
(of 30-40 min) within the stack before the run begins to avoid 
internal condensation.

    [Note: Unsaturated stacks do not have entrained droplets and 
operate at temperatures above the local dew point of the stack gas.]

    8.6.9.2 Shortened warm-up of unsaturated stacks. 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, except 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 (t<INF>r</INF>), 
based on achieving the data quality objectives or emission limit of 
the affected facility. We recommend 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 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, or 
sampling time, at each traverse point proportionately with the point 
velocity.
    8.7.1.1 Dwell time at first sampling point. Calculate the dwell 
time for the first point, t<INF>1</INF>, using Equation 22. You must 
use the data from the preliminary traverse. Here, N<INF>tp</INF> 
equals the total number of traverse points.
    8.7.1.2 Dwell time at remaining sampling points. Calculate the 
dwell time at each of the remaining traverse points, t<INF>n</INF>, 
using Equation 23. This time you must use the actual test run data.

    [Note: Round the dwell times to the nearest 15 seconds.] Each 
traverse point must have a dwell time of at least 2 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 
24 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 25 to 
calculate an average probe blockage correction factor 
(b<INF>f</INF>) if the diameter of your stack or duct is between 18 
and 24 inches. A probe blockage factor is calculated because of the 
flow blockage caused by the relatively large cross-sectional area of 
the combined cyclone sampling head, as discussed in Section 8.3.2.2 
and illustrated in Figure 8 of Section 17.

    [Note: The sampling head (including the PM<INF>10</INF> cyclone, 
PM<INF>2.5</INF> cyclone, pitot and filter holder) has a projected 
area of approximately 20.5 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 4 square inches to the full 20.5 inches. The average 
cross-sectional area blocked is 12 square inches.]

    8.7.2.3 Final adjusted velocity pressure. Calculate the final 
adjusted velocity pressure ([Delta]p<INF>s2</INF>) using Equation 
26.

    [Note: Figure 8 of Section 17 illustrates that the blockage 
effect of the large combined cyclone sampling head increases rapidly 
below diameters of 18 inches. Therefore, you must follow the 
procedures outlined in Method 1A to conduct tests in small stacks (< 
inches diameter). 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, 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)

[[Page 12984]]

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 Equations 22 and 23. In addition to 
these procedures, you must also use running starts and stops if the 
static pressure at the sampling location is more negative than 5 in. 
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 (<plus-minus> 10 
[deg]C, <plus-minus> 50 [deg]F).

    [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 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 insure proper particle sizing and prevent 
condensation on the walls of the cyclones.]

    Remove the protective cover from the nozzle. To begin sampling, 
immediately start the pump and adjust the flow to calculated 
isokinetic conditions. Position the probe at the first sampling 
point with the nozzle pointing directly into the gas stream. 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.]

    (a) Traverse the stack cross-section, as required by Method 1 
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 20 and 21) 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 the 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 the flow through the sampling system at the last 
sampling point. Remove the sampling train from the stack while it is 
still operating (running stop). Then stop the pump, and record the 
final dry gas meter reading and other test parameters on the field 
test data sheet.
    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. 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 if 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 sample head (combined 
cyclone/filter assembly) from the stack. 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. At the conclusion of the test, 
document final test conditions and remove the pitot tube and 
combined cyclone sampling head from the source. Make sure that you 
do not scrape the pitot tube or the combined cyclone sampling head 
against the port or stack walls.

    [Note: After you stop the gas flow, 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.]

    After cooling and when the probe can be safely handled, wipe off 
all external surfaces near the cyclone nozzle, and cap the inlet to 
cyclone I. Remove the combined cyclone/filter sampling head from the 
probe. Cap the outlet of the filter housing to prevent particulate 
matter 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 ACFM or 4 percent of the average 
sampling rate during the test run (whichever is less), the run is 
invalid, and you must repeat it.
    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 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 
condensable particulate matter in combination with this method, then 
leave the silica in the impinger for recovery after the post-test 
nitrogen purge is complete.
    8.7.5.5 Recovery of particulate matter. Recovery involves the 
quantitative transfer of particles in the following size range: > 10 
micrometers; <= 10 micrometers but > 2.5 micrometers; and <= 2.5 
micrometers. You must use a Nylon or Teflon 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, <= PM<INF>2.5</INF> 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 identified as Container <greek-i>1. Using a dry 
Nylon bristle brush and/or a sharp-edged blade, carefully transfer 
any particulate matter 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 <= 2.5 
micrometers that are caught on the in-stack filter.
    (b) Container #2, <ls-thn-eq> PM<INF>10</INF> micrometer 
filterable particulate--Quantitatively recover the particulate 
matter from the cyclone I cup and acetone rinses (and brush 
cleaning) 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 must keep any dust found on the 
outside of cyclone I and cyclone nozzle external surfaces out of the 
sample. This container holds particulate matter > 10 micrometers.
    (c) Container #3, Filterable particulate <= 10 micrometer and 
<ls-thn-eq> 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 <greek-i>3. 
Seal the container and mark the liquid level on the outside. This 
container holds particulate matter <= 10 micrometers but > 2.5 
micrometers.
    (d) Container #4, <= PM<INF>2.5</INF> micrometers acetone rinses 
of the exit tube of cyclone IV and front half of the filter holder--
Retrieve the acetone rinses (and brush cleaning) of the exit tube of 
cyclone IV and the front half of the filter holder in container 
<greek-i>4. Seal the container and mark the liquid level on the 
outside of the container. This container holds particulate matter 
that is <= 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. This container holds the remainder of the liquid water from 
the emission gases.
    (f) Container #6, Silica Gel Absorbent--Transfer the silica gel 
to its original container

[[Page 12985]]

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 <greek-i>6 are weighed during 
sample analysis.
    (g) Container #7, Acetone Rinse Blank--Take 100 ml of the 
acetone directly from the wash bottle you used, and place it in 
Container <greek-i>7 labeled Acetone Rinse 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 
using data quality indicators that require review of recording and 
transfer of raw data, calculations, and documentation of testing 
procedures.
    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 Health and Safety Plan. Develop a health and safety plan to 
ensure the safety of your employees who are on site conducting the 
particulate emission test. Your plan must conform to all applicable 
OSHA, MSHA, and DOT regulatory requirements. The procedures must 
also conform to the plant health and safety requirements.
    9.5 Calibration Checks. Perform calibration check procedures on 
analytical balances each time they are used.
    9.6 Glassware. Use class A volumetric glassware for titrations, 
or calibrate your equipment against NIST traceable glassware.

10.0 Calibration and Standardization

    [Note: Maintain a laboratory log of all calibrations.]

    10.1 Gas Flow Velocities. Measure the gas flow velocities at the 
sampling locations using Method 2. You must use an S-type pitot tube 
that meets the required EPA specifications (EPA Publication 600/4-
77-0217b) during these velocity measurements. 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 
oriented properly 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.

    [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. Calibrate the thermocouples using 
the procedures described in Section 10.1.4.1.2 of Method 2 to 
calibrate the thermocouples. Calibrate each temperature sensor at a 
minimum of three points over the anticipated range of use against an 
NIST-traceable mercury-in-glass thermometer.
    10.3 Nozzles. You may use stainless steel (316 or equivalent) or 
Teflon[supreg]-coated nozzles for isokinetic sampling. Make sure 
that all nozzles are thoroughly cleaned, visually inspected, and 
calibrated according to the procedure outlined in Section 10.1 of 
Method 5.
    10.4 Dry Gas Meter Calibration. Calibrate your dry gas meter 
following the calibration procedures in Section 16.1 of Method 5. 
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 pretest and post-test 
calibrations must agree within <plus-minus>5 percent.

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. 
Alternatively, data may be recorded electronically using software 
applications such as the Electronic Reporting Tool (ERT) located at 
the following internet address: (http://www.epa.gov/ttn/chief/ert/ert_tool.html).
    11.2 Dry Weight of Particulate Matter. Determine the dry weight 
of particulate following procedures outlined in this section.
    11.2.1 Container <greek-i>1, <= PM <INF>2.5</INF> micrometer 
filterable particulate. Transfer the filter and any loose 
particulate from the sample container to a tared glass weighing 
dish. Desiccate for 24 hours in a desiccator containing anhydrous 
calcium sulfate or indicating silica gel. Weigh to a constant 
weight, and report the results to the nearest 0.1 mg. For the 
purposes of this section, the term ``constant weight'' means a 
difference of no more than 0.5 mg or 1 percent of total weight less 
tare weight, whichever is greater, between two consecutive 
weighings, with no less than 6 hours of desiccation time between 
weighings.
    11.2.2 Container <greek-i>2, > PM <INF>10</INF> micrometer 
filterable particulate acetone rinse. Separately treat this 
container like Container <greek-i>1.
    11.2.3 Container <greek-i>3, Filterable particulate <= 10 
micrometer and >= 2.5 micrometers acetone rinse. Separately treat 
this container like Container <greek-i>1.
    11.2.4 Container <greek-i>4, <= PM <INF>2.5</INF> 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, and evaporate to dryness at 
ambient temperature and pressure. Desiccate for 24 hours, and weigh 
to a constant weight. Report the results to the nearest 0.1 g.
    11.2.5 Container <greek-i>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 <plus-minus>1 
ml or gravimetrically to <plus-minus>0.5 g.
    11.2.6 Container <greek-i>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 <greek-i>7, Acetone rinse blank. Use 100 ml of 
acetone from the blank container for this analysis. If insufficient 
liquid is available or if the acetone has been lost due to container 
breakage, either void the sample or use methods, subject to the 
approval of the Administrator, to correct the final results. 
Transfer 100 ml of the acetone to a clean 250 ml beaker. Evaporate 
the acetone at room temperature and pressure in a laboratory hood to 
approximately 10 ml. Quantitatively transfer the beaker contents to 
a 50 ml preweighed tin, and evaporate 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 for compliance 
testing specifies English units. The following nomenclature is used.

A = Area of stack or duct at sampling location, square inches.
A<INF>n</INF> = Area of nozzle, square feet.
b<INF>f</INF> = Average blockage factor calculated in Equation 25, 
dimensionless.
B<INF>ws</INF> = Moisture content of gas stream, fraction e.g., 10% 
H<INF>2</INF>O is B<INF>ws</INF> = 0.10).
C = Cunningham correction factor for particle diameter, 
D<INF>p</INF>, and calculated using the actual stack gas 
temperature, dimensionless.
%CO<INF>2</INF> = Carbon Dioxide content of gas stream, % by volume.
C<INF>a</INF> = Acetone blank concentration, mg/mg.
C<INF>fPM10</INF> = Conc. of filterable PM<INF>10</INF> particulate 
matter, gr/DSCF.

[[Page 12986]]

C<INF>fPM2.5</INF> = Conc. of filterable PM<INF>2.5</INF> 
particulate matter, gr/DSCF.
C<INF>p</INF> = Pitot coefficient for the combined cyclone pitot, 
dimensionless.
C<INF>p</INF>' = Coefficient for the pitot used in the preliminary 
traverse, dimensionless.
C<INF>r</INF> = Re-estimated Cunningham correction factor for 
particle diameter equivalent to the actual cut size diameter and 
calculated using the actual stack gas temperature, dimensionless.
C<INF>tf</INF> = Conc. of total filterable particulate matter, gr/
DSCF.
C<INF>1</INF> = -150.3162 (micropoise)
C<INF>2</INF> = 18.0614 (micropoise/K \0.5\) = 13.4622 (micropoise/R 
\0.5\)
C<INF>3</INF> = 1.19183 x 10 \6\ (micropoise/K \2\) = 3.86153 x 10 
\6\ (micropoise/R \2\)
C<INF>4</INF> = 0.591123 (micropoise)
C<INF>5</INF> = 91.9723 (micropoise)
C<INF>6</INF> = 4.91705 x 10 <SUP>-5</SUP> (micropoise/K \2\) = 
1.51761 x 10 <SUP>-5</SUP> (micropoise/R \2\)
D= Inner diameter of sampling nozzle mounted on Cyclone I, in.
D<INF>p</INF> = Physical particle size, micrometers.
D<INF>50</INF> = Particle cut diameter, micrometers.
D<INF>50-1</INF>= Re-calculated particle cut diameters based on re-
estimated C<INF>r</INF>, micrometers.
D<INF>50LL</INF> = Cut diameter for cyclone I corresponding to the 
2.25 micrometer cut diameter for cyclone IV, micrometers.
D<INF>50N</INF> = D<INF>50</INF> value for cyclone IV calculated 
during the Nth iterative step, micrometers.
D<INF>50 (N+1)</INF> = D<INF>50</INF> value for cyclone IV 
calculated during the N+1 iterative step, micrometers.
D<INF>50T</INF> = Cyclone I cut diameter corresponding to the middle 
of the overlap zone shown in Figure 9 of Section 17, micrometers.
I = Percent isokinetic sampling, dimensionless.
in. = Inches
K<INF>p</INF> = 85.49, [(ft/sec)/(pounds/mole -[deg]R)].
m<INF>a</INF> = Mass of residue of acetone after evaporation, mg.
M<INF>d</INF> = Molecular weight of dry gas, pounds/pound mole.
M<INF>w</INF> = Molecular weight of wet gas, pounds/pound mole.
M<INF>1</INF> = Milligrams of particulate matter collected on the 
filter, <= 2.5 micrometers.
M<INF>2</INF> = Milligrams of particulate matter recovered from 
Container <greek-i>2 (acetone blank corrected), >10 micrometers.
M<INF>3</INF> = Milligrams of particulate matter recovered from 
Container <greek-i>3 (acetone blank corrected), <=10 and >2.5 
micrometers.
M<INF>4</INF> = Milligrams of particulate matter recovered from 
Container <greek-i>4 (acetone blank corrected), <=2.5 micrometers.
N<INF>tp</INF> = Number of iterative steps or total traverse points.
N<INF>re</INF> = Reynolds number, dimensionless.
%O<INF>2,wet</INF> = 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 %O<INF>2</INF> must be multiplied by the 
quantity (1-B<INF>ws</INF>) to convert to the actual volume 
fraction. Therefore, %O<INF>2,wet</INF> = (1-B<INF>ws</INF>) * 
%O<INF>2</INF>, dry]

P<INF>bar</INF> = Barometric pressure, in. Hg.
P<INF>s</INF> = Absolute stack gas pressure, in. Hg.
Q<INF>s</INF> = Sampling rate for cyclone I to achieve specified 
D<INF>50</INF>, ACFM.
Q<INF>sST</INF> = Dry gas sampling rate through the sampling 
assembly, DSCFM.
Q<INF>I</INF> = Sampling rate for cyclone I to achieve specified 
D<INF>50</INF>, ACFM.
Q<INF>IV</INF> = Sampling rate for cyclone IV to achieve specified 
D<INF>50</INF>, ACFM.
R<INF>max</INF> = Nozzle/stack velocity ratio parameter, 
dimensionless.
R<INF>min</INF> = Nozzle/stack velocity ratio parameter, 
dimensionless.
T<INF>m</INF> = Meter box and orifice gas temperature, [deg]R.
t<INF>n</INF> = Sampling time at point n, min.
t<INF>r</INF> = Total projected run time, min.
T<INF>s</INF> = Absolute stack gas temperature, [deg]R.
t<INF>1</INF> = Sampling time at point 1, min.
v<INF>max</INF> = Maximum gas velocity calculated from Equations 18 
or 19, ft/sec.
v<INF>min</INF> = Minimum gas velocity calculated from Equations 16 
or 17, ft/sec.
v<INF>n</INF> = Sample gas velocity in the nozzle, ft/sec.
v<INF>s</INF> = Velocity of stack gas, ft/sec.
V<INF>a</INF> = Volume of acetone blank, ml.
V<INF>aw</INF> = Volume of acetone used in blank wash, ml.
V<INF>c</INF> = Quantity of water captured in impingers and silica 
gel, ml.
V<INF>m</INF> = Dry gas meter volume sampled, ACF.
V<INF>ms</INF> = Dry gas meter volume sampled, corrected to standard 
conditions, DSCF.
V<INF>ws</INF> = Volume of water vapor, SCF.
V<INF>b</INF> = Volume of aliquot taken for IC analysis, ml.
V<INF>ic</INF> = Volume of impinger contents sample, ml.
W<INF>a</INF> = Weight of residue in acetone blank wash, mg.
Z = Ratio between estimated cyclone IV D<INF>50</INF> values, 
dimensionless.
[Delta]H = Meter box orifice pressure drop, in. W.C.
[Delta]H<INF>@</INF> = Pressure drop across orifice at flow rate of 
0.75 SCFM at standard conditions, in. W.C.

    [Note: specific to each orifice and meter box.]

[([Delta]p)\0.5\]<INF>avg</INF> = Average of square roots of the 
velocity pressures measured during the preliminary traverse, in. 
W.C.
[Delta]p<INF>m</INF> = Observed velocity pressure using S-type pitot 
tube in preliminary traverse, in. W.C.
[Delta]p<INF>max</INF> = Maximum velocity pressure, in. W.C.
[Delta]p<INF>min</INF> = Minimum velocity pressure, in. W.C.
[Delta]p<INF>n</INF> = Velocity pressure measured at point n during 
the test run, in. W.C.
[Delta]p<INF>s</INF> = Velocity pressure calculated in Equation 24, 
in. W.C.
[Delta]p<INF>s1</INF> = Velocity pressure adjusted for combined 
cyclone pitot tube, in. W.C.
[Delta]p<INF>s2</INF> = Velocity pressure corrected for blockage, 
in. W.C.
[Delta]p<INF>1</INF> = Velocity pressure measured at point 1, in. 
W.C.
[gamma] = Dry gas meter gamma value, dimensionless.
[mu] = Gas viscosity, micropoise.
[thetas] = Total run time, minutes.
[rho]<INF>a</INF> = 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 D<INF>50</INF> of cyclone IV and the 
concentrations of the particulate matter in the various size ranges.
    12.3.1 D<INF>50</INF> of cyclone IV. To determine the actual 
D<INF>50</INF> for cyclone IV, recalculate the Cunningham correction 
factor and the Reynolds number for the best estimate of cyclone IV 
D<INF>50</INF>. 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 D<INF>50</INF> of 2.5 
micrometers into Equation 4. This will give you a new Cunningham 
correction factor that is based on actual data.
    12.3.1.2 Initial D<INF>50</INF> for cyclone IV. Determine the 
initial estimate for cyclone IV D<INF>50</INF> using the test 
condition Reynolds number calculated with Equation 8 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 
D<INF>50</INF> for cyclone IV with Equation 33, using actual test 
data.
    (b) If the Reynolds number is equal to or greater than 3,162, 
calculate the D<INF>50</INF> for cyclone IV with Equation 34, using 
actual test data.
    (c) Insert the ``new'' D<INF>50</INF> value calculated by either 
Equation 33 or 34 into Equation 35 to re-establish the Cunningham 
Correction Factor (C<INF>r</INF>).

    [Note: Use the test condition calculated Reynolds number to 
determine the most appropriate equation (Equation 33 or 34).]

    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 D<INF>50-1</INF>.
    (a) Use Equation 36 to calculate the re-established cyclone IV 
D<INF>50-1</INF> if the Reynolds number is less than 3,162.
    (b) Use Equation 37 to calculate the re-established cyclone IV 
D<INF>50-1</INF> if the Reynolds number is equal to or greater than 
3,162.
    12.3.1.4 Establishing ``Z'' values. The ``Z'' value is the 
result of an analysis that you must perform to determine if the 
Cunningham correction factor is acceptable. Compare the calculated 
cyclone IV D<INF>50</INF> (either Equation 33 or 34) to the re-
established cyclone IV D<INF>50-1</INF> (either Equation 36 or 37) 
values based upon the test condition calculated Reynolds number 
(Equation 38). Follow these procedures.
    (a) Use Equation 38 to calculate the ``Z''. If the ``Z'' value 
is between 0.99 and 1.01, the D<INF>50-1</INF> value is the best 
estimate of the cyclone IV D<INF>50</INF> cut diameter for your test 
run.
    (b) If the ``Z'' value is greater than 1.01 or less than 0.99, 
re-establish a Cunningham correction factor based on the 
D<INF>50-1</INF> value determined in either Equations 36 or 37, 
depending upon the test condition Reynolds number.
    (c) Use the second revised Cunningham correction to re-calculate 
the cyclone IV D<INF>50</INF>.
    (d) Repeat this iterative process as many times as necessary 
using the prescribed

[[Page 12987]]

equations until you achieve the criteria documented in Equation 39.
    12.3.2 Particulate concentration. Use the particulate catch 
weights in the combined cyclone sampling train to calculate the 
concentration of particulate matter in the various size ranges. You 
must correct the concentrations for the acetone blank.
    12.3.2.1 Acetone blank concentration. Use Equation 41 to 
calculate the acetone blank concentration (C<INF>a</INF>).
    12.3.2.2 Acetone blank weight. Use Equation 42 to calculate the 
acetone blank weight (W<INF>a</INF>).

    [Note: Correct each of the particulate matter weights per size 
fraction by subtracting the acetone blank weight (that is, 
M<INF>2,3,4</INF>-W<INF>a</INF>)].

    12.3.2.3 Particulate weight catch per size fraction. Subtract 
the weight of the acetone blank from the particulate weight catch in 
each size fraction.

    [Note: Do not subtract a blank value of greater than 0.001 
percent of the weight of the acetone used from the sample weight. 
Use the following procedures.]

    (a) Use Equation 43 to calculate the particulate matter 
recovered from Containers <greek-i>1, <greek-i>2, <greek-i>3, and 
<greek-i>4. This is the total collectable particulate matter 
(C<INF>tf</INF>).
    (b) Use Equation 44 to determine the quantitative recovery of 
PM<INF>10</INF> particulate matter (C<INF>fPM10</INF>) from 
Containers <greek-i>1, <greek-i>3, and <greek-i>4.
    (c) Use Equation 45 to determine the quantitative recovery of 
PM<INF>2.5</INF> particulate (C<INF>fPM</INF><INF>2.5</INF>) 
recovered from Containers <greek-i>1 and <greek-i>4.
    12.4 Reporting. You must include the following list of 
conventional elements in the emissions test report.
    (a) Emission test description including any deviations from this 
protocol.
    (b) Summary data tables on a run-by-run basis.
    (c) Flowchart of the process or processes tested.
    (d) Sketch of the sampling location.
    (e) Preliminary traverse data sheets including cyclonic flow 
checks.
    (f) Raw field data sheets.
    (g) Laboratory analytical sheets and case narratives.
    (h) Sample calculations.
    (i) Pretest and post-test calibration data.
    (j) Chain of custody forms.
    (k) Documentation of process and air pollution control system 
data.
    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] TP25MR09.000

    Molecular Weight of Wet Gas. Calculate the molecular weight of 
the stack gas on a wet basis using Equation 2.
[GRAPHIC] [TIFF OMITTED] TP25MR09.001

    Gas Viscosity. Calculate the gas viscosity using Equation 3. 
This equation uses constants for gas temperatures in [deg]R.
[GRAPHIC] [TIFF OMITTED] TP25MR09.002

    Cunningham Correction Factor. The Cunningham correction factor 
is calculated for a 2.25 micrometer diameter particle.
[GRAPHIC] [TIFF OMITTED] TP25MR09.003

    Lower Limit Cut Diameter for Cyclone I for Nre < 3,162. The 
Cunningham correction factor is for a 2.25 micrometer diameter 
particle.
[GRAPHIC] [TIFF OMITTED] TP25MR09.004

    Cut Diameter for Cyclone I for the Middle of the Overlap Zone.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.005
    
    Sampling Rate.

[[Page 12988]]

[GRAPHIC] [TIFF OMITTED] TP25MR09.006

    Reynolds Number.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.007
    
    Meter Box Orifice Pressure Drop.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.008
    
    Lower Limit Cut Diameter for Cyclone I for Nre >= 3,162. The 
Cunningham correction factor is for a 2.25 micrometer diameter 
particle.
[GRAPHIC] [TIFF OMITTED] TP25MR09.009

    Velocity of Stack Gas. Correct the mean preliminary velocity 
pressure for C<INF>p</INF> and blockage using Equations 23, 24, and 
25.
[GRAPHIC] [TIFF OMITTED] TP25MR09.010

    Calculated Nozzle Diameter for Acceptable Sampling Rate.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.011
    
    Velocity of Gas in Nozzle.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.012
    
    Minimum Nozzle/Stack Velocity Ratio Parameter.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.013
    
    Maximum Nozzle/Stack Velocity Ratio Parameter.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.014
    
    Minimum Gas Velocity for Rmin <= 0.5.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.015
    
    Minimum Gas Velocity for Rmin >= 0.5.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.016
    
    Maximum Gas Velocity for Rmax < 1.5.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.017
    
    Maximum Gas Velocity for R<INF>max</INF> <ls-thn-eq>= 1.5.

[[Page 12989]]

[GRAPHIC] [TIFF OMITTED] TP25MR09.018

    Minimum Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.019
    
    Maximum Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.020
    
    Sampling Time at Point 1. N<INF>tp</INF> is the total number of 
traverse points. You must use the preliminary velocity traverse 
data.
[GRAPHIC] [TIFF OMITTED] TP25MR09.021

    Sampling Time at Point n. You must use the actual test run data 
at each point, n, and test run point 1.
[GRAPHIC] [TIFF OMITTED] TP25MR09.022

    Adjusted Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.023
    
    Average Probe Blockage Factor.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.024
    
    Velocity Pressure.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.025
    
    Dry Gas Volume Sampled at Standard Conditions.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.026
    
    Sample Flow Rate at Standard Conditions.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.027
    
    Volume of Water Vapor.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.028
    
    Moisture Content of Gas Stream.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.029
    
    Sampling Rate.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.030
    


[[Page 12990]]


    [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] TP25MR09.031

    Particle Cut Diameter for N<INF>re</INF> < 3,162 for Cyclone IV. 
C must be recalculated using the actual test run data and a 
D<INF>50</INF> (D<INF>p</INF>) of 2.5.
[GRAPHIC] [TIFF OMITTED] TP25MR09.032

    Particle Cut Diameter for N<INF>re</INF> <ls-thn-eq>= 3,162 for 
Cyclone IV. C must be recalculated using the actual test run data 
and a D<INF>50</INF> (D<INF>p</INF>) of 2.5.
[GRAPHIC] [TIFF OMITTED] TP25MR09.033

    Re-estimated Cunningham Correction Factor. You must use the 
actual test run Reynolds Number (N<INF>re</INF>) value and select 
the appropriate D<INF>50</INF> from Equation 32 or 33 (or Equation 
36 or 37 if reiterating).
[GRAPHIC] [TIFF OMITTED] TP25MR09.034

    Re-calculated Particle Cut Diameter for N<INF>re</INF> < 3,162.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.035
    
    Re-calculated Particle Cut Diameter for N <ls-thn-eq>= 3,162.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.036
    
    Ratio (Z) Between D<INF>50</INF> and D<INF>50-1</INF> Values.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.037
    
    Acceptance Criteria for Z Values. The number of iterative steps 
is represented by N.
[GRAPHIC] [TIFF OMITTED] TP25MR09.038


[[Page 12991]]


    Percent Isokinetic Sampling.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.039
    
    Acetone Blank Concentration.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.040
    
    Acetone Blank Weight.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.041
    
    Concentration of Total Filterable Particulate Matter.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.042
    
    Concentration of Filterable PM<INF>10</INF> Particulate Matter.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.043
    
    Concentration of Filterable PM<INF>2.5</INF> Particulate Matter.
    [GRAPHIC] [TIFF OMITTED] TP25MR09.044
    
13.0 Method Performance

    (a) Field evaluation of PM<INF>10</INF> and total particulate 
matter showed that the precision of constant sampling rate method 
was the same magnitude as Method 17 (approximately 5 percent). 
Precision in PM<INF>10</INF> and PM<INF>10</INF> fraction between 
multiple trains showed standard deviations of 2 to 4 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 PM<INF>10</INF> method 
for total mass, referenced to Method 17, was -2<plus-minus> 4.4 
percent. A small bias was found between Method 201A and Method 17 
total particulate matter (10%) (Farthing, 1988).
    (b) Laboratory evaluation and guidance for PM<INF>10</INF> 
cyclones were designed to limit error due to spatial variations to 
10 percent. The maximum allowable error due to anisokinetic sampling 
was limited to <plus-minus>20 percent for 10 [mu]m particles in 
laboratory tests (Farthing, 1988b).

14.0 Pollution Prevention

    [Reserved]

15.0 Waste Management

    [Reserved]

16.0 References

    We used the following references to develop this test method:
    1. Dawes, S.S., and W.E. Farthing. ``Application Guide for 
Measurement of PM<INF>2.5</INF> 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), November 1990.
    2. U.S. Environmental Protection Agency, Federal Reference 
Methods 1 through 5 and Method 17, 40 CFR 60, Appendix A.
    3. Richards, J.R. ``Test protocol: PCA PM<INF>10</INF>/
PM<INF>2.5</INF> Emission Factor Chemical Characterization 
Testing,'' PCA R&D Serial No. 2081, Portland Cement Association, 
1996.
    4. Farthing and Co-workers, 1988a ``PM<INF>10</INF> Source 
Measurement Methodology: Field Studies,'' EPA 600/3-88/055, NTIS 
PB89-194287/AS, U.S. Environmental Protection Agency, Research 
Triangle Park, NC 27711.
    5. Farthing and Dawes, 1988b ``Application Guide for Source 
PM<INF>10</INF> Measurement with Constant Sampling Rate,'' EPA/600/
3-88-057, U.S. Environmental Protection Agency, Research Triangle 
Park, NC 27711.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

    You must use the following tables, diagrams, flowcharts, and 
data to complete this test method successfully.

           Table 1--Typical Particulate Matter Concentrations
------------------------------------------------------------------------
          Particle size range             Concentration and % by weight
------------------------------------------------------------------------
Total collectable particulate..........  0.015 gr/DSCF.
<= 10 and > 2.5 micrometers............  40% of total collectable
                                          particulate matter.
<= 2.5 micrometers.....................  20% of total collectable
                                          particulate matter.
------------------------------------------------------------------------


[[Page 12992]]


              Table 2--Required Cyclone Cut Diameters (D50)
------------------------------------------------------------------------
                                             Min. cut        Max. cut
                 Cyclone                     diameter        diameter
                                           (Micrometer)    (Micrometer)
------------------------------------------------------------------------
PM10 Cyclone (Cyclone I from five stage                9              11
 cyclone)...............................
PM2.5 Cyclone (Cyclone IV from five                 2.25            2.75
 stage cyclone).........................
------------------------------------------------------------------------


                      Table 3--Pretest Calculations
------------------------------------------------------------------------
                                 To calculate . .
    If you are using . . .              .              Then use . . .
------------------------------------------------------------------------
Preliminary data..............  dry gas molecular  Equation 1.
                                 weight, Md.
Dry gas molecular weight (Md)   wet gas molecular  Equation 2 \a\.
 and preliminary moisture        weight, MW.
 content of the gas stream.
Stack gas temperature, and      gas viscosity,     Equation 3.
 oxygen and moisture content     [mu].
 of the gas stream.
Gas viscosity, [mu]...........  Cunningham         Equation 4.
                                 correction
                                 factor \b\, C.
Reynolds Number \c\ (Nre).....  preliminary lower  Equation 5.
Nre < 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     Equation 7.
                                 rate for cyclone
                                 I, QI(Qs).
QI(Qs) from Equation 7........  (verify) the       Equation 8.
                                 assumed Reynolds
                                 number.
------------------------------------------------------------------------
\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 9.


       Table 4--[Delta]H Values Based on Preliminary Traverse Data
------------------------------------------------------------------------
                                                                 Ts +
    Stack temperature ([deg]R)      Ts-50[deg]       Ts        50[deg]
------------------------------------------------------------------------
[Delta]H, (in. W.C.).............            -            -            -
------------------------------------------------------------------------


          Table 5--Verification of the Assumed Reynolds Number
------------------------------------------------------------------------
       If the Nre is . . .            Then . . .           And . . .
------------------------------------------------------------------------
< 3,162.........................  Calculate [Delta]H
                                   for the meter box.
>= 3,162........................  Recalculate D50LL   Substitute the
                                   using Equation 10.  ``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 27 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 in.
                                          Hg).
Dry gas sampling rate (QsST)...........  Must be calculated using
                                          Equation 28.
Volume of water condensed (Vws)........  Use Equation 29 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 with Equation
                                          30.
Sampling rate (Qs).....................  Calculate this with Equation
                                          31.
Test condition Reynolds number\a\......  Use Equation 8 to calculate the
                                          actual Reynolds number during
                                          test conditions.
Actual D50 of Cyclone I................  Calculate this with Equation
                                          32. This calculation is based
                                          on the average temperatures
                                          and pressures measured during
                                          the test run.
Stack gas velocity (vs)................  Calculate this with Equation
                                          11.
Percent isokinetic rate (%I)...........  Calculate this with Equation
                                          40.
------------------------------------------------------------------------
\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.


[[Page 12993]]

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[[Page 12994]]

[GRAPHIC] [TIFF OMITTED] TP25MR09.051


[[Page 12995]]

[GRAPHIC] [TIFF OMITTED] TP25MR09.052


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BILLING CODE 6560-50-C

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METHOD 202--DRY IMPINGER METHOD FOR DETERMINING CONDENSABLE PARTICULATE 
EMISSIONS FROM STATIONARY SOURCES

1.0 Scope and Applicability

    1.1 Scope. The U.S. Environmental Protection Agency (U.S. EPA or 
``we'') developed this method to describe the procedures that the 
stack tester (``you'') must follow to measure condensable 
particulate matter (CPM) emissions from stationary sources. This 
method includes procedures for measuring both organic and inorganic 
CPM.
    1.2 Applicability. You can use this method to measure CPM from 
stationary source emissions after filterable particulate matter has 
been removed. CPM is measured in the emissions after removal from 
the stack and after passing through a filter. You can use Method 17 
to collect condensable and filterable particulate material from 
sources operating at stack temperatures and/or samples collected 
below 30 [deg]C (85 [deg]F) if the filter is treated as described in 
Sections 8.5.4.4 and 11.2.1 of this method. You may use this method 
only for stationary source emission measurements.
    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 Results. To obtain reliable results, you must 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 
Part 51:
    (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 PM<INF>10</INF> and 
PM<INF>2.5</INF> Emissions from Stationary Sources (Constant 
Sampling Rate Procedure)
    1.5 Additional Methods. You will need additional test methods to 
measure filterable particulate matter. You may use this method to 
collect CPM in conjunction with Method 5 or 17 of Appendices A-1 
through A-3 and A-6 to Part 60 or, Method 201A of Appendix M to Part 
51. The sample train operation and front end recovery and analysis 
are conducted according to the filterable particulate method you 
choose. This method addresses the equipment, preparation, and 
analysis necessary to measure only CPM.
    1.6 Limitations. You can use this method to measure emissions 
following a wet scrubber only when this method is combined with a 
filterable particulate method that operates at high enough 
temperatures to cause water droplets sampled through the probe to 
become gaseous.
    1.7 Conditions. You must maintain isokinetic sampling conditions 
to meet the requirements of the filterable particulate method used 
in conjunction with this method. You must sample at the required 
number of sampling points specified in Method 5, 17, or 201A. Also, 
if you are using this method as an alternative to a required 
performance test method, you must receive approval from the 
appropriate authorities prior to conducting the test.

2.0 Summary of Method

    2.1 Summary. The CPM is collected in dry impingers after 
filterable particulate material has been collected on filters 
maintained above 30 [deg]C (85 [deg]F) using Method 5, 17, or 201A. 
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 
all fractions represents the CPM. Compared to the December 17, 1991 
promulgated Method 202, this method removes water from the 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 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 Particulate Matter. 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 (N<INF>2</INF>) 
immediately after sample collection to remove dissolved sulfur 
dioxide (SO<INF>2</INF>) gases from the impinger. The CPM filter is 
extracted with water and methylene chloride. The impinger solution 
is then extracted with methylene chloride (MeCl<INF>2</INF>). 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 SO<INF>2</INF> are reduced using a condenser and 
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 Primary PM. 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.
    3.2 Filterable PM. 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.
    3.3 Primary PM<INF>10</INF>. Primary PM<INF>10</INF> (also known 
as direct PM<INF>10</INF>, total PM<INF>10</INF>, PM<INF>10</INF> or 
filterable PM<INF>10</INF>, and condensable PM, individually) means 
particulate matter with an aerodynamic diameter equal to or less 
than 10 micrometers.
    3.4 Primary PM<INF>2.5</INF>. Primary PM<INF>2.5</INF> (also 
known as direct PM<INF>2.5</INF>, total PM<INF>2.5</INF>, 
PM<INF>2.5</INF>, or filterable PM<INF>2.5</INF>, and condensable 
PM, individually) means solid particles emitted directly from an air 
emissions source or activity, or gaseous emissions or liquid 
droplets from an air emissions source or activity that condense to 
form particulate matter at ambient temperatures. Direct 
PM<INF>2.5</INF> 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).
    3.5 Condensable PM (CPM). Condensable PM means material that is 
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. Note that all 
condensable PM is assumed to be in the PM<INF>2.5</INF> size 
fraction (Reference: Part 51, Subpart Z (51.1000)).

4.0 Interferences [Reserved]

5.0 Safety

    Disclaimer: You may have to use hazardous materials, operations, 
and equipment while performing this method. We do not provide 
information on appropriate safety and health practices. You are 
responsible for determining the applicability of regulatory 
limitations and establishing appropriate safety and health 
practices. Handle materials and equipment properly.

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 in Appendix M to Part 
51. 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 consistent with the sampling train 
for collecting filterable particulate using Method 5, 17, or 201A 
with the following exceptions or additions:
    6.1.1 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 dropout impinger or flask, 
followed by a modified Greenburg-Smith impinger with an open tube 
tip as described in Section 6.1.1.8 of Method 5.
    6.1.2 CPM Filter Holder. The modified Greenburg-Smith impinger 
is followed by a filter holder that is either glass, stainless steel 
(316 or equivalent), or Teflon[supreg]-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 Teflon[supreg] O-ring, stainless steel, ceramic or 
Teflon[supreg] filter support and a final Teflon[supreg] O-ring. At 
the exit of the CPM filter, install a Teflon[supreg]-coated or 
stainless steel encased thermocouple that is in contact with the gas 
stream.
    6.1.3 Long Stem Impinger Insert. You will need a long stem 
modified Greenburg Smith

[[Page 13004]]

impinger insert for the dropout impinger to perform the nitrogen 
purge of the sampling train.
    6.2 Sample Recovery Equipment.
    6.2.1 Condensable Particulate Matter Recovery.
    6.2.1.1 Nitrogen Purge Line. You must use inert tubing and 
fittings capable of delivering at least 20 liters/min of nitrogen 
gas to the impinger train from a standard gas cylinder (see Figure 2 
of Section 18). You may use standard 0.6 cm (1/4-in.) tubing and 
compression fittings in conjunction with an adjustable pressure 
regulator and needle valve.
    6.2.1.2 Rotameter. You must use a rotameter capable of measuring 
gas flow up to 20 L/min. The rotameter must be accurate to 5 percent 
of full scale.
    6.2.1.3 Ultra-high Purity (UHP) Nitrogen Gas. Compressed ultra-
pure nitrogen, regulator, and filter must be capable of providing at 
least 20 L/min purge gas for 1 hour through the sampling train.
    6.3 Analysis. The following equipment is necessary for CPM 
sample recovery and analysis:
    6.3.1 Separatory Funnel. Glass, 1 liter.
    6.3.2 Weighing Tins. 50 mL.
    6.3.3 Glass Beakers. 300 to 500 mL.
    6.3.4 Drying Equipment. Hot plate or oven with temperature 
control.
    6.3.5 Pipets. 5 mL.
    6.3.6 Burette. Glass, 0 to 100 mL in 0.1 mL graduations.
    6.3.7 Analytical Balance. Analytical balance capable of weighing 
0.0001 g (0.1 milligram). For extremely low emission sources, a 
balance capable of weighing 0.00001 g (0.01 milligram) may be 
required.
    6.3.8 pH Meter. A meter capable of determining the acidity of 
liquid within 0.1 pH units.

7.0 Reagents and Standards

    7.1 Sample Collection. To collect a sample, you will need a 
Teflon[supreg] 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 Filter. You must use a Teflon[reg] membrane filter that 
does not have an organic binder. The filter must also have an 
efficiency of at least 99.95 percent (<0.05 percent penetration) on 
0.3 micron particles. You may use test data from the supplier's 
quality control program to document filter efficiency. If the source 
you are sampling has SO<INF>2</INF> or sulfur trioxide 
(SO<INF>3</INF>) emissions, then you must use a filter that will not 
react with SO<INF>2</INF> or SO<INF>3</INF>. Depending on your 
application and project data quality objectives (DQOs), filters are 
commercially available in 47 mm and larger sizes.
    7.1.2 Silica Gel. Use an indicating-type silica gel of 6 to 16 
mesh. We must approve other types of desiccants (equivalent or 
better) before you use them. Allow the silica gel to dry for 2 hours 
at 175 [deg]C (350 [deg]F) if it is being reused. You do not have to 
dry new silica gel.
    7.1.3 Water. Use deionized distilled ultra-filtered water (to 
conform to ASTM D1193-06, Type 1 water or equivalent) (incorporated 
by reference) to recover material caught in the impinger, if 
required. The Director of the Federal Register approves this 
incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 
CFR part 51. You may obtain a copy from American Society for Testing 
and Materials (ASTM), 100 Barr Harbor Drive, Post Office Box C700, 
West Conshohocken, PA 19428-2959. You may inspect a copy at the 
Office of Federal Register, 800 North Capitol Street, NW., Suite 
700, Washington, DC.
    7.1.4 Crushed Ice. Obtain from the best readily available 
source.
    7.1.5 Nitrogen Gas. Use Ultra-High Purity (UHP) 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 ppm oxygen, 1 ppm total hydrocarbons as carbon, and 2 ppm 
moisture.
    7.2 Sample Recovery and Analytical Reagents. You will need 
acetone, MeCl<INF>2</INF>, anhydrous sodium sulfate, ammonia 
hydroxide (NH<INF>4</INF>OH), 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. 
Find additional information on each of these items 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 residue blank. You must use acetone with blank values <1 ppm, 
by weight, residue.
    7.2.2 Methylene Chloride, American Chemical Society (ACS) grade. 
You must use methylene chloride with a blank value <1.5 ppm, by 
weight, residue.
    7.2.3 Water. Use deionized distilled ultra-filtered water (to 
conform to ASTM D1193-06, Type 1 or equivalent) (incorporated by 
reference) to recover material caught in the impinger.
    7.2.4 Condensable Particulate Sample Desiccant. Use indicating-
type anhydrous sodium sulfate to desiccate water and organic extract 
residue samples.
    7.2.5 Ammonium Hydroxide. Use NIST traceable or equivalent (0.1 
N) NH<INF>4</INF>OH.
    7.2.6 Standard Buffer Solutions. Use one buffer with a neutral 
pH and a second buffer solution with an acid pH.

8.0 Sample Collection, Preservation, Storage, and Transport

    8.1 Qualifications. This is a complex test method. To obtain 
reliable results, you must 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 glassware prior to field tests 
as described in Section 8.4, including baking glassware at 300 
[deg]C for 6 hours prior to use. Cleaned, baked glassware is used at 
the start of each new source category tested. Analyze reagent blanks 
(water, acetone, and methylene chloride) 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 by 
filterable particulate sampling method setup run in conjunction with 
this method including:
    (a) Determining the sampling site location and traverse points.
    (b) Calculating probe/cyclone blockage.
    (c) Verifying the absence of cyclonic flow.
    (d) Completing a preliminary velocity profile, and selecting a 
nozzle(s).
    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. Then you must do all of 
the following:
    8.3.1.1 Sampling site. Choose a location that maximizes the 
distance from upstream and downstream flow disturbances.
    8.3.1.2 Traverse points. Use the recommended maximum 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 
(\1/2\ 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 
sampling train glassware must be cleaned prior to the test with soap 
and water, and rinsed using tap water, deionized water, acetone, and 
finally, MeCl<INF>2</INF>. It is important to completely remove all 
silicone grease from areas that will be exposed to the 
MeCl<INF>2</INF> rinse during sample recovery. After cleaning, you 
must bake glassware at 300 [deg]C for 6 hours prior to each source 
type sampled. Prior to each sampling run, the train glassware used 
to collect condensable particulate matter must be rinsed thoroughly 
with deionized, distilled ultra-filtered water that conforms to ASTM 
D1193-06, Type 1 or equivalent (incorporated by reference).
    8.4.1 Condenser and Dropout Impinger. Add a Method 23 type 
condenser and a condensate dropout impinger without bubbler tube 
after the final in-stack or out-of-stack hot filter assembly. The 
Method 23 type stack gas condenser is described in Section 2.1.2 of 
Method 23. It must be capable of cooling the stack gas to less than 
30 [deg]C (85 [deg]F).
    8.4.2 Backup Impinger. The dropout impinger is followed by a 
modified Greenburg Smith impinger with no taper (see Figure 1 of 
Section 18). Place the dropout and other impingers in an insulated 
box with water at <= 30 [deg]C (<= 85 [deg]F). At the start of the 
tests, the water dropout and backup impinger 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 6.1.2 following the modified Greenburg-
Smith impinger. The connection between the CPM filter and the 
moisture trap impinger includes 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

[[Page 13005]]

Teflon[reg] or steel encased thermocouple must be in contact with 
the sample gas).]

    8.4.4 Moisture Traps. You must use a modified Greenburg-Smith 
impinger containing 100 mL of water or the alternative described in 
Method 5 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, 17, or 201A 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 (ACFM) 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, 17, or 201A) 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 <=30 [deg]C (<=85 
[deg]F) during sample collection.
    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 ACFM or 4 percent of the average sampling rate during 
the test run (whichever is less), then the run is invalid and you 
must repeat it.
    8.5.3 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. Leave the ice 
in the second impinger box 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).
    8.5.3.1 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).
    8.5.3.2 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. If insufficient water 
was collected, you must add a measured amount of degassed deionized, 
distilled ultra-filtered ASTM D1193-06, Type 1 or equivalent) 
(incorporated by reference) water until the impinger tip is at least 
1 cm below the surface of the water. You must record the amount of 
water added to the dropout impinger (see Figure 4 of Section 18) to 
correct the moisture content of the effluent gas.

    (Note: Prior to use, water must be degassed using a nitrogen 
purge bubbled through the water for at least 15 minutes to remove 
dissolved oxygen).

    8.5.3.3 With no flow of gas through the clean purge line and 
fittings, attach the line to a purged inline filter. 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 nitrogen delivery rates to obtain the following 
conditions: (1) 20 liters/min or [Delta]H@, and (2) a positive 
overflow rate through the rotameter of less than 2 liters/min. 
Condition (2) 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. During the purge, 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 below 30 [deg]C (85 [deg]F). Continue the purge 
under these conditions for 1 hour, checking the rotameter and 
[Delta]H value(s) periodically. After 1 hour, 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. Measure the 
liquid in the first 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 book.
    8.5.4 Sample Recovery.
    8.5.4.1 Recovery of Filterable Particulate Matter. Recovery of 
filterable particulate matter involves the quantitative transfer of 
particles according to the filterable particulate sampling method 
(i.e., Method 5, 17 or 201A).
    8.5.4.2 CPM Container <greek-i>1, Aqueous Liquid Impinger 
Contents. Quantitatively transfer liquid from the dropout and the 
impinger prior to the CPM filter into a clean sample bottle (glass 
or plastic). 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 add it to the 
same sample bottle. Mark the liquid level on the bottle. CPM 
Container <greek-i>1 holds the water soluble CPM captured in the 
impingers.
    8.5.4.3 CPM Container <greek-i>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. Then repeat the entire procedure with two 
rinses of MeCl<INF>2</INF>, and save both solvents in a separate 
glass container identified as CPM Container <greek-i>2. Mark the 
liquid level on the jar.
    8.5.4.4 CPM Container <greek-i>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 identified as CPM Container <greek-i>3.
    8.5.4.5 CPM Container <greek-i>4, Cold Impinger Water. You must 
weigh or measure the volume of the contents of CPM Container 
<greek-i>4 either in the field or during sample analysis (see 
Section 11.2.3). 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 sample bottle (glass or plastic). Mark the liquid level 
on the bottle. This container holds the remainder of the liquid 
water from the emission gases.
    8.5.4.6 CPM Container <greek-i>5, Silica Gel Absorbent. You must 
weigh the contents of CPM Container <greek-i>5 in the field or 
during sample analysis (see Section 11.2.4). If the silica gel has 
been weighed in the field to measure water content, then it can be 
discarded. Otherwise, transfer the silica gel to its original 
container 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.
    8.5.4.7 CPM Container <greek-i>6, Acetone Rinse Blank. Take 150 
mL of the acetone directly from the wash bottle you used, and place 
it in CPM Container <greek-i>6, labeled Acetone Rinse Blank (see 
Section 11.2.5 for analysis). Mark the liquid level on the bottle.
    8.5.4.8 CPM Container <greek-i>7, Water Rinse Blank. Take 150 mL 
of the water directly from the wash bottle you used, and place it in 
CPM Container <greek-i>7, labeled Water Rinse Blank (see Section 
11.2.6 for analysis). Mark the liquid level on the bottle.
    8.5.4.9 CPM Container <greek-i>8, Methylene Chloride Rinse 
Blank. Take 150 mL of the MeCl<INF>2</INF> directly from the wash 
bottle you used, and place it in CPM Container <greek-i>8, labeled 
Methylene Chloride Rinse Blank (see

[[Page 13006]]

Section 11.2.7 for analysis). Mark the liquid level on the bottle.
    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 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 Health and Safety Plan. Develop a health and safety plan to 
ensure the safety of your employees who are on-site conducting the 
particulate emission test. Your plan must conform with all 
applicable Occupational Safety and Health Administration (OSHA), 
Mine Safety and Health Administration (MSHA), and Department of 
Transportation (DOT) regulatory requirements. The procedures must 
also conform to the plant health and safety requirements.
    9.5 Calibration Checks. Perform calibration check procedures on 
analytical balances each time they are used.
    9.6 Glassware. Use class A volumetric glassware for titrations, 
or calibrate your equipment against National Institute of Standards 
and Technology (NIST) traceable glassware.
    9.7 Analytical Balance. Check the calibration of your analytical 
balance each day 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.
    9.8 Reagent Blanks. You must run blanks of water, acetone, and 
methylene chloride used for field recovery and sample analysis. 
Analyze at least one sample (100 mL minimum) of each reagent that 
you plan to use for sample recovery and analysis before you begin 
testing. Running blanks before field use will verify low blank 
concentrations, thereby reducing the potential for a high field 
blank on test samples.
    9.9 Field Reagent Blanks. You must run at least one field blank 
of water, acetone, and methylene chloride you use for field 
recovery. Running independent reagent field blanks will verify that 
low blank concentrations were maintained during field solvent use 
and demonstrate that reagents have not been contaminated during 
field tests.
    9.10 Field Train Blank. You must recover a minimum of one field 
train blank for each set of compliance tests at the facility. 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 3. You must purge the 
assembled train as 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.
    9.11 Audit Procedure. Concurrent with compliance sample 
analysis, and if available, analyze audit material to evaluate the 
technique of the analyst and the standards preparation. Use the same 
staff, analytical reagents, and analytical system for both 
compliance samples and the EPA audit sample. If this condition is 
met, auditing of subsequent compliance analyses for the same 
enforcement agency within 30 days is not required. An audit sample 
set may not be used to validate different sets of compliance samples 
under the jurisdiction of different enforcement agencies, unless 
prior arrangements are made with both enforcement agencies.
    9.12 Audit Samples. As of the publication date of this test 
method, audit materials are not available. If audit materials become 
available, audit samples will be supplied only to enforcement 
agencies for compliance tests. Audit samples can be requested by a 
State agency. Audit materials are requested online by authorized 
regulatory authorities at the following internet address: http://www.sscap.net/. Authorization can be obtained by contacting an EPA 
Emission Measurement Center QA Team Member listed on the EPA TTN Web 
site at the following internet address: http://www.epa.gov/ttn/emc/email.html#qaqc. The request for the audit sample must be made at 
least 30 days prior to the scheduled compliance sample analysis.
    9.13 Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit 
sample concentration and the analyst's name on the audit response 
form included with the audit instructions. Send one copy to the EPA 
Regional Office or the appropriate enforcement agency.

10.0 Calibration and Standardization

    Maintain a log 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 10.1.4.1.2 
of Method 2 of Appendix A-1 to Part 60. Calibrate each temperature 
sensor at a minimum of three points over the anticipated range of 
use against an NIST-traceable mercury-in-glass thermometer.
    10.2 Ammonium Hydroxide. The 0.1 N NH<INF>4</INF>OH used for 
titrations in this method is made as follows: Add 7 mL of 
concentrated (14.8 M) NH<INF>4</INF>OH to l liter of water. 
Standardize against standardized 0.1 N H<INF>2</INF>SO<INF>4</INF>, 
and calculate the exact normality using a procedure parallel to that 
described in Section 5.5 of Method 6 of Appendix A-4 to 40 CFR part 
60. Alternatively, purchase 0.1 N NH<INF>4</INF>OH that has been 
standardized against a NIST reference material. Record the normality 
on the Condensable Particulate Matter Work Table (see Figure 5 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 (ERT), available at the following internet address: 
http://www.epa.gov/ttn/chief/ert/ert_tool.html. Record the 
condensable particulate data on the Condensable Particulate Matter 
Work Table (see Figure 5 of Section 18).
    (b) Measure the liquid in all containers either volumetrically 
to <plus-minus> 1 mL or gravimetrically to <plus-minus> 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 Particulate Matter Analysis. See the flow chart 
in Figure 6 of Section 18 for the steps to process and combine 
fractions from the CPM train.
    11.2.1 Container <greek-i>3, CPM Filter Sample. 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. If the sample 
was collected by Method 17 because the stack temperature was below 
30 [deg]C (85 [deg]F), process the filter extracts as described in 
this section without combination with any other portion from the 
train.
    11.2.1.1 Extract the water soluble (aqueous or inorganic) CPM 
from the CPM filter as described in this section. Fold the CPM 
filter in quarters, and place 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 2 minutes. 
Combine the aqueous extract with the contents of Container 
<greek-i>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 as 
described in this section. Add sufficient methylene chloride to 
cover the filter (e.g., 10 mL of water). Place the extractor tube 
into a sonication bath and extract the organic soluble material for 
a minimum of 2 minutes. Combine the organic extract with the 
contents of Container <greek-i>2. Repeat this extraction step twice 
for a total of three extractions.

[[Page 13007]]

    11.2.2 CPM Container <greek-i>1, Aqueous Liquid Impinger 
Contents. Analyze the water soluble CPM in Container 1 as described 
in this section. Place the contents of Container <greek-i>1 into a 
separatory funnel. Add approximately 30 mL of MeCl<INF>2</INF> to 
the funnel, mix well, and drain off the lower organic phase. Repeat 
this procedure twice with 30 mL of MeCl<INF>2</INF> each time 
combining the organic phase from each extraction. Each time, leave a 
small amount of the organic/MeCl<INF>2</INF> 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.
    11.2.2.1 CPM Container <greek-i>2. Combine the organic extract 
from Container <greek-i>1 with the organic train rinse in Container 
2.
    11.2.2.2 Organic Fraction Weight Determination. 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 50-mL preweighed 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 6 hours to a constant weight (i.e., <= 0.5 mg change 
from previous weighing), and report results to the nearest 0.1 mg on 
the Condensable Particulate Matter Work Table (see Figure 5 of 
Section 18).
    11.2.2.3 Inorganic Fraction Weight Determination. 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. Redissolve the residue in 100 mL of 
deionized distilled ultra-filtered water (ASTM D1193-06, Type 1 
water or equivalent) (incorporated by reference).
    11.2.2.4 Use titration to neutralize acid in the sample and 
remove water of hydration. Calibrate the pH meter with the neutral 
and acid buffer solutions; then titrate the sample with 0.1N 
NH<INF>4</INF>OH to a pH of 7.0, as indicated by the pH meter. 
Record the volume of titrant used on the Condensable Particulate 
Matter Work Table (see Figure 5 of Section 18).
    11.2.2.5 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 50-mL preweighed 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 6 hours to a 
constant weight (i.e., <= 0.5 mg change from previous weighing), and 
report results to the nearest 0.1 mg on the Condensable Particulate 
Matter Work Table (see Figure 5 of Section 18).
    11.2.2.6 Calculate the correction factor to subtract the 
NH4<SUP>+</SUP> retained in the sample using Equation 1 in Section 
12.
    11.2.3 CPM Container <greek-i>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 <greek-i>4 either volumetrically to <plus-minus> 1 mL or 
gravimetrically to <plus-minus> 0.5 g, and record the volume or 
weight on the filterable particulate analytical data sheet of the 
filterable particulate matter test method.
    11.2.4 CPM Container <greek-i>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 particulate matter test method.
    11.2.5 Container <greek-i>6, Acetone Field Rinse Blank. Use 100 
mL of acetone from the blank container for this analysis. If 
insufficient liquid is available or if the acetone has been lost due 
to container breakage, either void the sample, or use methods, 
subject to the approval of the Administrator, to correct the final 
results. Transfer 100 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 the beaker contents to a 50-mL 
preweighed 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 6 hours to a constant weight (i.e., <= 0.5 mg change 
from previous weighing), and report results to the nearest 0.1 mg on 
Figure 3.
    11.2.6 Water Rinse Field Blank, Container <greek-i>7. Use 100 mL 
of the water from the blank container for this analysis. If 
insufficient liquid is available, or if the water has been lost due 
to container breakage, either void the sample, or use methods, 
subject to the approval of the Administrator, to correct the final 
results. 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 preweighed 
50-mL 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 6 hours to a constant weight (i.e., <= 0.5 mg change 
from previous weighing) and report results to the nearest 0.1 mg on 
Figure 3.
    11.2.7 Methylene Chloride Field Reagent Blank, Container 
<greek-i>8. Use 100 mL of MeCl<INF>2</INF> from the blank container 
for this analysis. Transfer 100 mL of the MeCl<INF>2</INF> to a 
clean 250-mL beaker. Evaporate the methylene chloride 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 50-mL preweighed 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 6 hours to a constant weight 
(i.e., <= 0.5 mg change from previous weighing), and report results 
to the nearest 0.1 mg on Figure 3.

12.0 Calculations and Data Analysis

    12.1 Nomenclature. Report results in International System of 
Units (SI units) unless the regulatory authority for compliance 
testing specifies English units. The following nomenclature is used.

[Delta]H<INF>@</INF> = Pressure drop across orifice at flow rate of 
0.75 SCFM at standard conditions, in. W.C.

    [Note: specific to each orifice and meter box.]

17.03 = mg/milliequivalents for ammonium ion.
ACFM = Actual cubic feet per minute.
C<INF>cpm</INF> = Concentration of the condensable particulate 
matter in the stack gas, dry basis, corrected to standard 
conditions, milligrams/dry standard cubic foot.
m<INF>c</INF> = Mass of the NH<INF>4</INF><SUP>+</SUP> added to 
sample to form ammonium sulfate, mg.
m<INF>cpm</INF> = Mass of the total condensable particulate matter, 
mg.
m<INF>fb</INF> = Mass of field train total CPM blank, mg
m<INF>i</INF> = Mass of inorganic CPM matter, mg.
m<INF>ib</INF> = Mass of field train inorganic CPM blank, mg.
m<INF>o</INF> = Mass of organic CPM, mg.
m<INF>ob</INF> = Mass of organic field train blank, mg.
m<INF>r</INF> = Mass of dried sample from inorganic fraction, mg.
N = Normality of ammonium hydroxide titrant.
V<INF>m(std)</INF> = 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.
V<INF>t</INF> = Volume of NH<INF>4</INF>OH titrant, mL.
V<INF>p</INF> = 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 Condensable Particulate 
Matter Work Table (see Figure 5 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.
[GRAPHIC] [TIFF OMITTED] TP25MR09.045

    12.2.2 Mass of the Field Blank (mg). Per Section 9.9, the mass 
of the field blank, m<INF>fb</INF>, shall not exceed 2.0 mg.
[GRAPHIC] [TIFF OMITTED] TP25MR09.046

    12.2.3 Mass of Inorganic CPM (mg).
    [GRAPHIC] [TIFF OMITTED] TP25MR09.047
    
    12.2.4 Total Mass of CPM (mg).
    [GRAPHIC] [TIFF OMITTED] TP25MR09.048
    
    12.2.5 Concentration of CPM (mg/dscf).

[[Page 13008]]

[GRAPHIC] [TIFF OMITTED] TP25MR09.049

    12.3 Emissions Test Report. Include the following list of 
conventional elements in the emissions test report.
    (a) Emission test description including any deviations from this 
protocol.
    (b) Summary data tables on a run-by-run basis that include the 
condensable particulate mass.
    (c) Flowchart of the process or processes tested.
    (d) Sketch of the sampling location.
    (e) Preliminary traverse data sheets including cyclonic flow 
checks.
    (f) Raw field data sheets and copies of field log pages.
    (g) Laboratory analytical sheets and case narratives.
    (h) Pretest and post test reagent blank results.
    (i) Sample calculations.
    (j) Pretest and post-test calibration data.
    (k) Chain of custody forms.
    (l) Documentation of process and air pollution control system 
data.

13.0 Method Performance [Reserved]

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 [Reserved]

17.0 References

    1. 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.
    2. Richards, J., T. Holder, and D. Goshaw. ``Optimized Method 
202 Sampling Train to Minimize the Biases Associated with Method 202 
Measurement of Condensable Particulate Matter Emissions.'' Paper 
presented at Air & Waste Management Association Hazardous Waste 
Combustion Specialty Conference. St. Louis, Missouri. November 2-3, 
2005.
    3. DeWees, W.D., S.C. Steinsberger, G.M. Plummer, L.T. Lay, G.D. 
McAlister, and R.T. Shigehara. ``Laboratory and Field Evaluation of 
the 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. DeWees, W.D. and K.C. Steinsberger. ``Method Development and 
Evaluation of Draft Protocol for Measurement of Condensable 
Particulate Emissions.'' Draft Report. November 17, 1989.
    5. Texas Air Control Board, Laboratory Division. ``Determination 
of Particulate in Stack Gases Containing Sulfuric Acid and/or Sulfur 
Dioxide.'' Laboratory Methods for Determination of Air Pollutants. 
Modified December 3, 1976.
    6. Nothstein, Greg. Masters Thesis. University of Washington. 
Department of Environmental Health. Seattle, Washington.
    7. ``Particulate Source Test Procedures Adopted by Puget Sound 
Air Pollution Control Agency Board of Directors.'' Puget Sound Air 
Pollution Control Agency, Engineering Division. Seattle, Washington. 
August 11, 1983.
    8. Commonwealth of Pennsylvania, Department of Environmental 
Resources. 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.
    9. Wisconsin Department of Natural Resources. Air Management 
Operations Handbook, Revision 3. January 11, 1988.
    10. U.S. Environmental Protection Agency, ``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.
    11. U.S. Environmental Protection Agency, ``Evaluation and 
Improvement of Condensable Particulate Matter Measurement,'' EPA 
Contract No. EP-D-07-097, Work Assignment 2-03, October 2008.
    12. Electric Power Research Institute (EPRI), ``Laboratory 
Comparison of Methods to Sample and Analyze Condensable Particulate 
Matter,'' EPRI Agreement EP-P24373/C11811 Condensable Particulate 
Methods: EPRI Collaboration with EPA, October 2008.

[[Page 13009]]

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[[Page 13010]]


[GRAPHIC] [TIFF OMITTED] TP25MR09.061


[[Page 13011]]



    Figure 3--Field Train Blank Condensable Particulate Calculations
------------------------------------------------------------------------
 
------------------------------------------------------------------------
         Field Train Blank Condensable Particulate Calculations
------------------------------------------------------------------------
Plant
Date
Blank No.
CPM Filter No.
Water volume added to purge train (Vp)         ml
------------------------------------------------------------------------
                        Field Reagent Blank Mass
------------------------------------------------------------------------
Water (Section 11.2.6).......................  mg
Acetone (Section 11.2.5).....................  mg
Methylene Chloride (Section 11.2.7)..........  mg
------------------------------------------------------------------------
                     Field Train Reagent Blank Mass
------------------------------------------------------------------------
Mass of Organic CPM (mob)(Section 11.2.2.2)..  mg
Mass of Inorganic CPM (mib)(Equation 3)......  mg
Mass of the Field Train Blank (not to exceed   mg
 2.0 mg) (Equation 2).
------------------------------------------------------------------------



     Figure 4--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 5--Condensable Particulate Matter Work Table
    Calculations for Recovery of Condensable Particulate Matter (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.
    Was significant volume of                     ________  ............
     organic rinse lost during
     transport? Yes or No.
    If Yes, measure the volume                    ________  mL
     received. Estimate the volume
     lost during transport.
 
For Titration
    Normality of NH4OH (N) (Section               ________  N
     10.2).
    Volume of titrant (Vt) (Section               ________  mL
     11.2.2.4).
    Mass of NH4 added (mc) (Equation              ________  mg
     1).
 
For CPM Blank Weights
    Inorganic Train Field Blank                   ________  mg
     Mass(mib) (Section 9.9).
    Organic Train Field Blank Mass                ________  mg
     (mob) (Section 9.9).
    Mass of Train Field Blank (Mfb)               ________  mg
     (max. 2 mg) (Equation 2).
 
For CPM Train Weights
    Mass of Organic CPM (mo)                      ________  mg
     (Section 11.2.2.2).
    Mass of Inorganic CPM (mi)                    ________  mg
     (Equation 3).
    Total CPM Mass (mcpm) (Equation               ________  mg
     4).
------------------------------------------------------------------------


[[Page 13012]]

[GRAPHIC] [TIFF OMITTED] TP25MR09.062

 [FR Doc. E9-6178 Filed 3-24-09; 8:45 am]
BILLING CODE 6560-50-C


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