12970 Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 51 

[EPA–HQ–OAR–2008–0348; FRL–8784–5] 

RIN 2060–AO58 

Methods for Measurement of Filterable 

PM10 and PM2.5 and Measurement of 

Condensable Particulate Matter 

Emissions From Stationary Sources 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Proposed rule. 

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 (μm) (PM2.5 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 PM2.5 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: 

• http://www.regulations.gov. Follow 

the on-line instructions for submitting 

comments. 

• E-mail: Send your comments via 

electronic mail to a-and-rdocket@epa.gov. 

• Fax: (202) 566–9744. 

• Mail: Methods for Measurement of 

Filterable PM10 and PM2.5 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. 

• 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 PM10 and PM2.5 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, email address: mozingo.kristal@epa.gov. 

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: sorrell.candace@epa.gov. For 

technical questions, contact Mr. Ron 

Myers, U.S. EPA, Office of Air Quality 

Planning and Standards, Sector Policies 

and Programs Division, Measurement 

Policy Group (D243–05), Research 

Triangle Park, NC 27711; telephone 

number: (919) 541–5407; fax number: 

(919) 541–1039; e-mail address: 

myers.ron@epa.gov. 

SUPPLEMENTARY INFORMATION: 


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Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 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 PM10 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 PM2.5 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: 

Category SIC 1

code 

NAICS2

code Examples of potentially 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 

1Standard 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 


PWALKER on PROD1PC71 with PROPOSALS3
12972 Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 

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)): 

• Method 201A—Determination of 

PM10 Emissions (Constant Sampling 

Rate Procedure), and 

• 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 highvolume sampler, which collects PM up 

to a nominal size of 25 to 45 μm 

(referred to as total suspended 

particulates or TSP). On October 2, 1979 

(44 FR 56730), EPA announced the first 

periodic review of the air quality criteria 

and 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 μm 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 μm), and using PM10 as the 

indicator for purposes of regulating the 

coarse fraction of PM10. 

Following promulgation of the 1997 

PM NAAQS, petitions for review were 

filed by a large number of parties, 

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 


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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 μg per 

cubic meter (μg/m3), retained the level 

of the annual PM2.5 annual standard at 

15 μg/m3, and revised the form of the 

annual PM2.5 standard by narrowing the 

constraints on the optional use of spatial 

averaging. With regard to the primary 

and secondary standards for PM10, EPA 

retained the 24-hour PM10 standard (150 

μg/m3) and revoked the annual standard 

because available evidence generally 

did not suggest a link between long-term 

exposure to current ambient levels of 

coarse particles and health or welfare 

effects. 

C. Measuring PM Emissions 

Section 110 of the CAA, as amended 

(42 U.S.C. 7410), requires 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: 

• Method 201A—Determination of 

PM10 Emissions (Constant Sampling 

Rate Procedure), and 

• 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 μm 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 instack nozzle/cyclones and filter 

assembly in a small duct will cause 

significant cross-sectional area 

interference and blockage leading to 

incorrect flow calculation and particle 

size separation. Additionally, the type 

of metal used to construct the Method 

201A cyclone may limit the 

applicability of the method when 

sampling at high stack temperatures 

(e.g., stainless steel cyclones are 

reported to gall and seize at 

temperatures greater than 260 °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 SO2 before it can form sulfuric 

acid (this is our preferred application of 

the Method 202 optional procedures). 

Inappropriate use (or omission) of the 

preferred or optional procedures in 

Method 202 can increase the potential 

for artifact formation. 

Considering the potential for 

variations in measured CPM emissions, 

we believe that further verification and 

refinement of Method 202 is appropriate 

to minimize the potential for artifact 

formation. We 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 


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12974 Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 

present in stack gas and also provided 

guidance for analyzing the collected 

samples. In 2005, an EPA contractor 

conducted a second study (‘‘Laboratory 

Evaluation of Method 202 to Determine 

Fate of SO2 in Impinger Water’’) that 

replicated some of the earlier EPA work 

and addressed some additional issues. 

The report of that work is available 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 PM2.5 as an 

indicator of health and welfare effects 

by the 1997 NAAQS revisions generates 

the need to quantify PM2.5 emissions 

from stationary sources. To respond to 

this need, we are proposing revisions to 

incorporate this capability into the test 

method for filterable PM10. 

III. This Action 

This action proposes to provide the 

capability of measuring PM2.5 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, PM10, and 

PM2.5. 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 PM2.5

as the indicator. This action will modify 

the current Method 201A sampling train 

configuration to allow for measurement 

of filterable PM10, filterable PM2.5, or 

both filterable PM10 and filterable PM2.5

from stationary sources. These 

amendments combine the existing 

method with the PM2.5 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 PM2.5 cyclone would 

be inserted between the PM10 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 commerciallyavailable 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, 


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all of the collected material would be 

considered PM2.5. 

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 SO2 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 SO2 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: 

• 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 °C); 

• Installing a recirculation pump in 

the ambient water bath to supply 

cooling water to the condenser; 

• 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 °C) (the first 

dry impinger will use a short-stem 

insert, and the second dry impinger will 

use a long-stem insert); 

• 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 

• Requiring that the temperature of 

the sample gas drawn through the CPM 

filter be maintained at ambient 

temperature (less than 30 °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: 

• Extracting the CPM filter with water 

and organic solvent; 

• 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; 

• Evaporating the remaining liquid to 

dryness at ambient temperature prior to 

neutralization with ammonium 

hydroxide; 

• Titrating the reconstituted residue 

with 0.1 normal ammonium hydroxide 

and a pH meter; 

• Evaporating the neutralized liquid 

to a minimum volume of 10 milliliters 

in an oven or hot plate; 

• Evaporating the final volume to 

dryness at ambient temperature; and 

• 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 °C (221 °F), where 

the proposed revision requires the last 

10 ml of the water to be evaporated at 

room temperature (not to exceed 30 °C 

(85 °F)) thereby retaining the CPM that 

would evaporate at the increased 

temperature. 

Prior to our adoption of the 1997 

PM2.5 NAAQS, several State and local 

air pollution control agencies had 

developed emission inventories that 

included CPM. Additionally, some 

agencies established enforceable CPM 

emissions limits or otherwise required 

that PM emissions testing include 

measurement of CPM. While this 

approach was viable in cases where the 

same test method was used to develop 

the CPM regulatory limits and to 

demonstrate facility compliance, there 

are substantial inconsistencies within 

and between States regarding the 

completeness and accuracy of CPM 

emission inventories and the test 

methods used to measure CPM 

emissions and 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 


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the NAAQS, the determination of direct 

PM emissions may be biased high or 

low, depending on the test methods 

used to estimate PM emissions, and the 

atmospheric conversion of SO2 to 

sulfates (or SO3) may be inaccurate or 

double-counted. Additionally, some 

State and local regulatory authorities 

have assumed that EPA Method 5 of 

Appendix A–3 to 40 CFR Part 60 

(Determination of Particulate Matter 

Emissions from Stationary Sources) 

provides a reasonable estimate of PM10

emissions. This assumption is incorrect 

because Method 5 does not provide 

particle sizing of the filterable 

component and does not quantify 

particulate caught in the impinger 

portion of the sampling train. Similar 

assumptions for measurements of PM2.5

will result in greater inaccuracies. 

With regard to State permitting 

programs, we recognize that, in some 

cases, existing Best Available Control 

Technology (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 

PM2.5 that are needed to demonstrate 

attainment of the PM2.5 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) PM2.5

emissions data that are more 

representative of the emissions of each 

source in their areas. In the PM2.5 NSR 

Implementation Rule, we stated that as 

part of this test methods rulemaking, we 

would ‘‘take comment on an earlier 

closing date for the transition period in 

the NSR program if we are on track to 

meet our expectation to complete the 

test method rule much earlier than 

January 1, 2011.’’ 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 

PM2.5 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 PM2.5 emissions, particularly for 

CPM. As needed to demonstrate 

attainment of the PM NAAQS, we also 

expect States to address the control of 

direct PM2.5 emissions, including CPM, 

with any new actions taken after 

January 1, 2011 and to address CPM 

emissions in any direct PM2.5

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 


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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 

PM10 cyclone and the PM2.5 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 °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 °C (85 °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® 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 


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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 PM2.5 emissions is owned by 

a State or local government, those 

governments may incur a minimal 

compliance costs associated with 

conducting tests to quantify PM2.5

emissions using the revised methods 

when they are promulgated. However, 

such tests would be conducted at the 

discretion of the State or local 

government and the compliance costs 

are not expected to impose a significant 

burden on those governments. 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 PM2.5

emissions is owned by a tribal 

government, those governments may 

incur minimal compliance costs 

associated with conducting tests to 

quantify PM2.5 emissions using the 

revised methods when they are 

promulgated. However, such tests 

would be conducted at the discretion of 

the tribal government and the 

compliance costs are not expected to 

impose a significant burden on those 

governments. Thus, Executive Order 

13175 does not apply to this action. 


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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 

(PM10) and 2.5 micrometer (PM2.5). If the gas 

filtration temperature exceeds 30 °C (85 °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 °C (85 °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 °C (85 °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 instack 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. 


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(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 °C (85 °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 PM10 and PM2.5 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 °C 

(500 °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 PM2.5 particle sizer and the 

filter. In addition, to satisfy Method 5 and 

Method 17 criteria, you may need to sample 

from more than 12 traverse points. Be aware 

that this method determines in-stack PM10

and PM2.5 filterable emissions by sampling 

from a recommended maximum of 12 sample 

points, at a constant flow rate through the 

train (the constant flow is necessary to 

maintain the size cuts of the cyclones), and 

with a filter that is at the stack temperature. 

In contrast, Method 5 or Method 17 trains are 

operated isokinetically with varying flow 

rates through the train. Method 5 and Method 

17 require sampling from as many as 24 

sample points. Method 5 uses an out-of-stack 

filter that is maintained at a constant 

temperature of 120 °C (248 °F). Further, to 

use this method in place of Method 5 or 

Method 17, you must extend the sampling 

time so that you collect the minimum mass 

necessary for weighing 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 PM10 and 

PM2.5, 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 PM2.5 cyclone from a 

conventional five-stage cascade cyclone train. 

The addition of a PM2.5 cyclone between the 

PM10 cyclone and the stack temperature filter 

in the sampling train supplements the 

measurement of PM10 with the measurement 

of fine particulate matter. Without the 

addition of the PM2.5 cyclone, the filterable 

particulate portion of the sampling train may 

be used to measure total and PM10 emissions. 

Likewise, with the exclusion of the PM10

cyclone, the filterable particulate portion of 

the sampling train may be used to measure 

total and PM2.5 emissions. Figure 1 of Section 

17 presents the schematic of the sampling 

train configured with 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 PM10 and PM2.5 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 PM10 and PM2.5 sizing 

devices. The following sections describe the 

sampling train’s primary design features in 

detail. 

6.1 Filterable Particulate Sampling Train 

Components. 

6.1.1 Nozzle. You must use stainless steel 

(316 or equivalent) or Teflon®-coated 

stainless steel nozzles with a sharp tapered 

leading edge. We recommend one of the 12 

nozzles listed in Figure 3 of Section 17 

because they meet design specifications 

when PM10 cyclones are used as part of the 

sampling train. We also recommend that you 

have a large number of nozzles in small 

diameter increments available to increase the 

likelihood of using a single nozzle for the 

entire traverse. We recommend one of the 

nozzles listed in Figure 4A or 4B of Section 

17 because they meet design specifications 

when PM2.5 cyclones are used without PM10

cyclones as part of the sampling train. 

6.1.2 PM10 and PM2.5 Sizing Device. Use 

a stainless steel (316 or equivalent) PM10 and 

PM2.5 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 PM10 and PM2.5 sizing 

devices to within ±0.02 cm of the design 

specifications. Example suppliers of PM10

and PM2.5 sizing devices include the 

following: 

(a) Environmental Supply Company, Inc., 

2142 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®-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® O-ring, a stainless steel screen that 

supports the filter, and a final Teflon® Oring. 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 


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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®. 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® 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 (SO2) or sulfite 

(SO3) emissions, you must use a filter that 

will not react with SO2 or SO3. 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 °C (350 °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 PM10 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 crosssectional 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 Stype pitot tube. 

(b) Average the absolute values of the 

angles that have a null velocity pressure. Do 

not use the sampling location if the average 

absolute value exceeds 20°. 

[Note: You can minimize the effects of 

cyclonic flow conditions by moving the 

sampling location, placing gas flow 

straighteners upstream of the sampling 

location or applying a modified sampling 

approach as described in EPA Guideline 

Document 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 


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thermocouple to conduct the traverse. 

Conduct the preliminary traverse as close as 

possible to the anticipated testing time on 

sources that are subject to hour-by-hour gas 

flow rate variations of approximately ±20 

percent and/or gas temperature variations of 

approximately ±10 °C (±50 °F). 

[Note: You should be aware that these 

variations can cause errors in the cyclone cut 

diameters and the isokinetic sampling 

velocities.] 

8.3.4.2 Velocity pressure range. Insert the 

S-type pitot tube at each traverse point, and 

record the range of velocity pressures 

measured on data form in Method 2. 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 bulbdry bulb measurement or hand-held 

hygrometer measurement to estimate the 

moisture content of sources with gas 

temperatures less than 71 °C (160 °F).] 

8.3.4.4 Particulate matter concentration 

in the gas stream. Determine the particulate 

matter concentration for the PM2.5 and the 

PM2.5 to PM10 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 sizespecific emissions, and controlled sizespecific particulate emissions. 

8.4 Pre-test Calculations. You must 

perform pre-test calculations to help select 

the appropriate gas sampling rate through 

cyclone I (PM10) and cyclone IV (PM2.5). 

Choosing the appropriate sampling rate will 

allow you to maintain the appropriate 

particle cut diameters based upon 

preliminary gas stream measurements, as 

specified in Table 2 of Section 17. 

8.4.1 Gas Sampling Rate. The gas 

sampling rate is defined by the performance 

curves for both cyclones, as illustrated in 

Figure 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 °F. At lower 

temperatures, it may be necessary to perform 

the PM10 and PM2.5 separately in order to 

meet the necessary particle size criteria 

shown in Table 2 of Section 17.0.] 

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 (Nre) by 

substituting the sampling rate (Qs) calculated 

in Equation 7 into Equation 8. Then use 

Table 5 of Section 17 to determine if the Nre

used in Equation 5 was correct. 

8.5.2 Final Sampling Rate. Recalculate 

the final sampling rate (Qs) if the assumed 

Reynolds number used in your initial 

calculation is not correct. Use Equation 7 to 

recalculate the optimum sampling rate (Qs). 

8.5.3 Meter Box DH. Use Equation 9 to 

calculate the meter box DH 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 DH to maintain the correct 

constant cut diameters. Therefore, use 

Equation 9 to recalculate the DH values for 

50°F above and below the stack temperature 

measured during the preliminary traverse 

(see Section 8.3.4.1), and document this 

information in Table 4 of Section 17.] 

8.5.4 Choosing a Sampling Nozzle. Select 

one or more nozzle sizes to provide for near 

isokinetic sampling rate (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, vs, 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 Qs. 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, 

Rmin. Use Equation 15 to calculate the 

maximum nozzle/stack velocity ratio, Rmax. 

8.5.4.2 Minimum gas velocity. Use 

Equation 16 to calculate the minimum gas 

velocity (vmin) if Rmin is an imaginary number 

(negative value under the square root 

function) or if Rmin is less than 0.5. Use 

Equation 17 to calculate vmin if Rmin is greater 

than or equal to 0.5. 

8.5.4.3 Maximum stack velocity. Use 

Equation 18 to calculate the maximum stack 

velocity (vmax) if Rmax is less than 1.5. Use 

Equation 19 to calculate the stack velocity if 

Rmax is greater than or equal to 1.5. 

8.5.4.4 Conversion of gas velocities to 

velocity pressure. Use Equation 20 to convert 

vmin to minimum velocity pressure, Dpmin. 

Use Equation 21 to convert vmax to maximum 

velocity pressure, Dpmax. 

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 

Dpmin and Dpmax. Make sure the following 

requirements are met. Then follow the 

procedures in Sections 8.5.5.1 and 8.5.5.2. 

(a) Choose an optimum nozzle that 

provides for isokinetic sampling conditions 

as close to 100 percent as possible. This is 

prudent because even if there are slight 

variations in the gas flow rate, gas 

temperature, or gas composition during the 

actual test, you have the maximum assurance 

of satisfying the isokinetic criteria. Generally, 

one of the two candidate nozzles selected 

will be closer to optimum (see Section 8.5.4). 

(b) When testing is for PM2.5 only, you may 

have only two traverse points out of 12 that 

are outside the range of the Dpmin and Dpmax

(i.e., 16 percent failure rate rounded to the 

nearest whole number). If the coarse fraction 

for PM10 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® 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 


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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 Orings used in the train have a temperature 

limit of approximately 205 °C (400 °F). Use 

cyclones with stainless steel sealing rings 

when stack temperatures exceed 205 °C (400 

°F). This method may not be suitable for 

sources with stack gas temperatures 

exceeding 260 °C (500 °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 Stype 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 ± 5.6 °C (68 ± 10 

°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 °C (220 °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 °C (85 °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 (±10 °C, ±50 °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 °C (50 °F) of the 

temperature used to calculate DH. If stack 

temperatures vary by more than 28 °C (50 °F), 

use the appropriate DH value calculated in 

Section 8.5.3. Determine the minimum 

number of traverse points as in Figure 7 of 

Section 17. Determine the minimum total 

projected sampling time (tr), 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, 

t1, using Equation 22. You must use the data 

from the preliminary traverse. Here, Ntp

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, tn, 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 (bf) 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 

PM10 cyclone, PM2.5 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 

(Dps2) 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 °C (50 °F) 


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of the temperature used to calculate DH. If 

stack temperatures vary by more than 28 °C 

(50 °F), use the appropriate DH value 

calculated in Section 8.5.3. Calculate the 

dwell time at each traverse point as in 

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 (± 10 °C, 

± 50 °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 DH 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 nonrepresentative 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, ≤ PM2.5 micrometer 

filterable particulate—Use tweezers and/or 

clean disposable surgical gloves to remove 

the filter from the filter holder. Place the 

filter in the petri dish that you identified as 

Container #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 instack filter. 

(b) Container #2, > PM10 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 > 2.5 micrometers—Place the 

solids from cyclone cup IV and the acetone 

(and brush cleaning) rinses of the cyclone I 

turnaround cup (above inner downcomer 

line), inside of the downcomer line, and 

interior surfaces of cyclone IV into Container 

#3. Seal the container and mark the liquid 

level on the outside. This container holds 

particulate matter ≤ 10 micrometers but > 2.5 

micrometers. 

(d) Container #4, ≤ PM2.5 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 #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 


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and seal. A funnel may make it easier to pour 

the silica gel without spilling. A rubber 

policeman may be used as an aid in removing 

the silica gel from the impinger. It is not 

necessary to remove the small amount of 

silica gel dust particles that may adhere to 

the impinger wall and are difficult to remove. 

Since the gain in weight is to be used for 

moisture calculations, do not use any water 

or other liquids to transfer the silica gel. If 

the silica gel has been weighed in the field 

to measure water content, it can be 

discarded. Otherwise the contents of 

Container #6 are weighed during sample 

analysis. 

(g) Container #7, Acetone Rinse Blank— 

Take 100 ml of the acetone directly from the 

wash bottle you used, and place it in 

Container #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 nonrepresentative 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 Stype 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®-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 ±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 #1, ≤ PM 2.5 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 #2, > PM 10 micrometer 

filterable particulate acetone rinse. 

Separately treat this container like Container 

#1. 

11.2.3 Container #3, Filterable particulate 

≤ 10 micrometer and ≥ 2.5 micrometers 

acetone rinse. Separately treat this container 

like Container #1. 

11.2.4 Container #4, ≤ PM 2.5 micrometers 

acetone rinse of the exit tube of cyclone IV 

and front half of the filter holder. Note the 

level of liquid in the container, and confirm 

on the analysis sheet whether leakage 

occurred during transport. If a noticeable 

amount of leakage has occurred, either void 

the sample or use methods, subject to the 

approval of the Administrator, to correct the 

final results. Quantitatively transfer the 

contents to a tared 250 ml beaker, 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 #5, Cold impinger water. 

If the amount of water has not been 

determined in the field, note the level of 

liquid in the container, and confirm on the 

analysis sheet whether leakage occurred 

during transport. If a noticeable amount of 

leakage has occurred, either void the sample 

or use methods, subject to the approval of the 

Administrator, to correct the final results. 

Measure the liquid in this container either 

volumetrically to ±1 ml or gravimetrically to 

±0.5 g. 

11.2.6 Container #6, Silica gel absorbent. 

Weigh the spent silica gel (or silica gel plus 

impinger) to the nearest 0.5 g using a balance. 

This step may be conducted in the field. 

11.2.7 Container #7, Acetone 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. 

An = Area of nozzle, square feet. 

bf = Average blockage factor calculated in 

Equation 25, dimensionless. 

Bws = Moisture content of gas stream, fraction 

e.g., 10% H2O is Bws = 0.10). 

C = Cunningham correction factor for particle 

diameter, Dp, and calculated using the 

actual stack gas temperature, 

dimensionless. 

%CO2 = Carbon Dioxide content of gas 

stream, % by volume. 

Ca = Acetone blank concentration, mg/mg. 

CfPM10 = Conc. of filterable PM10 particulate 

matter, gr/DSCF. 


PWALKER on PROD1PC71 with PROPOSALS3
12986 Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 

CfPM2.5 = Conc. of filterable PM2.5 particulate 

matter, gr/DSCF. 

Cp = Pitot coefficient for the combined 

cyclone pitot, dimensionless. 

Cp’ = Coefficient for the pitot used in the 

preliminary traverse, dimensionless. 

Cr = Re-estimated Cunningham correction 

factor for particle diameter equivalent to 

the actual cut size diameter and calculated 

using the actual stack gas temperature, 

dimensionless. 

Ctf = Conc. of total filterable particulate 

matter, gr/DSCF. 

C1 = ¥150.3162 (micropoise) 

C2 = 18.0614 (micropoise/K 0.5) = 13.4622 

(micropoise/R0.5) 

C3 = 1.19183 × 10 6 (micropoise/K 2) = 

3.86153 × 10 6 (micropoise/R2) 

C4 = 0.591123 (micropoise) 

C5 = 91.9723 (micropoise) 

C6 = 4.91705 × 10 ¥5 (micropoise/K 2) = 

1.51761 × 10 ¥5 (micropoise/R2) 

D= Inner diameter of sampling nozzle 

mounted on Cyclone I, in. 

Dp = Physical particle size, micrometers. 

D50 = Particle cut diameter, micrometers. 

D50¥1= Re-calculated particle cut diameters 

based on re-estimated Cr, micrometers. 

D50LL = Cut diameter for cyclone I 

corresponding to the 2.25 micrometer cut 

diameter for cyclone IV, micrometers. 

D50N = D50 value for cyclone IV calculated 

during the Nth iterative step, micrometers. 

D50 (N∂1) = D50 value for cyclone IV 

calculated during the N+1 iterative step, 

micrometers. 

D50T = Cyclone I cut diameter corresponding 

to the middle of the overlap zone shown 

in Figure 9 of Section 17, micrometers. 

I = Percent isokinetic sampling, 

dimensionless. 

in. = Inches 

Kp = 85.49, [(ft/sec)/(pounds/mole ¥°R)]. 

ma = Mass of residue of acetone after 

evaporation, mg. 

Md = Molecular weight of dry gas, pounds/ 

pound mole. 

Mw = Molecular weight of wet gas, pounds/ 

pound mole. 

M1 = Milligrams of particulate matter 

collected on the filter, ≤ 2.5 micrometers. 

M2 = Milligrams of particulate matter 

recovered from Container #2 (acetone 

blank corrected), >10 micrometers. 

M3 = Milligrams of particulate matter 

recovered from Container #3 (acetone 

blank corrected), ≤10 and >2.5 

micrometers. 

M4 = Milligrams of particulate matter 

recovered from Container #4 (acetone 

blank corrected), ≤2.5 micrometers. 

Ntp = Number of iterative steps or total 

traverse points. 

Nre = Reynolds number, dimensionless. 

%O2,wet = Oxygen content of gas stream, % 

by volume of wet gas. 

[Note: The oxygen percentage used in 

Equation 3 is on a wet gas basis. That means 

that since oxygen is typically measured on a 

dry gas basis, the measured %O2 must be 

multiplied by the quantity (1¥Bws) to 

convert to the actual volume fraction. 

Therefore, %O2,wet = (1¥Bws) * %O2, dry] 

Pbar = Barometric pressure, in. Hg. 

Ps = Absolute stack gas pressure, in. Hg. 

Qs = Sampling rate for cyclone I to achieve 

specified D50, ACFM. 

QsST = Dry gas sampling rate through the 

sampling assembly, DSCFM. 

QI = Sampling rate for cyclone I to achieve 

specified D50, ACFM. 

QIV = Sampling rate for cyclone IV to achieve 

specified D50, ACFM. 

Rmax = Nozzle/stack velocity ratio parameter, 

dimensionless. 

Rmin = Nozzle/stack velocity ratio parameter, 

dimensionless. 

Tm = Meter box and orifice gas temperature, 

°R. 

tn = Sampling time at point n, min. 

tr = Total projected run time, min. 

Ts = Absolute stack gas temperature, °R. 

t1 = Sampling time at point 1, min. 

vmax = Maximum gas velocity calculated from 

Equations 18 or 19, ft/sec. 

vmin = Minimum gas velocity calculated from 

Equations 16 or 17, ft/sec. 

vn = Sample gas velocity in the nozzle, ft/sec. 

vs = Velocity of stack gas, ft/sec. 

Va = Volume of acetone blank, ml. 

Vaw = Volume of acetone used in blank wash, 

ml. 

Vc = Quantity of water captured in impingers 

and silica gel, ml. 

Vm = Dry gas meter volume sampled, ACF. 

Vms = Dry gas meter volume sampled, 

corrected to standard conditions, DSCF. 

Vws = Volume of water vapor, SCF. 

Vb = Volume of aliquot taken for IC analysis, 

ml. 

Vic = Volume of impinger contents sample, 

ml. 

Wa = Weight of residue in acetone blank 

wash, mg. 

Z = Ratio between estimated cyclone IV D50

values, dimensionless. 

DH = Meter box orifice pressure drop, in. 

W.C. 

DH@ = 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.] 

[(Dp)0.5]avg = Average of square roots of the 

velocity pressures measured during the 

preliminary traverse, in. W.C. 

Dpm = Observed velocity pressure using Stype pitot tube in preliminary traverse, in. 

W.C. 

Dpmax = Maximum velocity pressure, in. W.C. 

Dpmin = Minimum velocity pressure, in. W.C. 

Dpn = Velocity pressure measured at point n 

during the test run, in. W.C. 

Dps = Velocity pressure calculated in 

Equation 24, in. W.C. 

Dps1 = Velocity pressure adjusted for 

combined cyclone pitot tube, in. W.C. 

Dps2 = Velocity pressure corrected for 

blockage, in. W.C. 

Dp1 = Velocity pressure measured at point 1, 

in. W.C. 

g = Dry gas meter gamma value, 

dimensionless. 

μ = Gas viscosity, micropoise. 

q = Total run time, minutes. 

ra = Density of acetone, mg/ml (see label on 

bottle). 

12.0 = Constant calculated as 60 percent of 

20.5 square inch cross-sectional area of 

combined cyclone head, square inches. 

12.2 Calculations. Perform all of the 

calculations found in Table 6 of Section 17. 

Table 6 of Section 17 also provides 

instructions and references for the 

calculations. 

12.3 Analyses. Analyze D50 of cyclone IV 

and the concentrations of the particulate 

matter in the various size ranges. 

12.3.1 D50 of cyclone IV. To determine 

the actual D50 for cyclone IV, recalculate the 

Cunningham correction factor and the 

Reynolds number for the best estimate of 

cyclone IV D50. The following sections 

describe additional information on how to 

recalculate the Cunningham correction factor 

and determine which Reynolds number to 

use. 

12.3.1.1 Cunningham correction factor. 

Recalculate the initial estimate of the 

Cunningham correction factor using the 

actual test data. Insert the actual test run data 

and D50 of 2.5 micrometers into Equation 4. 

This will give you a new Cunningham 

correction factor that is based on actual data. 

12.3.1.2 Initial D50 for cyclone IV. 

Determine the initial estimate for cyclone IV 

D50 using the test condition Reynolds number 

calculated with Equation 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 D50 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 D50 for 

cyclone IV with Equation 34, using actual 

test data. 

(c) Insert the ‘‘new’’ D50 value calculated 

by either Equation 33 or 34 into Equation 35 

to re-establish the Cunningham Correction 

Factor (Cr). 

[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 

D50–1. 

(a) Use Equation 36 to calculate the reestablished cyclone IV D50–1 if the Reynolds 

number is less than 3,162. 

(b) Use Equation 37 to calculate the reestablished cyclone IV D50–1 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 D50

(either Equation 33 or 34) to the reestablished cyclone IV D50–1 (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 

D50–1 value is the best estimate of the cyclone 

IV D50 cut diameter for your test run. 

(b) If the ‘‘Z’’ value is greater than 1.01 or 

less than 0.99, re-establish a Cunningham 

correction factor based on the D50–1 value 

determined in either Equations 36 or 37, 

depending upon the test condition Reynolds 

number. 

(c) Use the second revised Cunningham 

correction to re-calculate the cyclone IV D50. 

(d) Repeat this iterative process as many 

times as necessary using the prescribed 


PWALKER on PROD1PC71 with PROPOSALS3
Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 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 (Ca). 

12.3.2.2 Acetone blank weight. Use 

Equation 42 to calculate the acetone blank 

weight (Wa). 

[Note: Correct each of the particulate 

matter weights per size fraction by 

subtracting the acetone blank weight (that is, 

M2,3,4–Wa)]. 

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 

#1, #2, #3, and #4. This is the total 

collectable particulate matter (Ctf). 

(b) Use Equation 44 to determine the 

quantitative recovery of PM10 particulate 

matter (CfPM10) from Containers #1, #3, and 

#4. 

(c) Use Equation 45 to determine the 

quantitative recovery of PM2.5 particulate 

(CfPM2.5) recovered from Containers #1 and 

#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. 

M CO O O CO d = 0 44 0 32 0 28 100 .% .% . % % ( ) 2 2 22 + ( ) + −− ( ) Eq. 1

Molecular Weight of Wet Gas. Calculate the 

molecular weight of the stack gas on a wet 

basis using Equation 2. 

Mw = M 1 B B Eq. 2 d ws ws ( ) − + 18 ( )

Gas Viscosity. Calculate the gas viscosity 

using Equation 3. This equation uses 

constants for gas temperatures in °R. 

μ B B =+ + + ( ) − + ws ws

− C C T CT C O C C 12 3 s s wet

2

42 5 6 % , Eq. 3 Ts

2

Cunningham Correction Factor. The 

Cunningham correction factor is calculated 

for a 2.25 micrometer diameter particle. 

C

P D

T

s p M

s

w

 = + Eq. 4

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

⎡

⎣

⎢ ⎤

⎦

1 0 0057193 ⎥

0 5

.

.

μ

Lower Limit Cut Diameter for Cyclone I for 

Nre < 3,162. The Cunningham correction 

factor is for a 2.25 micrometer diameter 

particle. 

D

M P

T LL

w s

s

50 9 507 3 1 C Eq. 5

N < 0.3007

 0.1993

re

= ⎡

⎣

⎢ ⎤

⎦

⎥ . ( ) , 62

Cut Diameter for Cyclone I for the Middle 

of the Overlap Zone. D

D

Eq T

LL

50

50 11

2 6 = ⎛ +

⎝

⎜ ⎞

⎠

⎟ .

Sampling Rate. 


PWALKER on PROD1PC71 with PROPOSALS3EP25MR09.000</MATH> EP25MR09.001</MATH> EP25MR09.002</MATH> EP25MR09.003</MATH> EP25MR09.004</MATH> EP25MR09.005</MATH>
12988 Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 

Q Q T

MP D s I

s

ws T

 = = ( ) ⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

0 07296 ⎥ 1 0 2949

50

1 41

.

. .

μ

02

Eq. 7

Reynolds Number. 

N

P M

T

Q re

s w

s

s = × Eq. 8 ⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥ 8 64 105 . μ

Meter Box Orifice Pressure Drop. 

Δ

Δ H Eq Q BP

T

TM H

P

s ws s

s

m d

bar

= ⎡ ( ) −

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥

1 1 083 2

. @ . 9

Lower Limit Cut Diameter for Cyclone I for 

Nre ≥ 3,162. The Cunningham correction 

factor is for a 2.25 micrometer diameter 

particle. 

D

M P

T LL

w s

s

50

0 0600

 C 10 0959 Equation 10

N 0.4400

re

= ⎡

⎣

⎢ ⎤

⎦

⎥ .

.

( ) < 3162

Velocity of Stack Gas. Correct the mean 

preliminary velocity pressure for Cp and 

blockage using Equations 23, 24, and 25. 

v KC p T

P M s pp avg

s

s w

 Eq. 11 = ( ) ( ) ⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

Δ

Calculated Nozzle Diameter for Acceptable 

Sampling Rate. 

D Q

v

Eq. 12 s

s

= ⎡

⎣

⎢ ⎤

⎦

⎥ 3 056 0 5

. .

Velocity of Gas in Nozzle. 

V

Q

A n

s

n

 = Eq. 13 60

⎛

⎝

⎜ ⎞

⎠

⎟

Minimum Nozzle/Stack Velocity Ratio 

Parameter. 

R Q

v

s

n

min =+− ⎛ ( ) ( )

⎝

⎜

⎜

⎞

⎠

⎟

⎟ 0 2457 0 3072

0 2603 0 5

1 5 . . . ..

μ 0 5. ⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥ Eq. 14

Maximum Nozzle/Stack Velocity Ratio 

Parameter. 

R Q

v

s

n

max + = + ⎛ ( ) ( )

⎝

⎜

⎜

⎞

⎠

⎟

⎟ 0 4457 0 5690

0 2603 0 5

1 5 . . . ..

μ 0 5. ⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥ Eq. 15

Minimum Gas Velocity for Rmin ≤ 0.5. 

v v min n = Eq. 16 (.) 0 5

Minimum Gas Velocity for Rmin ≥ 0.5. 

v vR min min n = Eq. 17

Maximum Gas Velocity for Rmax < 1.5. 

v vR max max n = Eq. 18

Maximum Gas Velocity for Rmax ≥ 1.5. 


EP25MR09.006</MATH> EP25MR09.007</MATH> EP25MR09.008</MATH> EP25MR09.009</MATH> EP25MR09.010</MATH> EP25MR09.011</MATH> EP25MR09.012</MATH> EP25MR09.013</MATH> EP25MR09.014</MATH> EP25MR09.015</MATH> EP25MR09.016</MATH> EP25MR09.017</MATH>PWALKER on PROD1PC71 with PROPOSALS3
Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 12989 

v Eq max = v 1.5 19 . n ( ) Minimum Velocity Pressure. 

Δ × ⎡

⎣

⎢ ⎤

⎦

⎥

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

− = 1.3686 10 P M

T

v

C

 20 min

s w

s

min

p

p Eq 4

2

.

Maximum Velocity Pressure. 

Δ p Eq. 2 P M

T

v

C

s w

s p

max

max = × . ⎡

⎣

⎢ ⎤

⎦

⎥

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

− 1 3686 10 4

2

1

Sampling Time at Point 1. Ntp is the total 

number of traverse points. You must use the 

preliminary velocity traverse data. 

t p

p

t

N avg

r

tp

1

1 = Eq. 22 ( )

⎡

⎣

⎢

⎢

⎢

⎤

⎦

⎥

⎥

⎥

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

Δ

Δ

Sampling Time at Point n. You must use 

the actual test run data at each point, n, and 

test run point 1. 

t t p

p n

n = Eq. 23 1

1

Δ

Δ

Adjusted Velocity Pressure. 

Δ Δ Eq. 24 p p

C

C s m

p

p

= ⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

2

Average Probe Blockage Factor. 

b

A f Eq. 25 = 12 0.

Velocity Pressure. 

Δ Δ p p Eq. 26 b s s

f

2 1 1

1

2

= ( ) −

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

Dry Gas Volume Sampled at Standard 

Conditions. 

v V

P H

T ms m

bar

m

 = ⎡

⎣

⎢ ⎤

⎦

⎥ [ ]

+ ⎛

⎝

⎜ ⎞

⎠

⎟ ⎡

⎣

⎢

⎢

⎢

⎢

⎤

⎦

⎥

⎥

⎥

528

29 92

13 6

.

. γ

Δ

⎥

Eq. 27

Sample Flow Rate at Standard Conditions. 

Q V sST

ms Eq. 28 = θ

Volume of Water Vapor. 

V V ws c Eq. 29 = 0 04707 .

Moisture Content of Gas Stream. 

B V

V V ws

ws

ms ws

 = Eq. 30

+

⎡

⎣

⎢ ⎤

⎦

⎥

Sampling Rate. 

Q B

T

P Eq s

ws

s

s

 = Q 31 sST

29 92

528

1

1

. . ( ) −

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

⎡

⎣

⎢ ⎤

⎦

⎥


EP25MR09.018</MATH> EP25MR09.019</MATH> EP25MR09.020</MATH> EP25MR09.021</MATH> EP25MR09.022</MATH> ep25mr09.023</MATH> EP25MR09.024</MATH> EP25MR09.025</MATH> EP25MR09.026</MATH> EP25MR09.027</MATH> EP25MR09.028</MATH> EP25MR09.029</MATH> EP25MR09.030</MATH>PWALKER on PROD1PC71 with PROPOSALS3
12990 Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 

[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. 

D

P Q Eq

s s

50

0 2091 0 7091

 = 0.15625 T

M 

 32 s

w

 ⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥

. .

. μ

Particle Cut Diameter for Nre < 3,162 for 

Cyclone IV. C must be recalculated using the 

actual test run data and a D50 (Dp) of 2.5. 

D

Q M s w

50

1 1791 0 5

 = 0.0024302 1

C TP 

s

s

⎡ μ

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥

⎡

⎣

⎢ ⎤ . .

⎦

⎥ ( )

0 6790 .

Equation 33

N < 3162 re

Particle Cut Diameter for Nre ≥ 3,162 for 

Cyclone IV. C must be recalculated using the 

actual test run data and a D50 (Dp) of 2.5. 

D

Qs w

50

0 5 0

 0.019723 1

C

T

P M

 0.8058

s

s

= ⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥

⎡

⎣

⎢ ⎤

⎦

⎥ μ . .3058 Equation 34

N < 3162 ( ) re

Re-estimated Cunningham Correction 

Factor. You must use the actual test run 

Reynolds Number (Nre) value and select the 

appropriate D50 from Equation 32 or 33 (or 

Equation 36 or 37 if reiterating). 

C

P Eq r

s

 = 1 + 0.0057193 

 D

T

M

 35

50

s

w

⎡ μ

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥

0 5.

.

Re-calculated Particle Cut Diameter for Nre

< 3,162. 

D

Q M s w

50 1

1 1791 0 5

−

⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

 = 0.0024302 1

C TP r

s

s

μ . .

⎢ ⎤

⎦

⎥ ( )

0 6790 .

Equation 36

N < 3162 re

Re-calculated Particle Cut Diameter for N 

≥ 3,162. 

D

Q M s w

50 1

0 8058 0 5

−

⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ ⎤

⎦

⎥ ⎡

⎣

⎢ = 0.019723 1

C TP r

s

s

μ . .

⎤

⎦

⎥ ( )

0 3058 .

Equation 37

N < 3162 re

Ratio (Z) Between D50 and D50–1 Values. 

Z

D = Eq

D 38 50 − 1

50

.

Acceptance Criteria for Z Values. The 

number of iterative steps is represented by N. 

0 99 . . Z = 

D

D

 1.01 39 50

50 

N

N + 1

≤ ⎛

⎝

⎜

⎜

⎞

⎠

⎟

⎟

⎡

⎣

⎢

⎢

⎤

⎦

⎥

⎥

≤ Eq


EP25MR09.031</MATH> EP25MR09.032</MATH> EP25MR09.033</MATH> EP25MR09.034</MATH> EP25MR09.035</MATH> EP25MR09.036</MATH> EP25MR09.037</MATH> EP25MR09.038</MATH>PWALKER on PROD1PC71 with PROPOSALS3
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Percent Isokinetic Sampling. 

I Eq = 100 T V 29.92

 v A P 1 B 528

s ms

s n s ws 60 ‚ ( ) −

⎛

⎝

⎜

⎜

⎞

⎠

⎟

⎟ . 40

Acetone Blank Concentration. 

C Eq a = m

V 

 41 a

a ρa

.

Acetone Blank Weight. 

Wa = C V Eq. 42 a aw ρa

Concentration of Total Filterable 

Particulate Matter. 

C Eq t f

1234

ms

 = 7000

453,592

M + M + M + M

V

⎛

⎝

⎜ ⎞

⎠

⎟

⎡

⎣

⎢ ⎤

⎦

⎥ . 43

Concentration of Filterable PM10

Particulate Matter. 

C Eq fPM 10

134

ms

 = 7000

453,592

M + M + M

V

 44 ⎛

⎝

⎜ ⎞

⎠

⎟

⎡

⎣

⎢ ⎤

⎦

⎥ .

Concentration of Filterable PM2.5

Particulate Matter. 

C Eq fPM 2.5

1 4

ms

 = 7000

453,592

M + M

V

 45 ⎛

⎝

⎜ ⎞

⎠

⎟

⎡

⎣

⎢ ⎤

⎦

⎥ .

13.0 Method Performance 

(a) Field evaluation of PM10 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 PM10

and PM10 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 PM10 method for total mass, 

referenced to Method 17, was ¥2± 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 

PM10 cyclones were designed to limit error 

due to spatial variations to 10 percent. The 

maximum allowable error due to anisokinetic 

sampling was limited to ±20 percent for 10 

μm 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 

PM2.5 at Stationary Sources,’’ U.S. 

Environmental Protection Agency, 

Atmospheric Research and Exposure 

Assessment Laboratory, Research Triangle 

Park, NC 27511, EPA–600/3–90/057 (NTIS 

No.: PB 90–247198), 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 PM10/ 

PM2.5 Emission Factor Chemical 

Characterization Testing,’’ PCA R&D Serial 

No. 2081, Portland Cement Association, 

1996. 

4. Farthing and Co-workers, 1988a ‘‘PM10

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 PM10 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. 


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TABLE 2—REQUIRED CYCLONE CUT DIAMETERS (D50) 

Cyclone 

Min. cut diameter 

(Micrometer) 

Max. cut 

diameter 

(Micrometer) 

PM10 Cyclone (Cyclone I from five stage cyclone) ................................................................................................. 9 11 

PM2.5 Cyclone (Cyclone IV from five stage cyclone) .............................................................................................. 2.25 2.75 

TABLE 3—PRETEST CALCULATIONS

If you are using . . . To calculate . . . Then use . . . 

Preliminary data ......................................................................... dry gas molecular weight, Md ................................................... Equation 1. 

Dry gas molecular weight (Md) and preliminary moisture content of the gas stream.wet gas molecular weight, MW ................................................. Equation 2 a. 

Stack gas temperature, and oxygen and moisture content of 

the gas stream.

gas viscosity, μ ......................................................................... Equation 3. 

Gas viscosity, μ ......................................................................... Cunningham correction factor b, C ........................................... Equation 4. 

Reynolds Number c (Nre) ...........................................................

Nre < 3,162 .................................................................................

preliminary lower limit cut diameter for cyclone I, D50LL .......... Equation 5. 

D50LL from Equation 5 ............................................................... cut diameter for cyclone I for middle of the overlap zone, 

D50T.

Equation 6. 

D50T from Equation 6 ................................................................. final sampling rate for cyclone I, QI(Qs) ................................... Equation 7. 

QI(Qs) from Equation 7 .............................................................. (verify) the assumed Reynolds number ................................... Equation 8. 

a Use Method 4 to determine the moisture content of the stack gas. Use a wet bulb-dry bulb measurement device or hand-held hygrometer to 

estimate moisture content of sources with gas temperature less than 160 °F. bFor the lower cut diameter of cyclone IV, 2.25 micrometer. 

cVerify the assumed Reynolds number using the procedure in Section 8.5.1, before proceeding to Equation 9. 

TABLE 4—DH VALUES BASED ON PRELIMINARY TRAVERSE DATA

Stack temperature (°R) Ts¥50° Ts Ts + 50° 

DH, (in. W.C.) ........................................................................................................................................... ¥ ¥ ¥ 

TABLE 5—VERIFICATION OF THE ASSUMED REYNOLDS NUMBER

If the Nre is . . . Then . . . And . . . 

< 3,162 ............................................ Calculate DH for the meter box.

≥ 3,162 ............................................ Recalculate D50LL using Equation 10 ........................ Substitute the ‘‘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 °C,760 mm Hg or 68 °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 numbera ............................................ 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. 


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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 °C (85 °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 PM10

and PM2.5 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 °C (85 °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 

(N2) immediately after sample collection to 

remove dissolved sulfur dioxide (SO2) gases 

from the impinger. The CPM filter is 

extracted with water and methylene chloride. 

The impinger solution is then extracted with 

methylene chloride (MeCl2). The organic and 

aqueous fractions are dried and the residues 

are weighed. The total of the aqueous and 

organic fractions represents the CPM. 

2.1.2 Dry Impinger and Additional Filter. 

The potential artifacts from SO2 are reduced 

using a condenser and 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 PM10. Primary PM10 (also 

known as direct PM10, total PM10, PM10 or 

filterable PM10, and condensable PM, 

individually) means particulate matter with 

an aerodynamic diameter equal to or less 

than 10 micrometers. 

3.4 Primary PM2.5. Primary PM2.5 (also 

known as direct PM2.5, total PM2.5, PM2.5, or 

filterable PM2.5, 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 PM2.5

emissions include elemental carbon, directly 

emitted organic carbon, directly emitted 

sulfate, directly emitted nitrate, and other 

inorganic particles (including but not limited 

to crustal material, metals, and sea salt). 

3.5 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 PM2.5 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 GreenburgSmith 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®-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® O-ring, stainless 

steel, ceramic or Teflon® filter support and 

a final Teflon® O-ring. At the exit of the CPM 

filter, install a Teflon®-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 


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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® 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® 

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 

SO2 or sulfur trioxide (SO3) emissions, then 

you must use a filter that will not react with 

SO2 or SO3. 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 °C (350 °F) if 

it is being reused. You do not have to dry 

new silica gel. 

7.1.3 Water. Use deionized distilled ultrafiltered 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, MeCl2, 

anhydrous sodium sulfate, ammonia 

hydroxide (NH4OH), 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 ultrafiltered 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) NH4OH. 

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 °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, MeCl2. It is important to 

completely remove all silicone grease from 

areas that will be exposed to the MeCl2 rinse 

during sample recovery. After cleaning, you 

must bake glassware at 300 °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-ofstack 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 °C (85 

°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 °C (≤ 85 °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 


PWALKER on PROD1PC71 with PROPOSALS3
Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 13005 

Teflon® 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°C (68 °F) at the exit of the moisture 

traps. 

8.4.5 Silica Gel Trap. Place 200 to 300 g 

of silica gel in each of several air-tight 

containers. Weigh each container, including 

silica gel, to the nearest 0.5 g, and record this 

weight on the filterable particulate data 

sheet. As an alternative, the silica gel need 

not be preweighed, but may be weighed 

directly in its impinger or sampling holder 

just prior to train assembly. 

8.4.6 Leak-Check (Pretest). Use the 

procedures outlined in Method 5, 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 leakcheck of the pitot tube assembly. Follow the 

procedures outlined in Section 8.4.1 of 

Method 5. 

8.5 Sampling Train Operation. Operate 

the sampling train as described in the 

filterable particulate sampling method (i.e., 

Method 5, 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 °C (≤85 °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 °C (68 °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 DH@, 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 °C (85 °F). Continue the purge under these 

conditions for 1 hour, checking the rotameter 

and DH 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 #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 #1 holds the 

water soluble CPM captured in the 

impingers. 

8.5.4.3 CPM Container #2, Organic 

Rinses. Follow the water rinses of the probe 

extension, condenser, each impinger and all 

of the connecting glassware and front half of 

the CPM filter with an acetone rinse. Then 

repeat the entire procedure with two rinses 

of MeCl2, and save both solvents in a separate 

glass container identified as CPM Container 

#2. Mark the liquid level on the jar. 

8.5.4.4 CPM Container #3, CPM filter 

Sample. Use tweezers and/or clean 

disposable surgical gloves to remove the filter 

from the CPM filter holder. Place the filter in 

the petri dish identified as CPM Container 

#3. 

8.5.4.5 CPM Container #4, Cold Impinger 

Water. You must weigh or measure the 

volume of the contents of CPM Container #4 

either in the field or during sample analysis 

(see Section 11.2.3). 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 #5, Silica Gel 

Absorbent. You must weigh the contents of 

CPM Container #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 #6, Acetone Rinse 

Blank. Take 150 mL of the acetone directly 

from the wash bottle you used, and place it 

in CPM Container #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 #7, Water Rinse 

Blank. Take 150 mL of the water directly 

from the wash bottle you used, and place it 

in CPM Container #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 #8, Methylene 

Chloride Rinse Blank. Take 150 mL of the 

MeCl2 directly from the wash bottle you 

used, and place it in CPM Container #8, 

labeled Methylene Chloride Rinse Blank (see 


PWALKER on PROD1PC71 with PROPOSALS3
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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 °C (85 °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 nonrepresentative 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 

NH4OH used for titrations in this method is 

made as follows: Add 7 mL of concentrated 

(14.8 M) NH4OH to l liter of water. 

Standardize against standardized 0.1 N 

H2SO4, and calculate the exact normality 

using a procedure parallel to that described 

in Section 5.5 of Method 6 of Appendix A– 

4 to 40 CFR part 60. Alternatively, purchase 

0.1 N NH4OH that has been standardized 

against a NIST reference material. Record the 

normality on the 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 ± 1 mL or 

gravimetrically to ± 0.5 g. Confirm on the 

filterable particulate analytical data sheet 

whether leakage occurred during transport. If 

a noticeable amount of leakage has occurred, 

either void the sample or use methods, 

subject to the approval of the Administrator, 

to correct the final results. 

11.2 Condensable 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 #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 °C (85 

°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 #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 #2. 

Repeat this extraction step twice for a total 

of three extractions. 


PWALKER on PROD1PC71 with PROPOSALS3
Federal Register / Vol. 74, No. 56 / Wednesday, March 25, 2009 / Proposed Rules 13007 

11.2.2 CPM Container #1, Aqueous 

Liquid Impinger Contents. Analyze the water 

soluble CPM in Container 1 as described in 

this section. Place the contents of Container 

#1 into a separatory funnel. Add 

approximately 30 mL of MeCl2 to the funnel, 

mix well, and drain off the lower organic 

phase. Repeat this procedure twice with 30 

mL of MeCl2 each time combining the 

organic phase from each extraction. Each 

time, leave a small amount of the organic/ 

MeCl2 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 #2. Combine the 

organic extract from Container #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 

°C (85 °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 °C (85 

°F)) and pressure in a laboratory hood. 

Following evaporation, desiccate the organic 

fraction for 24 hours in a desiccator 

containing anhydrous calcium sulfate. Weigh 

at intervals of at least 6 hours to a constant 

weight (i.e., ≤ 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 °C, and allow to dry at room temperature 

(not to exceed 30 °C (85 °F). You must ensure 

that water and volatile acids have completely 

evaporated before neutralizing nonvolatile 

acids in the sample. 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 NH4OH 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 °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 °C (85 °F)) and 

pressure in a laboratory hood. Following 

evaporation, desiccate the residue for 24 

hours in a desiccator containing anhydrous 

calcium sulfate. Weigh at intervals of at least 

6 hours to a constant weight (i.e., ≤ 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∂ retained in the sample 

using Equation 1 in Section 12. 

11.2.3 CPM Container #4, Cold Impinger 

Water. If the amount of water has not been 

determined in the field, note the level of 

liquid in the container, and confirm on the 

filterable particulate analytical data sheet 

whether leakage occurred during transport. If 

a noticeable amount of leakage has occurred, 

either void the sample or use methods, 

subject to the approval of the Administrator, 

to correct the final results. Measure the liquid 

in Container #4 either volumetrically to ± 1 

mL or gravimetrically to ± 0.5 g, and record 

the volume or weight on the filterable 

particulate analytical data sheet of the 

filterable particulate matter test method. 

11.2.4 CPM Container #5, Silica Gel 

Absorbent. Weigh the spent silica gel (or 

silica gel plus impinger) to the nearest 0.5 g 

using a balance. This step may be conducted 

in the field. Record the weight on the 

filterable particulate analytical data sheet of 

the filterable particulate matter test method. 

11.2.5 Container #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 °C (85 °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 °C (85 

°F)) and pressure in a laboratory hood. 

Following evaporation, desiccate the residue 

for 24 hours in a desiccator containing 

anhydrous calcium sulfate. Weigh at 

intervals of at least 6 hours to a constant 

weight (i.e., ≤ 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 

#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 °C. Quantitatively transfer the beaker 

contents to a clean preweighed 50-mL tin, 

and evaporate to dryness at room 

temperature (not to exceed 30 °C (85 °F)) and 

pressure in a laboratory hood. Following 

evaporation, desiccate the residue for 24 

hours in a desiccator containing anhydrous 

calcium sulfate. Weigh at intervals of at least 

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 #8. Use 100 mL of MeCl2

from the blank container for this analysis. 

Transfer 100 mL of the MeCl2 to a clean 250- 

mL beaker. Evaporate the methylene chloride 

at room temperature (not to exceed 30 °C (85 

°F)) and pressure in a laboratory hood to 

approximately 10 mL. Quantitatively transfer 

the beaker contents to a 50-mL preweighed 

tin, and evaporate to dryness at room 

temperature (not to exceed 30 °C (85 °F)) and 

pressure in a laboratory hood. Following 

evaporation, desiccate the residue for 24 

hours in a desiccator containing anhydrous 

calcium sulfate. Weigh at intervals of at least 

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. 

DH@ = 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. 

Ccpm = Concentration of the condensable 

particulate matter in the stack gas, dry 

basis, corrected to standard conditions, 

milligrams/dry standard cubic foot. 

mc = Mass of the NH4

∂ added to sample to 

form ammonium sulfate, mg. 

mcpm = Mass of the total condensable 

particulate matter, mg. 

mfb = Mass of field train total CPM blank, mg 

mi = Mass of inorganic CPM matter, mg. 

mib = Mass of field train inorganic CPM 

blank, mg. 

mo = Mass of organic CPM, mg. 

mob = Mass of organic field train blank, mg. 

mr = Mass of dried sample from inorganic 

fraction, mg. 

N = Normality of ammonium hydroxide 

titrant. 

Vm(std) = Volume of gas sample measured by 

the dry gas meter, corrected to standard 

conditions, dry standard cubic meter 

(dscm) or dry standard cubic foot (dscf) as 

defined in Equation 5–1 of Method 5. 

Vt = Volume of NH4OH titrant, mL. 

Vp = Volume of water added during train 

purge. 

12.2 Calculations. Use the following 

equations to complete the calculations 

required in this test method. Enter the 

appropriate results from these calculations 

on the 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. 

mC = 17.03 v N Eq. 1 × × t

12.2.2 Mass of the Field Blank (mg). Per 

Section 9.9, the mass of the field blank, mfb, 

shall not exceed 2.0 mg. 

m Eq fb = m + m 2 ib ob .

12.2.3 Mass of Inorganic CPM (mg). 

m Eq i = m m 3 r c − .

12.2.4 Total Mass of CPM (mg). 

m Eq cpm = m + m m 4 i o fb − .

12.2.5 Concentration of CPM (mg/dscf). 


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C Eq cpm = m

V

 5 cpm

m std ( )

.

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. 


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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 

FIGURE 3—FIELD TRAIN BLANK CONDENSABLE PARTICULATE CALCULATIONS—Continued 

Mass of Inorganic CPM 

(mib)(Equation 3).

mg 

Mass of the Field Train Blank (not to 

exceed 2.0 mg) (Equation 2).

mg 

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] (Vp).

ml 

Date 

Run No. 

CPM Filter No. 

Water volume added to purge train 

[max 50 mL] (Vp).

ml 

Date 

Run No. 

CPM Filter No. 

Water volume added to purge train 

[max 50 mL] (Vp) 

ml 

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 ......................................................................... llllllll 

If Yes, measure the volume received ...................................................................................................................... llllllll 

Estimate the volume lost during transport ............................................................................................................... llllllll mL 

Was significant volume of organic rinse lost during transport? Yes or No ............................................................. llllllll 

If Yes, measure the volume received. Estimate the volume lost during transport .................................................. llllllll mL 

For Titration 

Normality of NH4OH (N) (Section 10.2) ................................................................................................................... llllllll N 

Volume of titrant (Vt) (Section 11.2.2.4) .................................................................................................................. llllllll mL 

Mass of NH4 added (mc) (Equation 1) ..................................................................................................................... llllllll mg 

For CPM Blank Weights 

Inorganic Train Field Blank Mass(mib) (Section 9.9) ............................................................................................... llllllll mg 

Organic Train Field Blank Mass (mob) (Section 9.9) ............................................................................................... llllllll mg 

Mass of Train Field Blank (Mfb) (max. 2 mg) (Equation 2) ..................................................................................... llllllll mg 

For CPM Train Weights 

Mass of Organic CPM (mo) (Section 11.2.2.2) ........................................................................................................ llllllll mg 

Mass of Inorganic CPM (mi) (Equation 3) ............................................................................................................... llllllll mg 

Total CPM Mass (mcpm) (Equation 4) ...................................................................................................................... llllllll mg 


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[FR Doc. E9–6178 Filed 3–24–09; 8:45 am] 

BILLING CODE 6560–50–C 


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