80118 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 51 

[EPA–HQ–OAR–2008–0348; FRL–9236–2] 

RIN 2060–AO58 

Methods for Measurement of Filterable 

PM10 and PM2.5 and Measurement of 

Condensable PM Emissions From 

Stationary Sources 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: This action promulgates 

amendments to Methods 201A and 202. 

The final amendments to Method 201A 

add a particle-sizing device to allow for 

sampling of particulate matter with 

mean aerodynamic diameters less than 

or equal to 2.5 micrometers (PM2.5 or 

fine particulate matter). The final 

amendments to Method 202 revise the 

sample collection and recovery 

procedures of the method to reduce the 

formation of reaction artifacts that could 

lead to inaccurate measurements of 

condensable particulate matter. 

Additionally, the final amendments to 

Method 202 eliminate most of the 

hardware and analytical options in the 

existing method, thereby increasing the 

precision of the method and improving 

the consistency in the measurements 

obtained between source tests 

performed under different regulatory 

authorities. 

This action also announces that EPA 

is taking no action to affect the already 

established January 1, 2011 sunset date 

for the New Source Review (NSR) 

transition period, during which EPA is 

not requiring that State NSR programs 

address condensable particulate matter 

emissions. 

DATES: This final action is effective on 

January 1, 2011. 

ADDRESSES: EPA has established a 

docket for this action under Docket ID 

No. EPA–HQ–OAR–2008–0348. All 

documents are listed in the http://www.

regulations.gov index. Although listed 

in the index, some information is not 

publicly available, e.g., confidential 

business information (CBI) or other 

information whose disclosure is 

restricted by statute. Certain other 

material, such as copyrighted material, 

will be publicly available only in hard 

copy form. Publicly available docket 

materials are available either 

electronically at http://www.regulations.

gov or in hard copy at the EPA Docket 

Center EPA/DC, EPA West, Room 3334, 

1301 Constitution Ave., NW., 

Washington, DC. The Public Reading 

Room is open from 8:30 a.m. to 4:30 

p.m., Monday through Friday, excluding 

legal holidays. The telephone number 

for the Public Reading Room is (202) 

566–1744, and the telephone number for 

the Air Docket Center is (202) 566–1742. 

FOR FURTHER INFORMATION CONTACT: For 

general information, contact Ms. 

Candace Sorrell, U.S. EPA, Office of Air 

Quality Planning and Standards, Air 

Quality Assessment Division, 

Measurement Technology Group (E143– 

02), Research Triangle Park, NC 27711; 

telephone number: (919) 541–1064; fax 

number; (919) 541–0516; e-mail address: 

sorrell.candace@epa.gov. For technical 

questions, contact Mr. Ron Myers, U.S. 

EPA, Office of Air Quality Planning and 

Standards, Sector Policies and Programs 

Division, Measurement Policy Group 

(D243–05), Research Triangle Park, NC 

27711; telephone number: (919) 541– 

5407; fax number: (919) 541–1039; 

e-mail address: myers.ron@epa.gov. 

SUPPLEMENTARY INFORMATION: 

Acronyms and Abbreviations. The 

following acronyms and abbreviations 

are used in this document. 

Dpmax maximum velocity pressure 

Dpmin minimum velocity pressure 

μm micrometers 

ASTM American Society for Testing and 

Materials 

AWMA Air and Waste Management 

Association 

CAA Clean Air Act 

CBI confidential business information 

CCM Controlled Condensation Method 

CPM condensable PM 

DOP dioctyl phthalate 

DOT Department of Transportation 

DQO data quality objective 

MSHA Mine Safety and Health 

Administration 

NAAQS National Ambient Air Quality 

Standards 

NSR New Source Review 

NTTAA National Technology Transfer and 

Advancement Act of 1995 

OSHA Occupational Safety and Health 

Administration 

PCB polychlorinated biphenyl 

PM particulate matter 

PM10 particulate matter less than or equal to 

10 micrometers 

PM2.5 particulate matter less than or equal 

to 2.5 micrometers 

ppmw parts per million by weight 

PTFE polytetrafluoropolymer 

RCRA Resource Conservation and Recovery 

Act 

RFA Regulatory Flexibility Act 

SBA Small Business Administration 

SIP State Implementation Plan 

SO2 sulfur dioxide 

TDS total dissolved solids 

TTN Technology Transfer Network 

UMRA Unfunded Mandates Reform Act 

www World Wide Web 

The information in this preamble is 

organized as follows: 

I. General Information 

A. Does this action apply to me? 

B. Where can I obtain a copy of this action 

and other related information? 

C. What is the effective date? 

D. Judicial Review 

II. Background 

A. Why is EPA issuing this final action? 

B. Particulate Matter National Ambient Air 

Quality Standards 

C. Measuring PM Emissions 

1. Method 201A 

2. Method 202 

III. Summary of Changes Since Proposal 

A. Method 201A 

B. Method 202 

C. How will the final amendments to 

methods 201A and 202 affect existing 

emission inventories, emission 

standards, and permit programs? 

IV. Summary of Final Methods 

A. Method 201A 

B. Method 202 

V. Summary of Public Comments and 

Responses 

A. Method 201A 

B. Method 202 

C. Conditional Test Method 039 (Dilution 

Method) 

VI. Statutory and Executive Order Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review 

B. Paperwork Reduction Act 

C. Regulatory Flexibility Act 

D. Unfunded Mandates Reform Act 

E. Executive Order 13132: Federalism 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

and Safety Risks 

H. Executive Order 13211: Actions 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution, or Use 

I. National Technology Transfer and 

Advancement Act 

J. Executive Order 12898: Federal Actions 

To Address Environmental Justice in 

Minority Populations and Low-Income 

Populations 

K. Congressional Review Act 

I. General Information 

A. Does this action apply to me? 

This action applies to you if you 

operate a stationary source that is 

subject to applicable requirements to 

control or measure total particulate 

matter (PM), total PM with mean 

aerodynamic diameters less than or 

equal to 10 micrometers (μm) (PM10), or 

total PM2.5, where EPA Method 202 is 

incorporated as a component of the 

applicable test method. 

In addition, this action applies to you 

if federal, State, or local agencies take 

certain additional independent actions. 

For example, this action applies to 

sources through actions by State and 

local agencies that implement 

condensable PM (CPM) control 

measures to attain the National Ambient 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80119 

1We recognize that this rule could be published 

at least 30 days before January 1, 2011, which 

would negate the need for this good cause finding, 

and we plan to request expedited publication of this 

rule in order to decrease the likelihood of a 

publication delay. However, as we cannot know the 

date of publication in advance of signing this rule, 

we are proceeding with this good cause finding for 

an effective date on or before January 1, 2011, in 

an abundance of caution in order to avoid the 

unnecessary regulatory confusion noted above. 

Air Quality Standards (NAAQS) for 

PM2.5 and specify the use of Method 202 

to demonstrate compliance with the 

control measures. State and local 

agencies that specify the use of Method 

201A or 202 would have to implement 

the following: (1) Adopt this method in 

rules or permits (either by incorporation 

by reference or by duplicating the 

method in its entirety), and (2) 

promulgate an emissions limit requiring 

the use of Method 201A or 202 (or an 

incorporated method based upon 

Method 201A or 202). This action also 

applies to stationary sources that are 

required to meet new applicable CPM 

requirements established through 

federal or State permits or rules, such as 

New Source Performance Standards and 

New Source Review (NSR), which 

specify the use of Method 201A or 202 

to demonstrate compliance with the 

control measures. 

The source categories and entities 

potentially affected include, but are not 

limited to, the following: 

Category NAICSa Examples of regulated entities 

Industry ............................................ 332410 ........................................... Fossil fuel steam generators. 

332410 ........................................... Industrial, commercial, institutional steam generating units. 

332410 ........................................... Electricity generating units. 

324110 ........................................... Petroleum refineries. 

562213 ........................................... Municipal waste combustors. 

322110 ........................................... Pulp and paper mills. 

325188 ........................................... Sulfuric acid plants. 

327310 ........................................... Portland cement plants. 

327410 ........................................... Lime manufacturing plants. 

211111, 212111, 212112, 212113 Coal preparation plants. 

331312, 331314 ............................. Primary and secondary aluminum plants. 

331111, 331513 ............................. Iron and steel plants. 

321219, 321211, 321212 .............. Plywood and reconstituted products plants. 

a North American Industrial Classification System. 

B. Where can I obtain a copy of this 

action and other related information? 

In addition to being available in the 

docket, an electronic copy of these final 

rules are also available on the World 

Wide Web (http://www.epa.gov/ttn/) 

through the Technology Transfer 

Network (TTN). Following the 

Administrator’s signature, a copy of 

these final rules will be posted on the 

TTN’s policy and guidance page for 

newly proposed or promulgated rules at 

http://www.epa.gov/ttn/oarpg. The TTN 

provides information and technology 

exchange in various areas of air 

pollution control. 

C. What is the effective date? 

The final rule amendments are 

effective on January 1, 2011. Section 

553(d) of the Administrative Procedure 

Act (APA), 5 U.S.C. Chapter 5, generally 

provides that rules may not take effect 

earlier than 30 days after they are 

published in the Federal Register. EPA 

is issuing this final rule under section 

307(d)(1) of the Clean Air Act, which 

states: ‘‘The provisions of section 553 

through 557 * * * of Title 5 shall not, 

except as expressly provided in this 

section, apply to actions to which this 

subsection applies.’’ Thus, section 

553(d) of the APA does not apply to this 

rule. EPA is nevertheless acting 

consistently with the purposes 

underlying APA section 553(d) in 

making this rule effective on January 1, 

2011. Section 5 U.S.C. 553(d)(3) allows 

an effective date less than 30 days after 

publication ‘‘as otherwise provided by 

the agency for good cause found and 

published with the rule.’’ As explained 

below, EPA finds that there is good 

cause for these rules to become effective 

on or before January 1, 2011, even if this 

date is not 30 days from date of 

publication in the Federal Register. 

While this action is being signed prior 

to December 1, 2010, there may be a 

delay in the publication of this rule as 

it contains many complex diagrams, 

equations, and charts, and is relatively 

long in length. The purpose of the 

30-day waiting period prescribed in 5 

U.S.C. 553(d) is to give affected parties 

a reasonable time to adjust their 

behavior and prepare before the final 

rule takes effect. Where, as here, the 

final rule will be signed and made 

available on the EPA website more than 

30 days before the effective date, but 

where the publication may be delayed 

due to the complexity and length of the 

rule, that purpose is still met. Moreover, 

since permitting authorities and 

regulated entities may need to rely on 

the methods described in these rules to 

carry out requirements of the SIP and 

NSR implementation rules that become 

effective on January 1, 2011 (see section 

III.C, infra), there would be unnecessary 

regulatory confusion if a publication 

delay caused this rule to become 

effective after January 1, 2011. 

Accordingly, we find good cause exists 

to make this rule effective on or before 

January 1, 2011, consistent with the 

purposes of 5 U.S.C. 553(d)(3).1

D. Judicial Review 

Under section 307(b)(1) of the Clean 

Air Act (CAA), judicial review of this 

final action is available only by filing a 

petition for review in the United States 

Court of Appeals for the District of 

Columbia Circuit by February 22, 2011. 

Under CAA section 307(b)(2), the 

requirements established by this action 

may not be challenged separately in any 

civil or criminal proceedings brought by 

EPA to enforce these requirements. 

Section 307(d)(7)(B) of the CAA 

further provides that ‘‘[o]nly an 

objection to a rule or procedure which 

was raised with reasonable specificity 

during the period for public comment 

(including any public hearing) may be 

raised during judicial review.’’ This 

section also provides a mechanism for 

EPA to convene a proceeding for 

reconsideration, ‘‘[i]f the person raising 

an objection can demonstrate to EPA 

that it was impracticable to raise such 

objection within [the period for public 

comment] or if the grounds for such 

objection arose after the period for 

public comment (but within the time 

specified for judicial review) and if such 

objection is of central relevance to the 

outcome of the rule.’’ Any person 

seeking to make such a demonstration to 

us should submit a Petition for 

Reconsideration to the Office of the 

Administrator, U.S. EPA, Room 3000, 


jlentini on DSKJ8SOYB1PROD with RULES2
80120 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

Ariel Rios Building, 1200 Pennsylvania 

Ave., NW., Washington, DC 20460, with 

a copy to both the person(s) listed in the 

preceding FOR FURTHER INFORMATION

CONTACT section, and the Associate 

General Counsel for the Air and 

Radiation Law Office, Office of General 

Counsel (Mail Code 2344A), U.S. EPA, 

1200 Pennsylvania Ave., NW., 

Washington, DC 20460. 

II. Background 

A. Why is EPA issuing this final action? 

Section 110 of the CAA, as amended 

(42 U.S.C. 7410), requires State and 

local air pollution control agencies to 

develop, and submit for EPA approval, 

State Implementation Plans (SIP) that 

provide for the attainment, 

maintenance, and enforcement of the 

NAAQS in each air quality control 

region (or portion thereof) within each 

State. The emissions inventories and 

analyses used in the State’s attainment 

demonstrations must consider PM10 and 

PM2.5 emissions from stationary sources 

that are significant contributors of 

primary PM10 and PM2.5 emissions. 

Primary or direct emissions are the solid 

particles or liquid droplets emitted 

directly from an air emissions source or 

activity, and the gaseous emissions or 

liquid droplets from an air emissions 

source or activity that condense to form 

PM or liquid droplets at ambient 

temperatures. 

Appendix A to subpart A of 40 CFR 

part 51 (Requirements for Preparation, 

Adoption, and Submittal of 

Implementation Plans) defines primary 

PM10 and PM2.5 as including both the 

filterable and condensable fractions of 

PM. Filterable PM consists of those 

particles that are directly emitted by a 

source as a solid or liquid at the stack 

(or similar release conditions) and 

captured on the filter of a stack test 

train. Condensable PM is the material 

that is in vapor phase at stack 

conditions but condenses and/or reacts 

upon cooling and dilution in the 

ambient air to form solid or liquid PM 

immediately after discharge from the 

stack. In response to the need to 

quantify primary PM10 and PM2.5

emissions from stationary sources, EPA 

previously developed and promulgated 

Method 201A (Determination of PM10

Emissions (Constant Sampling Rate 

Procedure)) and Method 202 

(Determination of Condensable 

Particulate Emissions from Stationary 

Sources) in 40 CFR part 51, appendix M 

(Recommended Test Methods for State 

Implementation Plans). 

On April 17, 1990 (56 FR 65433), EPA 

promulgated Method 201A in appendix 

M of 40 CFR part 51 to provide a test 

method for measuring filterable PM10

emissions from stationary sources. In 

EPA Method 201A, a gas sample is 

extracted at a constant flow rate through 

an in-stack sizing device that directs 

particles with aerodynamic diameters 

less than or equal to 10 μm to a filter. 

The particulate mass collected on the 

filter is determined gravimetrically after 

removal of uncombined water. 

On December 17, 1991 (56 FR 65433), 

EPA promulgated Method 202 in 

appendix M of 40 CFR part 51 to 

provide a test method for measuring 

CPM from stationary sources. Method 

202 uses water-filled impingers to cool, 

condense, and collect materials that are 

vaporous at stack conditions and 

become solid or liquid PM at ambient 

air temperatures. Method 202, as 

promulgated in 1991, contains several 

optional procedures that were intended 

to accommodate the various test 

methods used by State and local 

regulatory entities at the time Method 

202 was being developed. 

In this action, we are finalizing 

amendments to Methods 201A and 202 

to improve the measurement of fine PM 

emissions. For Method 201A, the final 

amendments add a particle-sizing 

device to allow for sampling of PM2.5

emissions. For Method 202, the final 

amendments will (1) revise the sample 

collection and recovery procedures of 

the method to reduce the potential for 

formation of reaction artifacts that are 

not related to the primary emission of 

CPM from the source but may be 

counted erroneously as CPM when 

using Method 202, and (2) eliminate 

most of the hardware and analytical 

options in the existing method. These 

changes increase the precision of 

Method 202 and improve the 

consistency in the measurements 

obtained between source tests 

performed under different regulatory 

authorities. 

B. Particulate Matter National Ambient 

Air Quality Standards 

Section 108 and 109 of the CAA 

govern the establishment and revision of 

the NAAQS. Section 108 of the CAA (42 

U.S.C. 7408) directs the Administrator 

to identify and list ‘‘air pollutants’’ that 

‘‘in his judgment, may reasonably be 

anticipated to endanger public health 

and welfare’’ and whose ‘‘presence 

* * * in the ambient air results from 

numerous or diverse mobile or 

stationary sources’’ and to issue air 

quality criteria for those that are listed. 

Air quality criteria are intended to 

‘‘accurately reflect the latest scientific 

knowledge useful in indicating the kind 

and extent of identifiable effects on 

public health or welfare which may be 

expected from the presence of [a] 

pollutant in ambient air * * *.’’ Section 

109 of the CAA (42 U.S.C. 7409) directs 

the Administrator to propose and 

promulgate primary and secondary 

NAAQS for pollutants listed under CAA 

section 108 to protect public health and 

welfare, respectively. Section 109 of the 

CAA also requires review of the NAAQS 

at 5-year intervals and that an 

independent scientific review 

committee ‘‘shall complete a review of 

the criteria * * * and the national 

primary and secondary ambient air 

quality standards * * * and shall 

recommend to the Administrator any 

new * * * standards and revisions of 

existing criteria and standards as may be 

appropriate * * *.’’ Since the early 

1980s, this independent review function 

has been performed by the Clean Air 

Scientific Advisory Committee. 

Initially, EPA established the PM 

NAAQS on April 30, 1971 (36 FR 8186), 

based on the original criteria document 

(Department of Health, Education, and 

Welfare, 1969). The reference method 

specified for determining attainment of 

the original standards was the highvolume sampler, which collects PM up 

to a nominal size of 25 to 45 μm 

(referred to as total suspended 

particulates or TSP). On October 2, 1979 

(44 FR 56730), EPA announced the first 

periodic review of the air quality criteria 

and PM NAAQS, and significant 

revisions to the original standards were 

promulgated on July 1, 1987 (52 FR 

24634). In that decision, EPA changed 

the indicator for particles from TSP to 

PM10. When that rule was challenged, 

the court upheld revised standards in all 

respects. Natural Resources Defense 

Council v. Administrator, 902 F. 2d 962 

(D.C. Cir. 1990, cert. denied, 498 U.S. 

1082 (1991). 

In April 1994, EPA announced its 

plans for the second periodic review of 

the air quality criteria and PM NAAQS, 

and the Agency promulgated significant 

revisions to the NAAQS on July 18, 

1997 (62 FR 38652). In that decision, 

EPA revised the PM NAAQS in several 

respects. While EPA determined that the 

PM NAAQS should continue to focus on 

particles less than or equal to 10 μm in 

diameter (PM10), EPA also determined 

that the fine and coarse fractions of 

PM10 should be considered separately. 

EPA added new standards, using PM2.5

as the indicator for fine particles (with 

PM2.5 referring to particles with a 

nominal mean aerodynamic diameter 

less than or equal to 2.5 μm), and using 

PM10 as the indicator for purposes of 

regulating the coarse fraction of PM10. 

Following promulgation of the 1997 

PM NAAQS, petitions for review were 

filed by a large number of parties 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80121 

addressing a broad range of issues. In 

May 1999, a three-judge panel of the 

U.S. Court of Appeals for the District of 

Columbia Circuit issued an initial 

decision that upheld EPA’s decision to 

establish fine particle standards. 

American Trucking Associations v. 

EPA, 175 F.3d 1027, 1055 (D.C. Cir. 

1999), reversed in part on other grounds 

in Whitman v. American Trucking 

Associations, 531 U.S. 457 (2001). The 

panel also found ‘‘ample support’’ for 

EPA’s decision to regulate coarse 

particle pollution, but vacated the 1997 

PM10 standards concluding that EPA 

had not provided a reasonable 

explanation justifying use of PM10 as an 

indicator for coarse particles. (Id. at 

1054–55.) Pursuant to the court’s 

decision, EPA removed the vacated 

1997 PM10 standards but retained the 

pre-existing 1987 PM10 standards (65 FR 

80776, December 22, 2000). 

On October 23, 1997, EPA published 

its plans for the third periodic review of 

the air quality criteria and PM NAAQS 

(62 FR 55201), including the 1997 PM2.5

standards and the 1987 PM10 standards. 

On October 17, 2006, EPA issued its 

final decision to revise the primary and 

secondary PM NAAQS to provide 

increased protection of public health 

and welfare respectively (71 FR 61144). 

With regard to the primary and 

secondary standards for fine particles, 

EPA revised the level of the 24-hour 

PM2.5 standard to 35 μg per cubic meter 

(μg/m3), retained the level of the annual 

PM2.5 annual standard at 15 μg/m3, and 

revised the form of the annual PM2.5

standard by narrowing the constraints 

on the optional use of spatial averaging. 

With regard to the primary and 

secondary standards for PM10, EPA 

retained the 24-hour PM10 standard (150 

μg/m3) and revoked the annual standard 

because available evidence generally 

did not suggest a link between long-term 

exposure to current ambient levels of 

coarse particles and health or welfare 

effects. 

C. Measuring PM Emissions 

Section 110 of the CAA, as amended 

(42 U.S.C. 7410), requires State and 

local air pollution control agencies to 

develop and submit plans (SIP) for EPA 

approval that provide for the 

attainment, maintenance, and 

enforcement of the NAAQS in each air 

quality control region (or portion 

thereof) within such State. 40 CFR part 

51 (Requirements for Preparation, 

Adoption, and Submittal of 

Implementation Plans) specifies the 

requirements for SIP. Appendix A to 

subpart A of 40 CFR part 51, defines 

primary PM10 and PM2.5 as including 

both the filterable and condensable 

fractions of PM. Filterable PM consists 

of those particles directly emitted by a 

source as a solid or liquid at the stack 

(or similar release conditions) and 

captured on the filter of a stack test 

train. Condensable PM is the material 

that is in vapor phase at stack 

conditions but which condenses and/or 

reacts upon cooling and dilution in the 

ambient air to form solid or liquid PM 

immediately after discharge from the 

stack. 

Promulgation of the 1987 NAAQS 

created the need for methods to quantify 

PM10 emissions from stationary sources. 

In response, EPA developed and 

promulgated the following test methods: 

• Method 201A—Determination of 

PM10 Emissions (Constant Sampling 

Rate Procedure), and 

• Method 202—Determination of 

Condensable Particulate Emissions from 

Stationary Sources. 

1. Method 201A 

Method 201A is a test method for 

measuring filterable PM10 emissions 

from stationary sources. With the 

exception of the PM10-sizing device, the 

current Method 201A sampling train is 

the same as the sampling train used for 

EPA Method 17 of appendix A–3 to 40 

CFR part 60. 

Method 201A cannot be used to 

measure emissions from stacks that have 

entrained moisture droplets (e.g., from a 

wet scrubber stack) since these stacks 

may have water droplets that are larger 

than the cut size of the PM10 sizing 

device. The presence of moisture would 

prevent an accurate measurement of 

total PM10 since any PM10 dissolved in 

larger water droplets would not be 

collected by the sizing device and 

would consequently be excluded in 

determining total PM10 mass. To 

measure PM10 in stacks where water 

droplets are known to exist, EPA’s 

Technical Information Document 09 

(Methods 201 and 201A in Presence of 

Water Droplets) recommends use of 

Method 5 of appendix A–3 to 40 CFR 

part 60 (or a comparable method) and 

consideration of the total particulate 

catch as PM10 emissions. 

Method 201A is also not applicable 

for stacks with small diameters (i.e., 18 

inches or less). The presence of the instack nozzle/cyclones and filter 

assembly in a small duct will cause 

significant cross-sectional area 

interference and blockage leading to 

incorrect flow calculation and particle 

size separation. Additionally, the type 

of metal used to construct the Method 

201A cyclone may limit the 

applicability of the method when 

sampling at high stack temperatures 

(e.g., stainless steel cyclones are 

reported to gall and seize at 

temperatures greater than 260 °C). 

2. Method 202 

Method 202 measures CPM from 

stationary sources. Method 202 contains 

several optional procedures that were 

intended to accommodate the various 

test methods used by State and local 

regulatory entities at the time Method 

202 was being developed. 

When conducted consistently and 

carefully, Method 202 provides 

acceptable precision for most emission 

sources. Method 202 has been used 

successfully in regulatory programs 

where the emission limits and 

compliance demonstrations are 

established based on a consistent 

application of the method and its 

associated options. However, when the 

same emission source is tested using 

different combinations of the optional 

procedures, there appears to be large 

variations in the measured CPM 

emissions. Additionally, during 

validation of the promulgated method, 

we determined that sulfur dioxide (SO2) 

gas (a typical component of emissions 

from several types of stationary sources) 

can be absorbed partially in the 

impinger solutions and can react 

chemically to form sulfuric acid. This 

sulfuric acid ‘‘artifact’’ is not related to 

the primary emission of CPM from the 

source, but may be counted erroneously 

as CPM when using Method 202. We 

consistently maintain that the artifact 

formation can be reduced by at least 90 

percent if a one-hour nitrogen purge of 

the impinger water is used to remove 

SO2 before it can form sulfuric acid (this 

is our preferred application of the 

Method 202 optional procedures). 

Inappropriate use or omission of the 

preferred or optional procedures in 

Method 202 can increase the potential 

for artifact formation. 

Considering the potential for 

variations in measured CPM emissions, 

we believe that further verification and 

refinement of Method 202 is appropriate 

to minimize the potential for artifact 

formation. We performed several studies 

to assess artifact formation when using 

Method 202. The results of our 1998 

laboratory study and field evaluation 

commissioned to evaluate the impinger 

approach can be found in ‘‘Laboratory 

and Field Evaluation of EPA’s Method 

5 Impinger Catch for Measuring 

Condensible Matter from Stationary 

Sources’’ at http://www.epa.gov/ttn/ 

emc/methods/m202doc1.pdf. 

The 1998 study verified the need for 

a nitrogen purge when SO2 is present in 

stack gas and provided guidance for 

analyzing the collected samples. In 

2005, an EPA contractor conducted a 


jlentini on DSKJ8SOYB1PROD with RULES2
80122 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

second study, ‘‘Laboratory Evaluation of 

Method 202 to Determine Fate of SO2 in 

Impinger Water,’’ that replicated some of 

the earlier EPA work and addressed 

some additional issues. The report of 

that work is available at http:// 

www.epa.gov/ttn/emc/methods/ 

m202doc2.pdf. This report also verified 

the need for a nitrogen purge and 

identified the primary factors that affect 

artifact formation. 

Also in 2005, a private testing 

contractor presented a possible minor 

modification to Method 202 at the Air 

and Waste Management Association 

(AWMA) specialty conference. The 

proposed modification, as described in 

their presentation titled ‘‘Optimized 

Method 202 Sampling Train to 

Minimize the Biases Associated with 

Method 202 Measurement of 

Condensable Particulate Matter 

Emissions,’’ involved the elimination of 

water from the first impingers. The 

presentation (available at http:// 

www.epa.gov/ttn/emc/methods/ 

m202doc3.pdf) concluded that 

modification of the promulgated method 

to use dry impingers resulted in a 

significant additional reduction in the 

sulfate artifact. 

In 2006, we began to conduct 

laboratory studies in collaboration with 

several stakeholders to characterize the 

artifact formation and other 

uncertainties associated with 

conducting Method 202 and to identify 

procedures that would minimize 

uncertainties when using Method 202. 

Since August 2006, we conducted two 

workshops in Research Triangle Park, 

NC to present and request comments on 

our plan for evaluating potential 

modifications to Method 202 that would 

reduce artifact formation, and also to 

discuss (1) Our progress in 

characterizing the performance of the 

modified method, (2) issues that require 

additional investigation, (3) the results 

of our laboratory studies, and (4) our 

commitments to extend the 

investigation through stakeholders 

external to EPA. Another meeting was 

held with experienced stack testers and 

vendors of emissions monitoring 

equipment to discuss hardware issues 

associated with modifications of the 

sampling equipment and the glassware 

for the proposed CPM test method. 

Summaries of the method evaluations, 

as well as meeting minutes from our 

workshops, can be found at http:// 

www.epa.gov/ttn/emc/methods/ 

method202.html. 

The laboratory studies that were 

performed fulfill a commitment in the 

preamble to the Clean Air Fine Particle 

Implementation Rule (72 FR 20586, 

April 25, 2007) to examine the 

relationship between several critical 

CPM sampling and analysis parameters 

and, to the extent necessary, promulgate 

revisions to incorporate improvements 

in the method. While these 

improvements in the stationary source 

test method for CPM will provide for 

more accurate and precise measurement 

of all PM, the addition of PM2.5 as an 

indicator of health and welfare effects 

by the 1997 NAAQS revisions generates 

the need to quantify PM2.5 emissions 

from stationary sources. To respond to 

this need, we are promulgating revisions 

to incorporate this capability into the 

test method for filterable PM10. 

III. Summary of Changes Since 

Proposal 

The methods in this final action 

contain several changes that were made 

as a result of public comments. The 

following sections present a summary of 

the changes to the methods. We explain 

the reasons for these changes in detail 

in the Summary of Public Comments 

and Responses section of this preamble. 

A. Method 201A 

Method 201A contains the following 

changes and clarifications: 

• Revised Section 1.5 to clarify that 

Method 201A cannot be used to 

measure emissions from stacks that have 

entrained moisture droplets (e.g., from a 

wet scrubber stack). 

• Removed the language in proposed 

Section 1.5 regarding ambient air 

contributions to PM. The decision to 

correct results for ambient air 

contributions is up to the permitting or 

regulatory authority. 

• Added definitions of Primary PM, 

Filterable PM, Primary PM2.5, Primary 

PM10, and CPM to Section 3.0. 

• Added a requirement to Sections 

6.1.3 and 8.6.3 stating that the filter 

must not be compressed between the 

gasket and the filter housing. 

• Clarified the sample recovery and 

analysis equipment in Section 6.2, 

including acceptable materials of 

construction, analytical balance, and 

fluoropolymer (polytetrafluoroethylene) 

beaker liners. 

• Revised Section 6.2 to add 

performance-based, residual mass 

contribution specifications for 

containers rather than specifying the 

type of container that must be used 

(storage containers must not contribute 

more than 0.1 mg of residual mass to the 

CPM measurements). 

• Revised Section 8.3.1 (regarding 

sampling ports) to state that a 4-inch 

port should be adequate for the single 

PM2.5 (or single PM10) sampling 

apparatus. However, testers will not be 

able to use conventional 4-inch ports if 

the combined dimension of the PM10

cyclone and the nozzle extending from 

the cyclone exceeds the internal 

diameter of the port. 

• Clarified the sampling procedures 

in Section 8.3.1 for cases where the 

PM2.5 cyclone is used without the PM10

cyclone. In these cases, samples are 

collected using the procedures specified 

in Section 11.3.2.2 of EPA Method 1, 

and the sampling time is extended at the 

replacement sampling point to include 

the duration of the unreachable traverse 

points. 

• Revised Section 8.3.2.2 to clarify 

that Method 201A is not applicable for 

stack diameters less than 26.5 inches 

when the combined PM10/PM2.5 cyclone 

is used. The in-stack nozzle/cyclones 

and filter assembly in stacks less than 

26.5 inches in diameter would cause 

significant cross-sectional area 

interference and blockage, leading to 

incorrect flow calculation and particle 

size separation. 

• Revised Section 8.5.5 to express the 

maximum failure rate of values outside 

the minimum-maximum velocity 

pressure range in terms of percent of 

values outside the range instead of the 

number of traverse points outside the 

range. 

• Revised section 8.6.1 to clarify that 

alternative designs are acceptable for 

fastening caps or covers to cyclones to 

avoid galling of the cyclone component 

threads in hot stacks. The method may 

be used at temperatures up to 1,000°F 

using stainless steel cyclones that are 

bolted together, rather than screwed 

together. Using ‘‘break-away’’ stainless 

steel bolts facilitates disassembly and 

circumvents the problem of thread 

galling. 

• Clarified sampling procedures in 

Section 8.7.3.3 to maintain the 

temperature of the cyclone sampling 

head within ± 10 °C of the stack 

temperature and to maintain flow until 

after removing and before inserting the 

sampling head. 

• Revised Section 11.2.7 to allow the 

use of tared fluoropolymer beaker liners 

for the acetone field reagent blank. 

B. Method 202 

Method 202 contains the following 

changes and clarifications: 

• Clarified the terminology used to 

refer to laboratory and field blanks 

throughout the method. 

• For health and safety reasons, 

replaced the use of methylene chloride 

with hexane throughout the method. 

• Clarified Section 1.2 by moving the 

discussion of filterable PM methods 

used in conjunction with Method 202 to 

Section 1.5. 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80123 

• Clarified Section 1.6 to specify that 

Method 202 can be used for measuring 

CPM in stacks that contain entrained 

moisture if the sampling temperature is 

sufficiently high to keep the moisture in 

the vapor phase. 

• Moved the recommendation to 

develop a health and safety plan from 

Section 9.4 to Section 5.0. 

• Added amber glass bottles to the list 

of sample recovery equipment in 

Section 6.2. 

• Added alternatives (fluoropolymer 

beaker liners or fluoropolymer baggies) 

to weighing tins to the list of analytical 

equipment in Section 6.2.2 (Section 6.3 

of the proposed method). 

• Added specifications for sample 

drying equipment in Section 6.2.2 

(Section 6.3 of the proposed method). 

• Clarified Section 6.3.7 regarding the 

use of an analytical balance with 

sensitivity to 0.00001 g (0.01 milligram). 

• Added an option to use a 

colorimetric pH indicator instead of a 

pH meter in Section 6.2.2 (Section 6.3 

of the proposed method). 

• Added a sonication device to the 

list of analytical equipment in Section 

6.2.2 (Section 6.3 of the proposed 

method). 

• Added performance-based, residual 

mass contribution specifications for 

containers and wash bottles in Section 

6.2.2 (Section 6.3 of the proposed 

method) rather than specifying the type 

of container that must be used. 

• Replaced the prescriptive language 

regarding filter materials in Section 

7.1.1 with performance-based 

requirements limiting the residual mass 

contribution. 

• Replaced the prescriptive language 

regarding water quality in Section 7.1.3 

with performance-based requirements 

for residual mass content. 

• Clarified Section 8.2 to specify that 

cleaned glassware must be used at the 

start of each new source category tested 

at a single facility. 

• Added a performance-based option 

to Section 8.4 to conduct a field train 

proof blank rather than meeting the 

glassware baking requirements in 

Section 8.2. 

• Clarified the sampling train 

configuration for the nitrogen purge 

procedures in Section 8.5.3.2 regarding 

pressurized purges. 

C. How will the final amendments to 

methods 201A and 202 affect existing 

emission inventories, emission 

standards, and permit programs? 

We anticipate that over time the 

changes in the test methods finalized in 

this action will result in, among other 

positive outcomes, more accurate 

emissions inventories of direct PM 

emissions and emissions standards that 

are more indicative of the actual impact 

of the source on the ambient air quality. 

Accurate emission inventories are 

critical for regulatory agencies to 

develop the control strategies and 

demonstrations necessary to attain air 

quality standards. When implemented, 

the test method revisions should 

improve our understanding of PM 

emissions due to the increased 

availability of more accurate emission 

tests and eventually through the 

incorporation of less biased test data 

into existing emissions factors. For 

CPM, the use of the revised method 

could reveal a reduced level of CPM 

emissions from a source compared to 

the emissions that would have been 

measured using Method 202 as typically 

performed. However, there may be some 

cases where the revised test method 

would reveal an increased level of CPM 

emissions from a source, depending on 

the relative emissions of filterable and 

CPM emissions from the source. For 

example, the existing Method 202 

allows complete evaporation of the 

water containing inorganic PM at 105 °C 

(221 °F), where the revised method 

requires the last 10 ml of the water to 

be evaporated at room temperature (not 

to exceed 30 °C (85 °F)), thereby 

retaining the CPM that would evaporate 

at the increased temperature. 

Prior to our adoption of the 1997 

PM2.5 NAAQS, several State and local 

air pollution control agencies had 

developed emission inventories that 

included CPM. Additionally, some 

agencies established enforceable CPM 

emissions limits or otherwise required 

that PM emissions testing include 

measurement of CPM. While this 

approach was viable in cases where the 

same test method was used to develop 

the CPM regulatory limits and to 

demonstrate facility compliance, there 

are substantial inconsistencies within 

and between States regarding the 

completeness and accuracy of CPM 

emission inventories and the test 

methods used to measure CPM 

emissions and demonstrate facility 

compliance. 

These amendments would serve to 

mitigate the potential difficulties that 

can arise when EPA and other 

regulatory entities attempt to use the 

test data from State and local agencies 

with inconsistent CPM test methods to 

develop emission factors, determine 

program applicability, or to establish 

emissions limits for CPM emission 

sources within a particular jurisdiction. 

For example, problems can arise when 

the test method used to develop a CPM 

emission limit is not the same as the test 

method specified in the rule for 

demonstrating compliance because the 

different test methods may quantify 

different components of PM (e.g., 

filterable versus condensable). Also, 

when emissions from State inventories 

are modeled to assess compliance with 

the NAAQS, the determination of direct 

PM emissions may be biased high or 

low, depending on the test methods 

used to estimate PM emissions, and the 

atmospheric conversion of SO2 to 

sulfates (or sulfur trioxide, SO3) may be 

inaccurate or double-counted. 

Additionally, some State and local 

regulatory authorities have assumed that 

EPA Method 5 of appendix A–3 to 40 

CFR part 60 (Determination of 

Particulate Matter Emissions from 

Stationary Sources) provides a 

reasonable estimate of PM10 emissions. 

This assumption is incorrect because 

Method 5 does not provide particle 

sizing of the filterable component and 

does not quantify particulate caught in 

the impinger portion of the sampling 

train. Similar assumptions for 

measurements of PM2.5 will result in 

greater inaccuracies. 

With regard to State permitting 

programs, we recognize that, in some 

cases, existing best available control 

technology, lowest achievable emission 

rate, or reasonably available control 

technology limits have been based on an 

identified control technology, and that 

the data used to determine the 

performance of that technology and to 

establish the limits may have focused on 

filterable PM and, thus, did not 

completely characterize PM emissions 

to the ambient air. While the source test 

methods used by State programs that 

developed the applicable permit limit 

may not have fully characterized the PM 

emissions, we have no information that 

would indicate that the test methods are 

inappropriate indicators of the control 

technologies’ performance for the 

portion of PM emissions that was 

addressed by the applicable 

requirement. As promulgated in the 

Clean Air Fine Particle Implementation 

Rule, after January 1, 2011, States are 

required to consider inclusion of CPM 

emissions in new or revised emissions 

limits that they establish. We will defer 

to the individual State’s judgment as to 

whether, and at what time it is 

appropriate to revise existing facility 

emission limits or operating permits to 

incorporate information from the 

revised CPM test method when it is 

promulgated. 

With regard to operating permits, the 

title V permit program does not 

generally impose new substantive air 

quality control requirements. In general, 

after emissions limits are established as 

CAA requirements under the SIP or a 


jlentini on DSKJ8SOYB1PROD with RULES2
80124 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

SIP-approved pre-construction review 

permit, they are included in the title V 

permits. Obviously, title V permits 

should be updated to reflect any 

revision of existing emission limits or 

new emission limits created in the 

context of the underlying applicable 

requirements. Also, if a permit contains 

previously promulgated test methods, it 

is not a given that the permit would 

always have to be revised should these 

test method changes be finalized (e.g., 

where test methods are incorporated 

into existing permits through 

incorporation by reference, no permit 

terms or conditions would necessarily 

have to change to reflect changes to 

those test methods). In any event, the 

need for action related to emissions 

source permitting, due to these changes 

to the test methods, would be 

determined based upon several factors 

such as the exact wording of the existing 

operating permit, the requirements of 

the EPA-approved SIP, and any changes 

that may need to be made to preconstruction review permits with 

respect to CPM measurement (e.g., 

emissions estimates may be based upon 

a source test method that did not 

measure CPM or upon a set of Method 

202 procedures that underestimated 

CPM emissions). 

In recognition of these issues, the 

Clean Air Fine Particle Implementation 

Rule contains provisions establishing a 

transition period for developing 

emission limits for condensable direct 

PM2.5 that are needed to demonstrate 

attainment of the PM2.5 NAAQS. The 

transition period for CPM is the time 

period during which the new rules and 

NSR permits issued to stationary 

sources are not required to address the 

condensable fraction of the sources’ PM 

emissions. The end date of the 

transition period (January 1, 2011) was 

adopted in the final Clean Air Fine 

Particle Implementation Rule (72 FR 

20586, April 25, 2007) and in the final 

Implementation of the New Source 

Review Program for Particulate Matter 

Less Than 2.5 Micrometers (PM2.5) rule 

(73 FR 28321, May 16, 2008). As 

discussed in these two rules, the intent 

of the transition period (which ends 

January 1, 2011) was to allow time for 

EPA to issue a CPM test method through 

notice and comment rulemaking, and 

for sources and States to collect 

additional total primary (filterable and 

condensable) PM2.5 emissions data to 

improve emissions information to the 

extent possible. In the PM2.5 NSR 

Implementation Rule, we stated that as 

part of this test methods rulemaking, we 

would ‘‘take comment on an earlier 

closing date for the transition period in 

the NSR program if we are on track to 

meet our expectation to complete the 

test method rule much earlier than 

January 1, 2011’’ (73 FR 28344). In the 

notice of proposed rulemaking for this 

final rule on amendments to Method 

201A and 202, EPA sought comment on 

whether to end the NSR transition 

period for CPM early (74 FR 12976). In 

this final rule, EPA is taking no action 

to affect the already established January 

1, 2011 sunset date for the NSR 

transition period. 

Source test data collected with the use 

of this updated test method will be 

incorporated into the tools (e.g., 

emission factors, emission inventories, 

air quality modeling) used to 

demonstrate the attainment of air 

quality standards. Areas that are 

designated nonattainment for the 1997 

PM2.5 NAAQS, and that have approved 

attainment dates of 2014 or 2015, are 

required to develop a mid-course review 

in 2011. If it is determined that 

additional control measures are needed 

to ensure the area will be on track to 

attain the standard by the attainment 

date, any new direct PM2.5 emission 

limits adopted by the State must address 

the condensable fraction and the 

filterable fraction of PM2.5. Additionally, 

the new test data could be used to 

improve the applicability and 

performance evaluations of various 

control technologies. 

IV. Summary of Final Methods 

A. Method 201A 

Method 201A measures PM emissions 

from stationary sources. The 

amendments to Method 201A add a 

PM2.5 measurement device (PM2.5

cyclone) that allows the method to 

measure filterable PM2.5, filterable PM10, 

or both filterable PM2.5 and filterable 

PM10. The method can also be used to 

measure coarse particles (i.e., the 

difference between measured PM10

concentration and the measured PM2.5

concentration). 

The amendments also add a PM2.5

cyclone to create a sampling train that 

includes a total of two cyclones (one 

cyclone to segregate particles with 

aerodynamic diameters greater than 10 

μm and one cyclone to segregate 

particles with aerodynamic diameters 

greater than 2.5 μm) and a final filter to 

collect particles with aerodynamic 

diameters less than or equal to 2.5 μm. 

The PM2.5 cyclone is inserted between 

the PM10 cyclone and the filter of the 

Method 201A sampling train. 

The revised method has several 

limitations. The method cannot be used 

to measure emissions from stacks that 

have entrained moisture droplets (e.g., 

from a wet scrubber stack) because size 

separation of the water droplets is not 

representative of the dry particle size 

released into the air. In addition, the 

method is not applicable for stacks with 

diameters less than 25.7 inches when 

the combined PM10/PM2.5 cyclone is 

used. Also, the method may not be 

suitable for sources with stack gas 

temperatures exceeding 260 °C (500 °F) 

when cyclones with screw-together caps 

are used because the threads of the 

cyclone components may gall or seize, 

thus preventing the recovery of the 

collected PM. However, the method may 

be used at temperatures up to 1,000 °F 

when using stainless steel cyclones that 

are bolted together rather than screwed 

together. Using ‘‘break-away’’ stainless 

steel bolts facilitates disassembly and 

circumvents the problem of thread 

galling. The method may also be used at 

temperatures up to 2,500 °F when using 

specialty high-temperature alloys. 

B. Method 202 

Method 202 measures concentrations 

of CPM in stationary source sample gas 

after the filterable PM has been removed 

using another test method such as 

Method 5, 17, or 201A. The CPM 

sampling train begins at the back half of 

the filterable PM filter holder and 

consists of a condenser, two dry 

impingers (temperatures maintained to 

less than 30 °C (85 °F)), and a CPM filter 

(temperature maintained between 20 °C 

(65 °F) and 30 °C (85 °F)). During the 

test, sample gases are cooled and CPM 

is collected in the dry impingers and on 

the CPM filter. As soon as possible after 

the post-test leak check has been 

conducted, any water collected in the 

dry impingers is purged with nitrogen 

gas for at least one hour to remove 

dissolved SO2 gas. 

After the nitrogen purge, the sampling 

train components downstream of the 

filterable PM filter (i.e., the probe 

extension (if any), condenser, 

impingers, front half of CPM filter 

holder, and the CPM filter) are rinsed 

with water to recover the inorganic 

CPM. The water rinse is followed by an 

acetone rinse and a hexane rinse to 

recover the organic CPM. The CPM filter 

is extracted using water to recover the 

inorganic components and hexane to 

recover the organic portion. The 

inorganic and organic fractions are then 

dried and the residues weighed. The 

sum of both fractions represents the 

total CPM collected by Method 202. 

V. Summary of Public Comments and 

Responses 

In response to the March 25, 2009 

proposed revisions to EPA Methods 

201A and 202, EPA received public 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80125 

comment letters from industry 

representatives, trade associations, State 

agencies, and environmental 

organizations. The public comments 

submitted to EPA addressed the 

proposed revisions to Methods 201A 

and 202 and our request for comments 

on whether to end the transition period 

for CPM in the NSR program on a date 

earlier than the current end date of 

January 1, 2011. 

This section provides responses to the 

more significant public comments 

received on the proposed revisions to 

Methods 201A and 202. Summaries and 

responses for all comments related to 

the proposed revisions to Methods 201A 

and 202, including those addressed in 

this preamble, are contained in the 

response to comments document 

located in the docket for this final action 

(Docket ID No. EPA–HQ–OAR–2008– 

0348). 

A. Method 201A 

1. Speciation 

Comment: One commenter stated that 

EPA should include guidance in 

Method 201A concerning speciation of 

the constituents present in the PM10, 

PM10–PM2.5, and PM2.5 size fractions. 

The commenter believes this 

information should be provided to 

support the use of speciated PM10, 

PM10–PM2.5, and PM2.5 data in source 

apportionment studies. 

Response: EPA did not revise the 

method to provide guidance for 

speciation of various particle fractions 

for source apportionment because 

Method 201A is not a speciation 

method. However, with judicious 

selection of filter media, sources may 

use this method for speciating the less 

volatile metals and use these data in 

source apportionment studies. Including 

details to adapt this method for 

speciation analysis would unduly 

increase the complexity of the method 

without increasing the precision of the 

mass measurements. 

2. Catch Weight and Sampling Times 

Comment: Several commenters 

requested that EPA specify the 

minimum solids catch weights needed 

in the PM10 and PM2.5 size fractions to 

help testing organizations determine the 

necessary sampling times, especially for 

sources with low PM concentrations. 

Other commenters expressed concern 

about extended sampling times that 

would be necessary to obtain enough 

sample to weigh accurately. One 

commenter stated that a reasonable limit 

must be put on sampling volume to 

limit potentially unnecessary sampling 

time and exorbitant stack testing costs 

that could quickly escalate with such a 

requirement. 

Response: We agree with the 

commenters that collecting sufficient 

weighable mass is important for the 

method to be precise. We also 

understand that the sampling rate used 

to attain the cyclone cut-points is 

typically less than the rate used during 

Method 5 sampling. However, EPA did 

not revise the method to dictate a 

minimum sampling volume or 

minimum catch weight that would be 

necessary to obtain a valid sample. One 

reason for not specifying a minimum 

sampling volume or minimum catch 

weight is that different regulatory 

authorities and testing programs have 

differing measurement goals. For 

example, some regulatory authorities 

will accept less precision if results are 

well below compliance limits. State 

agencies or individual regulated 

facilities may develop data quality 

objectives (DQO) for the test program, 

which may specify minimum detection 

limits, and/or minimum sample volume, 

and/or catch weight that would 

demonstrate that DQO can be met. Stack 

samplers should take into consideration 

the compliance limits set by their 

regulatory authority and determine the 

minimum amount of stack gas needed to 

show compliance if the mass of 

particulate is below the detection limit. 

Stack testers can use the minimum 

detection limit to determine the 

minimum stack gas volume. The stack 

tester may be able to estimate the 

necessary stack gas volume based on 

how much PM the source or source 

category is expected to emit (which 

could be determined from a previous 

test or from knowledge of the emissions 

for that source category). 

Alternatively, the minimum detection 

limit for a source can be determined by 

calculating the percent relative standard 

deviation for a series of field train 

recovery blanks. You will not be able to 

measure below the average train 

recovery blank level, and EPA 

recommends calculating a tester-specific 

detection limit by multiplying the 

standard deviation of field recovery 

train blanks by the appropriate 

‘‘Student’s t value’’ (e.g., for seven field 

train recovery blanks, the standard 

deviation of the results would be 

multiplied by three). Short of having 

Method 201A field recovery train blanks 

for cyclone and filter components of the 

sampling train, you may use the 

detection limit determined from EPA 

field tests. 

An estimated detection limit was 

determined from an EPA field 

evaluation of proposed Method 201A 

(see ‘‘Field Evaluation of an Improved 

Method for Sampling and Analysis of 

Filterable and Condensable PM,’’ Docket 

ID No. EPA–HQ–OAR–2008–0348). The 

estimated detection limit was calculated 

from the standard deviation of the 

differences from 10 quadruplicate 

sampling runs multiplied by the 

appropriate ‘‘Student’s t value’’ (n¥1 = 

9). Detection limits determined in this 

manner were (1) Total filterable PM: 

2.54 mg; (2) PM10: 1.44 mg; and (3) 

PM2.5: 1.35. These test runs showed 

more filterable particulate in the PM2.5

fraction, and total filterable particulate 

detection limits may be biased high due 

to the small particulate mass collected 

in the fraction greater than PM10. 

Comment: Two commenters 

questioned the use of reference methods 

to correct for ambient air in Section 1.5 

of the proposed Method 201A. One 

commenter believed that the statement 

would be used as a means to blame noncompliance on ambient contributions 

and would result in legal challenges and 

disputes of test results. The other 

commenter questioned whether it was 

the intent of EPA to not allow the use 

of the CPM test method for lowtemperature sources. 

Response: We agree with the 

commenters that Section 1.5 of the 

proposed method was unclear. Thus, 

Section 1.5 (Additional Methods) has 

been removed from the final method. 

For sources that have very low PM 

emissions, such as processes that burn 

clean fuels (e.g., natural gas) and/or use 

large volumes of dilution air (e.g., gas 

turbines and thermal oxidizers), any 

ambient air particulate introduced into 

the process operation could be a large 

component of total outlet PM emissions. 

However, the decision to correct results 

for fine PM measurements to account for 

ambient air contributions is up to the 

permitting or regulatory authority. It is 

likely that these adjustments would be 

limited to gas turbines and possibly 

sources fired with clean natural gas. 

Comment: Commenters expressed 

concern about the lack of a test method 

to measure PM2.5 in stacks with 

entrained moisture. Another commenter 

urged EPA to continue work to identify 

or develop a method for measuring 

filterable (or total) PM at sources with 

entrained moisture droplets in the stack 

(e.g., units with wet stacks due to wet 

flue gas desulfurization or wet 

scrubbers). Commenters requested that 

EPA provide guidance or identify a 

viable alternative for high-moisture 

stacks as soon as possible. One 

commenter stated that when conducting 

emission testing at facilities with similar 

wet stack conditions as described in the 

proposal preamble (74 FR 12973), that 

they support EPA’s position on the 


jlentini on DSKJ8SOYB1PROD with RULES2
80126 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

limitations of the proposed Method 

201A. 

One commenter was not satisfied with 

the use of Method 5 as the only 

acceptable method for sources with 

entrained water droplets. To provide 

more accurate emissions data for 

sources with ‘‘wet’’ stacks, the 

commenter is sponsoring the 

development of an advanced manual 

sampling technique that can accurately 

measure filterable PM2.5 in stacks with 

entrained water droplets. The 

commenter expects to complete field 

tests of this method in the near future. 

The commenter will share laboratory 

and field test evaluations of this new 

method. The commenter believes that 

this new method for filterable PM2.5

emissions in ‘‘wet’’ stacks will be highly 

compatible with proposed Method 201A 

for filterable PM2.5 emission testing in 

‘‘dry’’ stacks. 

Response: We are currently 

developing a method to measure PM in 

stacks with saturated water vapors and 

laboratory testing is ongoing. EPA has 

committed a significant budget and 

personnel to developing an acceptable 

method for sources with wet stacks and 

we plan to offer the method and 

protocol as soon as possible. EPA’s 

method development and evaluation is 

focused on the ‘‘Dried Particle Method’’ 

(See ‘‘Lab Work to Evaluate PM2.5

Collection with a Dilution Monitoring 

Device for Data Gathering for Emission 

Factor Development (Final Report)’’ in 

Docket ID No. EPA–HQ–OAR–2008– 

0348) that directly measures the mass 

emission rate of particles with specified 

aerodynamic size. In the meantime, the 

promulgated amendments to Methods 

201A and 202 improve their 

performance and reduce known 

artifacts. Testers should use these final, 

amended methods until a PM2.5 method 

for stack gases containing water droplets 

is promulgated. 

Regarding the advanced manual 

sampling technique that the commenter 

is currently developing for use in ‘‘wet’’ 

stacks, EPA acknowledges the sampling 

evaluations being conducted by the 

commenter. When the data become 

available, we will review the data to 

determine if the consistency and 

performance achieved by the advanced 

manual sampling technique referenced 

by the commenter are comparable to 

EPA’s wet-stack sampling method 

currently under development. If the data 

are comparable, we will consider 

whether the commenter’s sampling 

technique should be addressed (e.g., as 

an alternative method) when we 

propose an EPA wet-stack, particlesizing method in the future. 

Comment: Several commenters 

disagreed with EPA’s recommendation 

to use Method 5 on stacks with 

entrained moisture and to consider all 

the collected mass to be PM2.5. 

Commenters stated that the 

categorization of all PM measured by 

Method 5 as PM2.5 overstates the true 

emissions. One commenter supported 

EPA’s recommendation to use Method 5 

to determine PM10/PM2.5 filterable mass 

when measuring emissions following a 

wet scrubber. Another commenter stated 

that when conducting emissions testing 

at facilities with similar wet stack 

conditions, as described in the proposal 

preamble (74 FR 12973), they supported 

EPA’s position on the limitations of the 

proposed Method 201A. 

Response: EPA acknowledges that 

using Method 5 on stacks with 

entrained moisture and assuming that 

the catch is PM2.5 can potentially 

overestimate PM2.5 concentrations. EPA 

Method 5 measures total PM mass 

emissions from stationary sources. 

Method 5 does not specifically isolate 

PM10 or PM2.5. Method 17, similar to 

Method 5, measures total PM mass 

emissions, but it uses an in-stack filter 

operating at stack temperature instead of 

a heated probe and out-of-stack heated 

filter and thus, is suitable for only dry 

sources. 

Monitoring the emission of PM10 or 

PM2.5 from a wet gas stream is a 

challenging problem that has not been 

addressed successfully despite 

considerable effort. A consensus method 

to provide this information has not 

emerged. EPA has determined that 

particulate from wet stacks is expected 

to be primarily PM10 under most 

conditions typical of good wet scrubber 

design and operation. University of 

North Carolina particle physicists 

performed theoretical calculations based 

on a wet scrubber operating at 10,000 

parts per million by weight (ppmw) 

total dissolved solids (TDS) with water 

droplets up to 50 μm in size (see 

‘‘Development of Plans for Monitoring 

Emissions of PM2.5 and PM10 from 

Stationary Sources With Wet Stacks,’’ 

Docket ID No. EPA–HQ–OAR–2008– 

0348). They determined that water 

droplets under these conditions, when 

dried, would generate particles of 10 μm 

or less. Using the same theoretical basis 

(i.e., the ratio of TDS to water droplet 

size), EPA expects that water droplets 

up to 10 μm in size would generate 

dried particles of 2 μm or less and that 

water droplets up to 20 μm would 

generate dried particles up to 4 μm or 

less. 

Based on wet scrubber operation and 

typical mist eliminator performance, 

EPA has determined that the Method 5 

filterable particulate measurements are a 

satisfactory approximation of PM2.5

filterable particulate from controlled 

wet stack emissions. It is the States’ or 

regulatory authorities’ responsibility to 

interpret EPA’s recommendation to use 

Method 5 when measuring PM in stacks 

containing water droplets and to 

consider all of the collected material to 

be PM2.5. 

Because a completely acceptable 

method for measuring PM2.5 in wet 

stacks is not currently available, EPA 

understands the need to support the 

States with a PM2.5 method for wet 

stacks. EPA is currently developing this 

method and laboratory testing is 

ongoing. EPA has committed a 

significant budget and personnel to 

developing an acceptable method for 

sources with wet stacks, as explained 

above. In the meantime, the 

promulgated amendments to Methods 

201A and 202 improve their 

performance and reduce known 

artifacts. Testers should use these final, 

amended methods until a PM2.5 method 

for wet stack conditions is promulgated. 

Comment: Several commenters 

expressed concern about the limitation 

of the method for stack temperatures 

greater than 500 °F. One commenter 

asked that EPA investigate a possible 

modification to the method to utilize 

sampling equipment that can withstand 

higher stack temperatures. The 

commenter also introduced the 

possibility of moving the particle sizing 

device, at least for PM2.5, out of the stack 

and into a heated box, enabling use of 

a glass-lined probe for sampling. 

Another commenter stated that the 

operator of a hot stack should not be 

required to ‘‘take extraordinary 

measures’’ (such as using the metal 

Inconel) when such measures are not 

defined in the method, no less tested in 

the field for accuracy. The commenter 

encouraged EPA to develop an 

acceptable substitute method for hot 

stacks. As an alternative, the commenter 

recommended that Method 5 testing, in 

conjunction with AP–42 particle size 

distribution data specific to glass 

furnaces, should be used for 

measurement of PM2.5 in hot stacks. 

Response: EPA investigated 

additional alternatives to allow the use 

of screwed together cyclones at elevated 

stack temperatures. As a result of this 

investigation, EPA has revised Section 

8.6.1 of Method 201A to allow the 

method to be used at temperatures up to 

1,000 °F (538 °C) using stainless steel 

cyclones that are bolted together, rather 

than screwed together. Using ‘‘breakaway’’ stainless steel bolts facilitates 

disassembly and circumvents the 

problem of thread galling. If the 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80127 

stainless steel bolts seize, over-torquing 

such bolts causes them to break at the 

bolt head, thus releasing the cyclones 

without damaging the cyclone flanges 

(see ‘‘Review of Draft EPA Test Methods 

201A and 202 Related to the Use of High 

Temperature and Out-of-Stack Cyclone 

Collection,’’ Southern Research Institute, 

EPA Docket ID No. EPA–HQ–OAR– 

2008–0348). The method can be used at 

temperatures up to 2,500 °F using 

specially constructed high-temperature 

stainless steel alloys (Hastelloy or 

Haynes 230) with bolt-together closures 

using break-away bolts (see also 

‘‘Development of Particle Size Test 

Methods for Sampling High 

Temperature and High Moisture 

Sources,’’ California Environmental 

Protection Agency, Air Resources Board 

Research Division, 1994, NTIS PB95– 

170221). 

Regarding the use of a heated box 

external to the stack to house the 

cyclones, EPA disagrees with this 

approach because of the potential for 

significant losses of particulate in the 

nozzle and probe liner. EPA expects that 

transport losses for particles in the size 

range of interest would be significant 

enough to materially affect the 

measurement results. These losses 

would be caused by deposition 

primarily by impaction in the sampling 

nozzle (at the flow rates used in PM10

and PM2.5 sampling) and settling losses 

in horizontal probes. (See ‘‘Review of 

Draft EPA Test Methods 201A and 202 

Related to the Use of High Temperature 

and Out-of-Stack Cyclone Collection, 

Southern Research Institute,’’ EPA 

Docket ID No. EPA–HQ–OAR–2008– 

0348.) 

Sampling from ducts smaller than 

allowed by the blockage criteria or from 

ducts at high temperatures presents 

challenges that should be addressed by 

the source tester in conjunction with the 

regulatory authority. Method 201A does 

not permit the use of a nozzle and probe 

extension leading to an external heated 

oven to house the cyclones that would 

otherwise block stack flow or operate at 

stack temperatures beyond acceptable 

limits. Conventional screwed-together 

cyclones are designed to operate in 

stacks that have a blockage of less than 

three percent and have a temperature of 

less than 500 °F. 

Regarding the use of AP–42 as a 

replacement for PM10 or PM2.5

compliance testing, EPA has determined 

that this is not appropriate because of 

the uncertainty in the data due to 

variations in the particle sizing used to 

generate AP–42 emission factors. EPA’s 

AP–42 particle-sizing data for sources 

controlled by wet scrubbers are based 

upon particle sizing methodologies that 

are affected by the same influences and 

uncertainties that make particle sizing 

in stacks with entrained water droplets 

a challenging technical issue. Particlesizing information in AP–42 is based 

primarily upon data collected in the 

1970s and early 1980s. The 

uncertainties associated with methods 

used during this period of time result in 

particle-sizing data that are dated and 

may not reflect the best sampling 

technology or the emissions from 

current control devices. Particle-sizing 

data from the 1970s employed many 

measurement methodologies that were 

found to introduce indeterminate biases 

in the particle sizing data. Also, source 

testers implemented measurement 

methods in different ways to deal with 

particle-sizing methodology and sourcespecific measurement challenges. The 

inconsistencies associated with 

addressing measurement challenges and 

indeterminate biases led to higher 

uncertainties associated with the 

measurement method results. Therefore, 

AP–42 should not be used as a 

replacement for contemporary 

emissions testing. 

However, it may be acceptable to 

allow limited application of AP–42 

particle size distributions as screening 

assessments when the underlying 

biases, uncertainties, and variations of 

the particle-sizing are taken into 

consideration. For example, one simple 

method involves using terms that 

include factors (such as the TDS of the 

recirculating scrubber water, estimated 

water droplet size distribution of the 

exit gas, and total liquid mass) that are 

already used to calculate approximate 

emission factors. Instruments are 

commercially available that can 

continuously monitor TDS and water 

flow rate, and the output from these 

instruments could feed into an emission 

factor to provide a continuous estimate 

of emissions that varies with process 

conditions. However, work needs to be 

done to evaluate the reliability and bias 

of this type of candidate estimation 

method. The required data inputs for 

this type of estimation model need to be 

identified and the likelihood that these 

inputs can be provided by the emission 

source needs to be confirmed. Once the 

input data can be readily obtained, the 

estimation model(s) needs to be 

evaluated to bring the most promising 

methods to fruition. (See ‘‘Development 

of Plans for Monitoring Emissions of 

PM2.5 and PM10 from Stationary Sources 

with Wet Stacks, Department of 

Environmental Sciences and 

Engineering, University of North 

Carolina at Chapel Hill under 

subcontract to MACTEC Federal 

Programs,’’ EPA Contact No: EP–D–05– 

096, Work Assignment 2–05, August 

2007; Docket ID No. EPA–HQ–OAR– 

2008–0348). 

Comment: Several commenters 

requested changes to Section 6 of 

Method 201A regarding equipment and 

supplies. One commenter questioned 

the use of glass dishes and glass 250 ml 

beakers for drying the filter and rinses 

in proposed Method 201A. Another 

commenter stated that, at a minimum, 

the method should specify glass 

beakers, 50 ml weighing tins, and an 

analytical balance with a resolution of 

0.00001 g (0.01 mg). One commenter 

recommended that polyethylene 

transfer/storage bottles should be 

allowed to minimize the chance of 

breakage when in the field. 

Response: We revised Sections 6.2, 

11.2.4, and 11.2.7 of Method 201A to 

allow the use of fluoropolymer beaker 

liners for evaporating the particulate 

rinse solvent and the acetone field 

reagent blank, desiccating particulate to 

constant weight, and weighing 

particulate samples in the final 

evaporation step. We revised Section 

6.2, consistent with the commenter’s 

suggestions, and added glass beakers 

and an analytical balance with a 

resolution of 0.00001 g (0.01 mg) to the 

sample recovery and analytical 

equipment list. However, we did not 

include weighing tins because we 

determined that quantitative transfer of 

particles in acetone from a beaker to a 

weighing tin is not necessary and adds 

unnecessary imprecision to the final 

sample weight. Alternatively, EPA has 

changed the method to allow 

fluoropolymer beaker liners to be used 

to evaporate and weigh the samples. 

EPA revised Section 6.2.1 of Method 

201A by defining sample recovery items 

consistently with Method 5, except for 

wash bottles and sample storage bottles. 

Any container material is acceptable for 

wash bottles and storage bottles, but the 

container must not contribute more than 

0.05 mg of residual mass to the CPM 

measurements. 

Comment: Several commenters 

expressed concern about the proposed 

requirement to use a 6-inch sampling 

port. One commenter pointed out that 

using a 6-inch sampling port would be 

required only for the combined 

PM10/PM2.5 sampling apparatus. 

Another commenter stated that the 

physical dimensions of the cyclone 

would also cause problems with 

installation in the generally small fryer 

and dryer stacks. Another commenter 

noted that the partitioning of the 

filterable solids using bulky, in-stack 

cyclones creates several logistical and 

practical problems. The commenter 


jlentini on DSKJ8SOYB1PROD with RULES2
80128 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

stated that the size of the in-stack 

separation cyclones requires 

6-inch to 8-inch sampling ports that do 

not exist at the vast majority of 

stationary sources potentially affected 

by this final action. 

Response: EPA understands the 

commenters’ concerns regarding 

sampling port diameter requirements. 

However, facilities that are required to 

use Method 201A are responsible for 

ensuring that the stack has the 

appropriately sized sampling ports. The 

need for the larger port diameter has not 

changed from the requirement as stated 

in the 1990 version of this method. We 

revised Section 8.3.1 of Method 201A to 

more clearly describe when a 4-inch 

port may not accommodate the PM10

particle-sizing cyclone and the nozzle 

that extends from the cyclone and to 

highlight the need for a larger port in 

such situations. 

Comment: One commenter requested 

that EPA adjust the allowable number of 

traverse points that fall outside of the 

range of the Dpmin and Dpmax for cases in 

which more than the recommended 

maximum 12 traverse points are 

sampled by Method 201A. Many 

agencies require that more than the 

recommended maximum 12 traverse 

points be sampled if total filterable 

particulate is being determined. The 

commenter requested that the number of 

allowed out-of-range values be adjusted 

to match the stated failure rates 

expressed as percentages. 

Response: EPA agrees that increasing 

the number of allowable traverse points 

outside the range Dpmin and Dpmax is 

appropriate when more than the 

recommended number of traverse points 

are sampled. EPA has modified Section 

8.5.5 of the method to allow 16 percent 

failure rate rounded to the nearest 

whole number for PM2.5 only and 8 

percent failure rate rounded to the 

nearest whole number if the course 

fraction for PM10 determination is 

included. 

Comment: One commenter requested 

that EPA add a new section in Section 

8.3.2 to address ducts with diameters 

less than 18 inches. The commenter 

stated that the new section should state 

that ducts with diameters less than 18 

inches have blockage effects ranging 

from five to ten percent. Therefore, 

according to the commenter, when a test 

is conducted on these small ducts, the 

observed velocity pressures must be 

adjusted for the estimated blockage 

factor whenever the combined sampling 

apparatus blocks more than three 

percent of the stack or duct. 

For stacks smaller than 18 inches, one 

commenter asked if there would still be 

a blockage issue even when following 

the proposed Method 201A procedures, 

especially as the stack diameter gets 

smaller. The commenter also asked if 

there was a lower limit of stack diameter 

where the method cannot be used. 

One commenter stated that when 

conducting emissions testing at facilities 

with similar small stack (less than 18 

inches in diameter) conditions, as 

described in the proposal preamble (74 

FR 12973), their experience supported 

EPA’s position on the limitations of the 

proposed Method 201A. Another 

commenter pointed out an error in 

Section 8.7.2.3 that implied that the 

method could be used on stacks with 

diameters less than 18 inches. 

Another commenter requested that if 

testing of stacks less than 18 inches in 

diameter is still allowed and the testers 

are required to use Method 1A, then the 

option of using a standard pitot tube 

should apply. 

Response: We revised Section 8.7.2.3 

of Method 201A to clarify the lower 

limits of stack diameter for different 

sampling configurations. The combined 

PM10/PM2.5 filter sampling head and 

pitot tube is not applicable for stacks 

with a diameter less than 26.5 inches 

because the blockage is greater than six 

percent. Blockage above six percent is 

not allowed for the combined PM10/ 

PM2.5 filter sampling head and pitot 

tube. However, measurements for only 

PM2.5 may be possible using only a 

PM2.5 cyclone, pitot tube, and in-stack 

filter for stacks with a diameter less than 

26.5 inches. If the blockage exceeds 

three percent but is less than six percent 

in that configuration, you must follow 

the procedures outlined in Method 1A 

to conduct tests on stacks less than 26.5 

inches in diameter. In addition, you 

must conduct the velocity traverse 

downstream of the sampling location or 

immediately before the test run. 

We also modified Section 10.1 of the 

method to allow standard pitot tubes to 

be used downstream when significant 

blockage exists. As stated in Section 

8.3.2.2, you must adjust the observed 

velocity pressures for the estimated 

blockage factor whenever the sampling 

apparatus blocks three to six percent of 

the stack or duct. 

Comment: One commenter requested 

that the specification for the maximum 

allowable acetone blank value be 

changed from 0.001 percent by weight 

to either 1 ppmw or 0.0001 percent by 

weight to be consistent with the reagent 

specification stated in Section 7.2.1 of 

the method. 

Response: We agree with the 

commenter that maximum allowable 

acetone blank value should be 

consistent with the reagent specification 

stated in Section 7.2.1. Thus, we revised 

Section 12.3.2.3 of the final method to 

specify the maximum allowable acetone 

blank in terms of weight per volume of 

acetone (0.1 mg per 100 ml solvent), 

rather than percent weight. 

Comment: One commenter expressed 

concern about the approach in Section 

12.3.2.3 of the proposed method. The 

commenter stated that subtracting the 

acetone blank mass from the individual 

sample masses would be acceptable if 

the volumes of the acetone rinses are all 

exactly 100 ml. However, according to 

the commenter, this was not reality, and 

the accuracy of determining the blank 

correction suffers from this approach. 

The commenter suggested that rather 

than subtracting the mass of the acetone 

rinse blank dry residue directly from the 

sample masses, the concentration of the 

acetone rinse blank should be calculated 

as the mg of dry residue per ml of 

acetone rinse blank volume limited to 

the concentration of residue at 1 ppmw. 

The commenter stated that this 

concentration of the dry residue would 

be multiplied by the volume of the 

acetone in ml used to collect and 

recover each sample from the sampling 

head. The commenter stated that the 

resulting mass would be subtracted from 

the dry residue mass determined for the 

sample of interest. According to the 

commenter, this approach will provide 

a more accurate determination of the 

dry residue mass from the acetone rinse 

blank due to processing a larger volume 

of acetone, and assessment of the blank 

mass correction for each sample as it 

will be proportional to the amount of 

acetone used to collect each sample. 

The commenter stated that the liquid 

volume of the samples and blanks could 

be determined by either direct 

volumetric measurement or by 

multiplying the wet weight of the 

sample or blank by the density of the 

reagent at 20 °C. 

Response: We agree with the 

commenter and with the commenter’s 

suggested equation. Therefore, we 

revised Section 12.3.2.3 of the final 

method to accommodate different 

acetone rinse volumes. However, the 

correction must be proportional to the 

amount of solvent used. Some testers 

may use more solvent due to heavy 

deposits that are difficult to remove, 

while other testers may use less solvent. 

Therefore, the maximum adjustment is 

0.1 mg per 100 ml of the acetone used 

from the sample recovery. 

B. Method 202 

1. Extraction Solvent 

Comment: Three commenters noted 

that methylene chloride is highly toxic. 

One commenter stated the use of 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80129 

methylene chloride poses significant 

exposure risks to field test personnel, 

plant personnel working in the area of 

the mobile laboratory, and agency test 

observers. Two commenters stated that 

Method 202 should specify a less toxic 

solvent than methylene chloride, such 

as n-hexane. 

One commenter stated that EPA 

should sponsor a set of tests to confirm 

that n-hexane or another less-toxic 

solvent provides the sample rinse 

effectiveness as methylene chloride. 

Another commenter encouraged EPA to 

conduct future studies to identify a 

solvent to replace methylene chloride in 

Proposed Method 202 and in other EPA 

reference methods. 

Another commenter stated that the 

use of methylene chloride (a known 

carcinogen) as the cleaning and recovery 

solvent will require safety departments 

to develop procedures for appropriate 

handling on-site and the use of personal 

protection equipment for personnel that 

may be exposed to the solvent. The 

commenter noted that toluene, which is 

used in EPA Method 23, is a technically 

acceptable alternative to methylene 

chloride. The commenter suggested that 

EPA review the use of toluene as a 

replacement for methylene chloride in 

Method 202 (and OTM 028). 

Response: The extraction solvent 

specified in a particular test method is 

dependent on the analyte(s) of interest. 

If the target analyte is known, an 

appropriate solvent can be identified 

that has the desired recovery 

performance for that analyte. For 

Method 202, the pollutant measured by 

the method, CPM, is defined by the 

method (i.e., whatever remains after the 

sample recovery procedures is 

considered to be CPM regardless of its 

analyte group). Although no single 

solvent is universally applicable to all 

analyte groups, methylene chloride was 

chosen for the proposed method based 

upon studies (‘‘IERL–RTP Procedures 

Manual, Level 1, Environmental 

Assessment’’; EPA–600/2–76–160a; June 

1976) that showed it was the optimum 

solvent to recover polar and non-polar 

CPM. 

We acknowledge the commenters’ 

concerns regarding the toxicity of 

methylene chloride and the exposure 

hazards associated with its use, and we 

agree that the use of an alternative 

solvent is justified. However, because 

the recovery performance of solvents 

has been previously evaluated to 

support various EPA programs, we 

disagree with the commenters that 

additional studies are necessary to 

identify a suitable alternative solvent. 

In identifying an alternative solvent, 

we initially considered specifying 

toluene because its extraction 

performance for non-polar compounds 

is similar to methylene chloride. 

However, because the vapor pressure of 

toluene is lower than methylene 

chloride, additional time would be 

needed to evaporate the organic samples 

to dryness at room temperature (30°C or 

less). Because the additional 

evaporation time would be an 

additional burden on testing contractors 

and present the risk of losing 

condensable organic compounds, we 

rejected toluene as the replacement 

solvent. 

We also evaluated the solvents used 

for organic compound recovery in the 

analytical methods developed by EPA’s 

Office of Solid Waste (http:// 

www.epa.gov/epawaste/hazard/ 

testmethods/sw846/online/ 

3_series.htm). We reviewed EPA’s ‘‘Test 

Methods for Evaluating Solid Waste, 

Physical/Chemical Methods’’ (SW–846), 

which was developed to support the 

Resource Conservation and Recovery 

Act (RCRA) program, to identify test 

methods that covered the same types of 

compounds expected to comprise CPM. 

Based upon our review of SW–846, we 

identified Method M–3550c (Ultrasonic 

Extraction) as a comparable method (M– 

3550c is used to extract semi-volatile 

organic compounds from waste 

samples). Section 7.4 of M–3550c, 

which discusses extraction solvents, 

lists the following extraction solvents by 

class of compound: 

• Acetone/hexane or acetone/ 

methylene chloride can be used to 

extract semivolatile organics. 

• Acetone/hexane or acetone/ 

methylene chloride can be used to 

extract organochlorine pesticides. 

• Acetone/hexane, acetone/ 

methylene chloride, or hexane can be 

used to extract polychlorinated 

biphenyls (PCB). 

Of the above compound classes, the 

class that most closely relates to the 

type of high-molecular weight 

hydrocarbons expected to comprise 

organic CPM is PCB. Hexane is also 

listed as an alternative solvent (when 

used in combination with acetone) for 

the other compounds classes discussed 

in Section 7.4. Consequently, based 

upon this analysis, we have replaced 

methylene chloride with hexane in the 

final method. 

2. Sample and Blank Containers 

Comment: One commenter 

recommended that EPA revise the 

proposed method to specify the 

container type for each container (i.e., 

glass or plastic), and also whether the 

lid should have a Teflon® liner or 

whether another liner is acceptable. 

Response: We disagree with the 

commenter that the method should 

specify the material of construction of 

containers used for sample and blank 

recovery procedures. Although we 

believe that the most appropriate 

containers are constructed of glass and 

equipped with a fluoropolymer lid, we 

also believe that testing contractors 

should have the flexibility to select the 

type of containers that meet the 

performance specifications of the 

method. Therefore, we have revised the 

proposed method to add a performancebased specification for containers. 

Section 6.2.2 of the final method 

specifies that the containers used for 

sample and blank recovery procedures 

must not contribute more than 0.05 mg 

of residual mass to the CPM 

measurements. 

Accompanying edits were also made 

to the CPM container language in 

Section 8.5.4 (Sample Recovery). 

3. CPM Filter 

Comment: One commenter suggested 

that the language in Section 7.1.1 of the 

proposed method be revised to replace 

the term ‘‘Filter’’ with ‘‘CPM Filter’’ and 

replace ‘‘Teflon®’’ with ‘‘Teflon®, 

fluoropolymer or chemically 

equivalent.’’ Another commenter stated 

that the final method should allow for 

alternatives to Teflon® filters, such as 

quartz, polytetrafluoropolymer (PTFE) 

coated, or PTFE filters. 

Response: Based upon the comments 

received regarding the CPM filter, we 

revised the language in Section 7.1.1 to 

include performance-based 

specifications for the CPM filter rather 

than specifying a particular type of 

filter. Section 7.1.1 of the final method 

specifies that the CPM filter must be a 

non-reactive, non-disintegrating filter 

that does not contribute more than 0.5 

mg of residual mass to the CPM 

measurements. The CPM filter must 

have an efficiency of at least 99.95 

percent (less than 0.05 percent 

penetration) on 0.3 μm particles. 

Documentation of the CPM filter’s 

efficiency is based upon test data from 

the supplier’s quality control program. 

In selecting the appropriate CPM 

filter, testing contractors should avoid 

the mistake of equating the dioctyl 

phthalate size for the test particles to the 

pore size for the filter. Filters with pore 

sizes larger than the test particles can 

retain a high percentage of very small 

particles. In our evaluation of different 

types of filters, we determined that filter 

sizes of 47 mm are marginal, if not 

unacceptable, for use. Additionally, we 

believe that hydrophobic filters should 

be used to avoid absorption of water 

onto the CPM filter. 


jlentini on DSKJ8SOYB1PROD with RULES2
80130 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

4. Water Specifications 

Comment: Two commenters suggested 

that the final method specify the level 

of residue allowed for the water used to 

clean glassware and recovery samples, 

as was specified for acetone and 

methylene chloride. One commenter 

stated that the maximum percent 

residue by weight of the water should be 

specified to be consistent with the 

reagent specifications for acetone and 

methylene chloride. Three commenters 

noted that a residual mass level is not 

available for ASTM International 

D1193–06, Type I water. 

Response: The purpose of the field 

reagent blanks is to provide a testing 

contractor with information to target 

corrective actions, if necessary, if they 

have difficulty in meeting the residual 

mass allowance in the method. The 

method does not require analysis of 

field reagent blank samples, and the 

field reagent blank values are not used 

in correcting CPM measurements. 

However, we acknowledge that Figure 3 

could be misleading with regard to the 

field reagent blanks, and we have 

revised Figure 3 of the final method to 

remove the entries for the field reagents. 

We acknowledge that the residue 

level is not specified for ASTM 

International D1193–06, Type I water, 

and we agree with the commenters that 

the method should specify a residual 

mass level for water used to prepare 

glassware and recover samples. 

Therefore, we have revised Sections 

7.1.3 and 7.2.3 of the final method to 

specify that glassware preparation and 

sampling recovery must be conducted 

using deionized, ultra-filtered water that 

meets a residual blank value of 1 ppmw 

or less. We have also made 

accompanying changes to water 

specified in Sections 8.4, 8.5.3.2, and 

11.2.2.1 of the final method. We believe 

that this performance specification will 

provide flexibility to testing contractors 

in obtaining deionized, ultra-filtered 

water (e.g., water could be purchased 

with a vendor guarantee or the 

contractor could evaluate water they 

produce by evaporation and weighing of 

the residue). 

5. Glassware Baking Requirements 

Comment: Several commenters stated 

that the proposed requirement in 

Section 8.4 to bake glassware at 300°C 

for six hours was excessive. Several 

commenters stated that they had 

conducted experimental tests that 

showed that a lower baking temperature 

(e.g., 125°C for three hours) was 

sufficient to achieve the blank 

allowance specified in the method. One 

commenter stated that, based upon their 

experiments, no benefit was obtained 

from baking glassware. Another 

commenter stated that they had 

conducted numerous test runs on noncombustion sources without baking 

glassware and had achieved acceptable 

blank results. The commenter noted that 

there might be some emission sources 

where baking of glassware could be 

needed to meet the blank requirements, 

but the commenter stated that the 

mandatory baking requirements did not 

seem to be necessary for all sources. 

Another commenter stated that there is 

no laboratory data to determine if a 

lower temperature could be sufficient to 

achieve low background masses. Based 

upon experimental results, the 

commenter suggested allowing the use 

of baking of glassware at 125°C for three 

hours. 

One commenter stated that, because 

the presence of silicone grease on 

impinger surfaces is highly unlikely due 

to the prevalence of O-rings, baking the 

glassware at 125°C for three hours after 

cleaning is adequate. The commenter 

added that the baking requirements 

should be revised because hightemperature baking would destroy or 

deteriorate the O-rings typically used to 

seal impinger components. The 

commenter stated that the effort to 

remove these O-rings before baking and 

then replace them after baking is timeconsuming. Several commenters noted 

that the high-temperature baking 

requirements would be overly expensive 

(e.g., for large, high-temperature ovens) 

and time-consuming. 

Another commenter stated that the 

requirement for glassware baking only 

prior to the test makes little sense. The 

commenter questioned why the 

glassware could not be rinsed with the 

recovery solvents as is done between 

runs. The commenter noted that the 

proposed method mandates a reagent 

blank and questioned why the reagent 

blank could not be changed to a proof 

blank with a limit. 

One commenter stated that the 

requirement to bake glassware at 300 °C 

for six hours should be optional because 

it has not been possible to fully evaluate 

the supporting data and the need for 

such high temperature is not readily 

apparent for all situations. The 

commenter noted that the ‘‘Draft Project 

Report—Evaluation and Improvement of 

Condensable Particulate Measurement’’ 

may contain this information and 

recommended that the effect of pre-bake 

temperature and time on cleanliness of 

blanks be clearly presented in this 

report and include a table comparing 

the effect of 300 °C for six hours versus 

lower glassware preparation 

temperatures. Otherwise, according to 

the commenter, this requirement would 

require the stack tester to bring to the 

testing site a large amount of precleaned glassware, much more than 

what is currently normal for such 

testing. 

One commenter suggested that testing 

contractors be allowed to meet the blank 

level specified in the method however 

they can. The commenter stated that the 

prescriptive temperature requirement, 

particularly in light of the fact that there 

are no data showing that the 2 mg blank 

cannot be achieved at lower 

temperatures or through other means, 

did not serve a purpose. Another 

commenter recommended that the tester 

start with baked glassware for the first 

test and then be allowed to perform 

additional tests reusing the same 

glassware after it has been cleaned by 

chemical methods. If the chemical 

cleaning of the glassware is not 

adequate, the commenter noted that 

blank values would likely elevate, 

possibly eliminating the test from 

consideration. If the blanks do not 

elevate, the commenter stated that this 

scenario would be very cost-effective 

and would conserve resources. 

Response: Method 202 has the 

potential to measure CPM at very low 

levels. Consequently, the glassware used 

in the sampling train must be free from 

contamination to maximize the 

precision and accuracy of the CPM 

measurements. The glassware cleaning 

requirements contained in the proposed 

revisions to Method 202 were based 

upon experimental results that 

indicated that the allowable blank 

correction of the method could not be 

achieved without thorough cleaning and 

baking of the glassware at 300 °C for six 

hours. 

Based upon our review of the public 

comments received regarding the baking 

requirements, we have determined that 

it is appropriate to provide a 

performance-based option in Section 8.4 

for demonstrating the cleanliness of 

glassware used during the emission test. 

The option provides testing contractors 

with flexibility when preparing 

glassware while maintaining the 

cleanliness requirements of the method. 

As an alternative to baking glassware, 

the final method allows testing 

contractors to perform a proof blank of 

the sampling train. Field train proof 

blanks are recovered on-site from a 

clean, fully assembled sampling train 

prior to the first emissions test and 

provide the best indication of the lowest 

residual mass achievable by the tester. 

Field train recovery blanks are 

recovered from a sampling train after it 

has been used to collect emissions 

samples and has been rinsed in 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80131 

preparation for the second or third test 

in a series at a particular source. Use of 

field train recovery blanks allows the 

tester to account for and manage 

additional uncertainty that may be 

attributed to the tester’s ability to clean 

the sampling train between test runs in 

the field. 

6. Nitrogen Purge 

Comment: Three commenters 

requested that the nitrogen purge 

procedures specified in Section 8.5 of 

the proposed method be revised to 

allow for the dry gas meter to be 

disconnected from the sampling train 

before the nitrogen purge is be 

conducted. Two commenters stated that 

EPA should eliminate the portion of 

Figure 2 that shows the meter box and 

revise the text in the proposed Method 

202 to require purging in a clean 

environment without the need for a 

meter box. Three commenters added 

that allowing the dry gas meter to be 

disconnected from the sampling train 

would decrease the delay between tests 

(i.e., the dry gas meter could be used 

with a new sampling train while the 

purge is being conducted on the 

previous train). Three commenters also 

stated that requiring the dry gas meter 

to be connected to the sampling train 

during the purge will force testing 

contractors to bring extra equipment 

(e.g., sampling trains, dry gas meters) to 

the sampling site. 

Three commenters suggested that the 

purge should be conducted at the 

sample recovery location (e.g., mobile 

laboratory) rather than at the actual 

sampling location (e.g., roof, stack 

sampling platform). Two commenters 

noted that it is not practical to haul 

nitrogen cylinders to the sampling 

location. One commenter suggested that, 

after the final leak check, the open ends 

of the impinger train could be capped 

during transport to the sample recovery 

area to reduce the possibility of oxygen 

contamination. The commenter noted 

that the sample would not be exposed 

to any more air than when immediately 

connecting to the nitrogen purge line. 

Several commenters suggested that 

the proposed method be revised to 

allow testing contractors to conduct a 

positive-pressure purge instead of a 

negative-pressure purge using the dry 

gas meter. One commenter suggested 

that the purge gas flow rate be 

monitored by a rotameter instead of 

using the dry gas meter. The commenter 

noted that the flow rate is better 

regulated upstream of the impingers 

rather than downstream by the dry gas 

meter and using the rotameter to 

regulate the purge gas flow rate would 

reduce the potential for pressurizing the 

sampling train. Another commenter 

expressed concerns that if the vacuum 

drawn by the dry gas meter does not 

match the pressure from the nitrogen 

tank, then the impingers could become 

over-pressurized which could 

compromise the integrity of the 

sampling train components. 

One commenter recommended that 

the proposed testing protocol be 

modified to allow the tester to 

disassemble the impinger train to 

measure for moisture content prior to 

conducting the required nitrogen purge. 

One commenter noted that weighing the 

impingers prior to the nitrogen purge 

would provide a more accurate moisture 

catch determination and the need to 

measure the amount of degassed 

deionized water that is added (if any) 

would be eliminated. Three commenters 

added that, if the moisture content of 

the impingers is determined before the 

nitrogen purge, then testing contractors 

should be allowed to purge only the 

knock-out impinger, backup impinger, 

CPM filter, and first moisture trap 

impinger. One commenter stated that if 

the sampling train is purged by pushing 

nitrogen through the sampling train (i.e., 

positive pressure purge), then the 

sampling train components after the 

CPM filter thermocouple could be 

disconnected from the train before 

beginning the purge. One commenter 

suggested that the purge be conducted 

through a Teflon® tube inserted through 

a stopper into the impinger arm and 

then into the liquid to avoid 

compounding errors associated with 

adding water to the first impinger (if 

needed). The commenter stated that this 

would alleviate the need to break the 

fitting or add water, and prevent the 

potentially compounding error of water 

addition. Another commenter requested 

that a Teflon® line be inserted down 

and through the short-stem impinger 

extending below the water level in the 

impinger catch. The commenter stated 

that this would reduce the potential for 

breaking glassware and contamination 

when removing/inserting glassware 

stems. 

Three commenters suggested that the 

nitrogen purge requirements be revised 

to allow for any liquid collected in the 

first (drop-out) impinger to be 

transferred to the second (backup) 

impinger. The commenters noted that 

this approach would decrease the 

potential for contamination because a 

new piece of glassware (the long-stem 

impinger) would not be introduced into 

the sampling train. One commenter 

recommended that, after the liquid is 

transferred to the second impinger, the 

first impinger should be removed from 

the sampling train prior to the purge. 

Response: It was our intent in the 

proposed Method 202 to allow testing 

contractors the option of conducting 

either a pressurized purge (i.e., without 

the dry gas meter box and pump 

attached to the sampling train) or a 

vacuum purge (i.e., with the dry gas 

meter box attached to the sampling 

train). However, we acknowledge that 

the language in Section 8.5.3 and the 

sampling train depicted in Figure 2 of 

the proposed method were unclear. 

Consequently, we have revised Section 

8.5.3 and Figure 2 and added Figure 3 

to the final method to clarify that a 

pressurized purge is an acceptable 

alternative. 

With regard to the commenters’ 

suggestion to allow testing contractors 

to conduct the nitrogen purge at the 

sample recovery location instead of at 

the sampling location, we continue to 

believe that testing contractors should 

have the flexibility to conduct the 

nitrogen purge at the location of their 

choosing; therefore, the final method 

does not specify where the purge must 

be conducted. However, testing 

contractors should conduct the purge as 

soon as practicable after the post-test 

leak check to reduce the potential for 

artifact formation in the impinger water. 

With regard to the alternative 

sampling train configuration for the 

purge, we agree with the commenters 

that testing contractors should be 

allowed the option of determining the 

amount of moisture collected prior to 

conducting the nitrogen purge, 

transferring any water collected prior to 

the CPM filter to the second impinger, 

and performing the nitrogen purge on 

the second impinger and the CPM filter 

only. Therefore, Section 8.5.3.2 of the 

final method contains an alternative 

purge procedure. 

We disagree with the commenter’s 

suggestion to insert a Teflon® tube into 

the first impinger for conducting the 

nitrogen purge. Using the configuration 

suggested by the commenters, there is 

no provision to maintain the 

temperature of the purge gas. 

Consequently, we believe that a Teflon®

or other inert line used to purge the 

CPM train is not an acceptable 

alternative. Therefore, we are not 

revising Section 8.5.3.2 to allow the use 

of a Teflon® tube. 

C. Conditional Test Method 039 

(Dilution Method) 

Comment: Several commenters urged 

EPA to continue the development of 

dilution-based test methods for 

measuring PM2.5. One commenter 

supported EPA’s work through the 

stakeholder process to decrease and 

eliminate other pollutant interferences 


jlentini on DSKJ8SOYB1PROD with RULES2
80132 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

that can affect the accurate 

measurement of emissions of fine 

particles, particularly for wet stacks and 

high volume/low concentration gas 

streams. Another commenter 

encouraged EPA to use the stakeholder 

process, similar to that used for 

Methods 201A and 202, to move 

towards the promulgation of dilution 

methods and other test methods that can 

better measure emissions from hightemperature and high-moisture sources. 

One commenter asserted that dilution 

methods more correctly simulate the 

atmospheric process leading to the 

formation and deposition of PM in the 

atmosphere. Another commenter 

expected that EPA’s evaluation of an air 

dilution method would show that it is 

even more useful in accurately 

measuring direct PM2.5 filterable and 

condensable data for high temperature 

sources than the revised Methods 201A 

and 202. 

Response: EPA continues to evaluate 

the precision and bias of PM2.5 collected 

using dilution methods. In addition to 

EPA’s hardware design, several other 

hardware designs have been proposed 

that utilize dilution. While limited 

evaluations of EPA’s hardware design 

have been performed, the other 

hardware designs proposed have more 

limited evaluations. The consensus 

standards body, ASTM International, 

has embarked on preparation of a 

standard method for dilution sampling 

of particulate material. We will continue 

to evaluate dilution method procedures 

and support the efforts of the ASTM 

International in their development of a 

standard dilution-based test method for 

sampling PM. In addition to these 

development efforts, several other 

factors influence EPA’s decision to 

delay proposing a dilution based 

sampling method. One factor is that 

there is no widely accepted dilution 

method available at this time. Another 

factor is that the available dilution 

sampling hardware configurations share 

few of the equipment used by any of the 

existing sampling methods. As a result, 

testing contractors would be required to 

invest in this new equipment. This 

capital investment would require a 

higher charge for testing than for the 

existing methods. In addition, since 

dilution sampling is somewhat more 

complex, contractors are likely to 

initially charge a premium for this more 

complex testing. Lastly, the availability 

of hardware and experienced 

individuals to perform dilution 

sampling is extremely limited. EPA 

recognizes that there are limited 

applications where dilution sampling 

provides advantages over the standard 

test methods. As a result, we encourage 

sources that encounter these situations 

to request that the regulatory authority 

that established the requirement to use 

this method to approve the use of 

dilution sampling as an alternative to 

the test method specified for 

determining compliance. 

Comment: One commenter 

maintained that use of a test method to 

define what constitutes CPM for all 

sources is neither necessary, nor (in 

some cases) useful. For sources, like 

coal-fired boilers, where the only true 

condensable sulfate specie from coal 

combustion is sulfuric acid, the 

commenter stated that CPM could be 

better quantified by direct measurement 

using the Controlled Condensation 

Method (CCM). The commenter said 

that States should be allowed and, in 

the case of units with wet scrubbers, 

encouraged to use such direct 

measurements like CCM to quantify 

known CPM instead of using Method 

202. According to the commenter, if the 

use of CCM is not allowed, Method 202 

should include a procedure that allows 

sources to correct Method 202 results 

using results from simultaneous CCM 

test runs. In this procedure, according to 

the commenter, the source would be 

subtracting out essentially the same 

units of sulfate from Method 202 as 

would be added back in from the CCM 

results. If, on the other hand, sulfate 

artifacts do exist, the commenter said 

that the source would be subtracting ‘‘x’’ 

units of sulfate from Method 202 and 

adding back ‘‘y’’ units of sulfate from 

CCM to get an accurate measurement. 

Response: While SO3 may be the most 

abundant CPM emitted from coal fired 

combustion, there is indication that 

other compounds comprise CPM. Few 

speciation tests of coal and oil 

combustion have been preformed, but 

those that have indicate the presence of 

not only sulfate but also chloride, 

nitrate, ammonium ion, and a range of 

inorganic elements that are potentially 

components for CPM (including 

phosphorous, arsenic, and selenium). In 

addition, speciation tests have been able 

to identify components representing 

only about 60 percent of the mass. 

Therefore, the specific correction for 

sulfuric acid from coal combustion 

source emissions proposed by the 

commenter would add to the 

complexity of the method for all source 

categories while providing an advantage 

to only one specific source category. 

EPA continues to review methods that 

involve controlled condensation for 

sulfuric acid. Because no standard 

method is available for controlled 

condensate measurement of sulfuric 

acid, we have determined that providing 

additional guidance or correction of 

Method 202 results is premature. EPA is 

following current efforts by ASTM 

International to develop a standard 

controlled condensate method for 

sulfuric acid. In the meantime, testers 

and facilities should petition their 

regulatory authority to approve 

alternative data treatment for specific 

sources. 

VI. Statutory and Executive Order 

Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review 

This action is not a ‘‘significant 

regulatory action’’ under the terms of 

Executive Order (EO) 12866 (58 FR 

51735, October 4, 1993) and is, 

therefore, not subject to review under 

the EO. 

B. Paperwork Reduction Act 

This action does not impose an 

information collection burden under the 

provisions of the Paperwork Reduction 

Act, 44 U.S.C. 3501 et seq. Burden is 

defined at 5 CFR 1320.3(b). The final 

amendments do not contain any 

reporting or recordkeeping 

requirements. The final amendments 

revise two existing source test methods 

to allow one method to perform 

additional particle sizing at 2.5 μm and 

to improve the precision and accuracy 

of the other test method. 

C. Regulatory Flexibility Act 

The Regulatory Flexibility Act (RFA) 

generally requires an agency to prepare 

a regulatory flexibility analysis of any 

rule subject to notice and comment 

rulemaking requirements under the 

Administrative Procedure Act or any 

other statute unless the agency certifies 

that the rule will not have a significant 

economic impact on a substantial 

number of small entities. Small entities 

include small businesses, small 

organizations, and small governmental 

jurisdictions. 

For purposes of assessing the impacts 

of this rule on small entities, small 

entity is defined as: (1) A small business 

as defined by the Small Business 

Administration’s (SBA) regulations at 13 

CFR 121.201; (2) a small governmental 

jurisdiction that is a government of a 

city, county, town, school district or 

special district with a population of less 

than 50,000; and (3) a small 

organization that is any not-for-profit 

enterprise which is independently 

owned and operated and is not 

dominant in its field. 

After considering the economic 

impacts of this final rule on small 

entities, I certify that this action will not 

have a significant economic impact on 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80133 

a substantial number of small entities. 

This final rule will not impose any 

requirements on small entities. Most of 

the emission sources that will be 

required by State regulatory agencies 

(and federal regulators after 2011) to 

conduct tests using the revised methods 

are those that have PM emissions of 100 

tons per year or more. EPA expects that 

few, if any, of these emission sources 

will be small entities. 

Although this final action will not 

have a significant economic impact on 

a substantial number of small entities, 

EPA nonetheless has tried to reduce the 

impact of this final action on small 

entities. This final rule does not require 

any entities to use these final test 

methods. Such a requirement would be 

mandated by a separate independent 

regulatory action. However, upon 

promulgation of this final action, some 

entities may be required to use these test 

methods as a result of existing permits 

or regulations. Since the cost to use the 

final test methods is comparable to the 

cost of the methods they replace, little 

or no significant economic impact to 

small entities will accompany the 

increased precision and accuracy of the 

final test methods. After January 1, 

2011, when the transition period 

established in the Clean Air Fine 

Particle Implementation Rule expires, 

States are required to consider inclusion 

of pollutants measured by these test 

methods in new or revised regulations. 

The economic impacts caused by any 

new or revised State regulations for fine 

PM would be associated with those 

State rules and not with this final action 

to modify the existing test methods. 

Consequently, we believe that this final 

action imposes little if any adverse 

economic impact to small entities. 

D. Unfunded Mandates Reform Act 

This rule contains no federal 

mandates under the provisions of Title 

II of the Unfunded Mandates Reform 

Act of 1995 (UMRA), 2 U.S.C. 1531– 

1538 for State, local, and tribal 

governments or the private sector. The 

incremental costs associated with 

conducting the revised test methods 

(expected to be less than $1,000 per test) 

do not impose a significant burden on 

sources. Thus, this final action is not 

subject to the requirements of sections 

202 and 205 of the UMRA. 

This rule is also not subject to the 

requirements of section 203 of UMRA 

because it contains no regulatory 

requirements that might significantly or 

uniquely affect small governments. The 

low incremental cost associated with 

the revised test methods mitigates any 

significant or unique effects on small 

governments. 

E. Executive Order 13132: Federalism 

This action does not have federalism 

implications. It will not have substantial 

direct effects on the States, on the 

relationship between the national 

government and the States, or on the 

distribution of power and 

responsibilities among the various 

levels of government, as specified in 

Executive Order 13132. In cases where 

a source of PM2.5 emissions is owned by 

a State or local government, those 

governments may incur minimal 

compliance costs associated with 

conducting tests to quantify PM2.5

emissions using the revised methods 

when they are promulgated. However, 

such tests would be conducted at the 

discretion of the State or local 

government and the compliance costs 

are not expected to impose a significant 

burden on those governments. 

Additionally, the decision to review or 

modify existing operating permits to 

reflect the CPM measurement 

capabilities of the final test methods is 

at the discretion of State and local 

governments and any effects or costs 

arising from such actions are not 

required by this rule. Thus, Executive 

Order 13132 does not apply to this 

action. 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

This action does not have tribal 

implications, as specified in Executive 

Order 13175 (65 FR 67249, November 9, 

2000). In cases where a source of PM2.5

emissions is owned by a tribal 

government, those governments may 

incur minimal compliance costs 

associated with conducting tests to 

quantify PM2.5 emissions using the 

revised methods when they are 

promulgated. However, such tests 

would be conducted at the discretion of 

the tribal government and the 

compliance costs are not expected to 

impose a significant burden on those 

governments. Thus, Executive Order 

13175 does not apply to this action. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

and Safety Risks 

EPA interprets Executive Order 13045 

(62 FR 19885, April 23, 1997) as 

applying only to those regulatory 

actions that concern health or safety 

risks, such that the analysis required 

under section 5–501 of the Executive 

Order has the potential to influence the 

regulation. This action is not subject to 

Executive Order 13045 because it does 

not establish an environmental standard 

intended to mitigate health or safety 

risks. 

H. Executive Order 13211: Actions 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution, or Use 

This action is not subject to Executive 

Order 13211 (66 FR 28355, May 22, 

2001) because it is not a significant 

regulatory action under Executive Order 

12866. 

I. National Technology Transfer and 

Advancement Act 

Section 12(d) of the National 

Technology Transfer and Advancement 

Act of 1995 (NTTAA), Public Law 104– 

113, 12(d) (15 U.S.C. 272 note) directs 

EPA to use voluntary consensus 

standards in its regulatory activities 

unless to do so would be inconsistent 

with applicable law or otherwise 

impractical. Voluntary consensus 

standards are technical standards (e.g., 

materials specifications, test methods, 

sampling procedures, and business 

practices) that are developed or adopted 

by voluntary consensus standards 

bodies. NTTAA directs EPA to provide 

Congress, through OMB, explanations 

when the Agency decides not to use 

available and applicable voluntary 

consensus standards. 

This action involves technical 

standards. EPA has decided to use two 

voluntary consensus standards that 

were identified at proposal to be 

applicable for use within the amended 

test methods. The first voluntary 

consensus standard cited in proposed 

Method 202 was ASTM International 

Method D2986–95a (1999), ‘‘Standard 

Method for Evaluation of Air, Assay 

Media by the Monodisperse DOP 

(Dioctyl Phthalate) Smoke Test,’’ for its 

procedures to conduct filter efficiency 

tests. In the final Method 202, we 

replaced the prescriptive requirement to 

use a filter meeting ASTM International 

D2986–95a (1999) with a performancebased requirement limiting the residual 

mass contribution. The performance 

based approach specifies that the CPM 

filter must be a non-reactive, nondisintegrating filter that does not 

contribute more than 0.5 mg of residual 

mass to the CPM measurements. 

Regarding efficiency, the CPM filter 

must have an efficiency of at least 99.95 

percent (< 0.05 percent penetration) on 

0.3 μm particles. 

The second voluntary consensus 

standard cited in proposed Method 202 

was ASTM International D1193–06, 

‘‘Standard Specification for Reagent 

Water,’’ for the proper selection of 

distilled ultra-filtered water. In response 

to public comments, we applied a 


jlentini on DSKJ8SOYB1PROD with RULES2
80134 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

performance-based approach in the final 

Method 202 that requires deionized, 

ultra-filtered water that contains 1.0 

ppmw (1 mg/L) residual mass or less. 

J. Executive Order 12898: Federal 

Actions To Address Environmental 

Justice in Minority Populations and 

Low-Income Populations 

Executive Order 12898 (59 FR 7629, 

February 16, 1994) establishes federal 

executive policy on environmental 

justice. Its main provision directs 

federal agencies, to the greatest extent 

practicable and permitted by law, to 

make environmental justice part of their 

mission by identifying and addressing, 

as appropriate, disproportionately high 

and adverse human health or 

environmental effects of their programs, 

policies, and activities on minority 

populations and low-income 

populations in the United States. 

EPA has determined that this final 

rule will not have disproportionately 

high and adverse human health or 

environmental effects on minority or 

low-income populations because it 

increases the level of environmental 

protection for all affected populations 

without having any disproportionately 

high and adverse human health or 

environmental effects on any 

population, including any minority or 

low-income population. The final 

amendments revise existing test 

methods to improve the accuracies of 

the measurements that are expected to 

improve environmental quality and 

reduce health risks for areas that may be 

designated as nonattainment. 

K. Congressional Review Act 

The Congressional Review Act, 5 

U.S.C. 801 et seq., as added by the Small 

Business Regulatory Enforcement 

Fairness Act of 1996, generally provides 

that before a rule may take effect, the 

agency promulgating the rule must 

submit a rule report, which includes a 

copy of the rule, to each House of the 

Congress and to the Comptroller General 

of the United States. Section 808 allows 

the issuing agency to make a rule 

effective sooner than otherwise 

provided by the CRA if the agency 

makes a good cause finding that notice 

and public procedure is impracticable, 

unnecessary or contrary to the public 

interest. This determination must be 

supported by a brief statement. 5 U.S.C. 

808(2). As stated previously, EPA has 

made such a good cause finding, 

including the reasons therefore, and 

established an effective date of January 

1, 2011 (see section I.C, supra). EPA will 

submit a report containing this rule and 

other required information to the U.S. 

Senate, the U.S. House of 

Representatives, and the Comptroller 

General of the United States prior to 

publication of the rule in the Federal 

Register. This action is not a ‘‘major 

rule’’ as defined by 5 U.S.C. 804(2). 

List of Subjects in 40 CFR Part 51 

Administrative practice and 

procedure, Air pollution control, Carbon 

monoxide, Intergovernmental relations, 

Lead, Nitrogen oxide, Ozone, PM, 

Reporting and recordkeeping 

requirements, Sulfur compounds, 

Volatile organic compounds. 

Dated: December 1, 2010. 

Lisa P. Jackson, 

Administrator. 

■ For the reasons stated in the preamble, 

title 40, chapter I of the Code of Federal 

Regulations is amended as follows: 

PART 51—[AMENDED] 

■ 1. The authority citation for part 51 

continues to read as follows: 

Authority: 23 U.S.C. 101; 42 U.S.C 7401– 

7671q. 

■ 2. Amend appendix M by revising 

Methods 201A and 202 to read as 

follows: 

Appendix M to Part 51—Recommended 

Test Methods for State Implementation 

Plans 

* * * * * 

METHOD 201A—DETERMINATION OF 

PM10 AND PM2.5 EMISSIONS FROM 

STATIONARY SOURCES (Constant 

Sampling Rate Procedure) 

1.0 Scope and Applicability 

1.1 Scope. The U.S. Environmental 

Protection Agency (U.S. EPA or ‘‘we’’) 

developed this method to describe the 

procedures that the stack tester (‘‘you’’) must 

follow to measure filterable particulate 

matter (PM) emissions equal to or less than 

a nominal aerodynamic diameter of 10 

micrometers (PM10) and 2.5 micrometers 

(PM2.5). This method can be used to measure 

coarse particles (i.e., the difference between 

the measured PM10 concentration and the 

measured PM2.5 concentration). 

1.2 Applicability. This method addresses 

the equipment, preparation, and analysis 

necessary to measure filterable PM. You can 

use this method to measure filterable PM 

from stationary sources only. Filterable PM is 

collected in stack with this method (i.e., the 

method measures materials that are solid or 

liquid at stack conditions). If the gas filtration 

temperature exceeds 30 °C (85 °F), then you 

may use the procedures in this method to 

measure only filterable PM (material that 

does not pass through a filter or a cyclone/ 

filter combination). If the gas filtration 

temperature exceeds 30 °C (85 °F), and you 

must measure both the filterable and 

condensable (material that condenses after 

passing through a filter) components of total 

primary (direct) PM emissions to the 

atmosphere, then you must combine the 

procedures in this method with the 

procedures in Method 202 of appendix M to 

this part for measuring condensable PM. 

However, if the gas filtration temperature 

never exceeds 30 °C (85 °F), then use of 

Method 202 of appendix M to this part is not 

required to measure total primary PM. 

1.3 Responsibility. You are responsible 

for obtaining the equipment and supplies you 

will need to use this method. You must also 

develop your own procedures for following 

this method and any additional procedures to 

ensure accurate sampling and analytical 

measurements. 

1.4 Additional Methods. To obtain 

results, you must have a thorough knowledge 

of the following test methods found in 

appendices A–1 through A–3 of 40 CFR part 

60: 

(a) Method 1—Sample and velocity 

traverses for stationary sources. 

(b) Method 2—Determination of stack gas 

velocity and volumetric flow rate (Type S 

pitot tube). 

(c) Method 3—Gas analysis for the 

determination of dry molecular weight. 

(d) Method 4—Determination of moisture 

content in stack gases. 

(e) Method 5—Determination of particulate 

matter emissions from stationary sources. 

1.5 Limitations. You cannot use this 

method to measure emissions in which water 

droplets are present because the size 

separation of the water droplets may not be 

representative of the dry particle size 

released into the air. To measure filterable 

PM10 and PM2.5 in emissions where water 

droplets are known to exist, we recommend 

that you use Method 5 of appendix A–3 to 

part 60. Because of the temperature limit of 

the O-rings used in this sampling train, you 

must follow the procedures in Section 8.6.1 

to test emissions from stack gas temperatures 

exceeding 205 °C (400 °F). 

1.6 Conditions. You can use this method 

to obtain particle sizing at 10 micrometers 

and or 2.5 micrometers if you sample within 

80 and 120 percent of isokinetic flow. You 

can also use this method to obtain total 

filterable particulate if you sample within 90 

to 110 percent of isokinetic flow, the number 

of sampling points is the same as required by 

Method 5 of appendix A–3 to part 60 or 

Method 17 of appendix A–6 to part 60, and 

the filter temperature is within an acceptable 

range for these methods. For Method 5, the 

acceptable range for the filter temperature is 

generally 120 °C (248 °F) unless a higher or 

lower temperature is specified. The 

acceptable range varies depending on the 

source, control technology and applicable 

rule or permit condition. To satisfy Method 

5 criteria, you may need to remove the instack filter and use an out-of-stack filter and 

recover the PM in the probe between the 

PM2.5 particle sizer and the filter. In addition, 

to satisfy Method 5 and Method 17 criteria, 

you may need to sample from more than 12 

traverse points. Be aware that this method 

determines in-stack PM10 and PM2.5 filterable 

emissions by sampling from a recommended 

maximum of 12 sample points, at a constant 

flow rate through the train (the constant flow 

is necessary to maintain the size cuts of the 

cyclones), and with a filter that is at the stack 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80135 

temperature. In contrast, Method 5 or Method 

17 trains are operated isokinetically with 

varying flow rates through the train. Method 

5 and Method 17 require sampling from as 

many as 24 sample points. Method 5 uses an 

out-of-stack filter that is maintained at a 

constant temperature of 120 °C (248 °F). 

Further, to use this method in place of 

Method 5 or Method 17, you must extend the 

sampling time so that you collect the 

minimum mass necessary for weighing each 

portion of this sampling train. Also, if you 

are using this method as an alternative to a 

test method specified in a regulatory 

requirement (e.g., a requirement to conduct a 

compliance or performance test), then you 

must receive approval from the authority that 

established the regulatory requirement before 

you conduct the test. 

2.0 Summary of Method 

2.1 Summary. To measure PM10 and 

PM2.5, extract a sample of gas at a 

predetermined constant flow rate through an 

in-stack sizing device. The particle-sizing 

device separates particles with nominal 

aerodynamic diameters of 10 micrometers 

and 2.5 micrometers. To minimize variations 

in the isokinetic sampling conditions, you 

must establish well-defined limits. After a 

sample is obtained, remove uncombined 

water from the particulate, then use 

gravimetric analysis to determine the 

particulate mass for each size fraction. The 

original method, as promulgated in 1990, has 

been changed by adding a PM2.5 cyclone 

downstream of the PM10 cyclone. Both 

cyclones were developed and evaluated as 

part of a conventional five-stage cascade 

cyclone train. The addition of a PM2.5

cyclone between the PM10 cyclone and the 

stack temperature filter in the sampling train 

supplements the measurement of PM10 with 

the measurement of PM2.5. Without the 

addition of the PM2.5 cyclone, the filterable 

particulate portion of the sampling train may 

be used to measure total and PM10 emissions. 

Likewise, with the exclusion of the PM10

cyclone, the filterable particulate portion of 

the sampling train may be used to measure 

total and PM2.5 emissions. Figure 1 of Section 

17 presents the schematic of the sampling 

train configured with this change. 

3.0 Definitions 

3.1 Condensable particulate matter (CPM) 

means material that is vapor phase at stack 

conditions, but condenses and/or reacts upon 

cooling and dilution in the ambient air to 

form solid or liquid PM immediately after 

discharge from the stack. Note that all CPM 

is assumed to be in the PM2.5 size fraction. 

3.2 Constant weight means a difference of 

no more than 0.5 mg or one percent of total 

weight less tare weight, whichever is greater, 

between two consecutive weighings, with no 

less than six hours of desiccation time 

between weighings. 

3.3 Filterable particulate matter (PM) 

means particles that are emitted directly by 

a source as a solid or liquid at stack or release 

conditions and captured on the filter of a 

stack test train. 

3.4 Primary particulate matter (PM) (also 

known as direct PM) means particles that 

enter the atmosphere as a direct emission 

from a stack or an open source. Primary PM 

has two components: Filterable PM and 

condensable PM. These two PM components 

have no upper particle size limit. 

3.5 Primary PM2.5 (also known as direct 

PM2.5, total PM2.5, PM2.5, or combined 

filterable PM2.5 and condensable PM) means 

PM with an aerodynamic diameter less than 

or equal to 2.5 micrometers. These solid 

particles are emitted directly from an air 

emissions source or activity, or are the 

gaseous or vaporous emissions from an air 

emissions source or activity that condense to 

form PM at ambient temperatures. Direct 

PM2.5 emissions include elemental carbon, 

directly emitted organic carbon, directly 

emitted sulfate, directly emitted nitrate, and 

other inorganic particles (including but not 

limited to crustal material, metals, and sea 

salt). 

3.6 Primary PM10 (also known as direct 

PM10, total PM10, PM10, or the combination 

of filterable PM10 and condensable PM) 

means PM with an aerodynamic diameter 

equal to or less than 10 micrometers. 

4.0 Interferences 

You cannot use this method to measure 

emissions where water droplets are present 

because the size separation of the water 

droplets may not be representative of the dry 

particle size released into the air. Stacks with 

entrained moisture droplets may have water 

droplets larger than the cut sizes for the 

cyclones. These water droplets normally 

contain particles and dissolved solids that 

become PM10 and PM2.5 following 

evaporation of the water. 

5.0 Safety 

5.1 Disclaimer. Because the performance 

of this method may require the use of 

hazardous materials, operations, and 

equipment, you should develop a health and 

safety plan to ensure the safety of your 

employees who are on site conducting the 

particulate emission test. Your plan should 

conform with all applicable Occupational 

Safety and Health Administration, Mine 

Safety and Health Administration, and 

Department of Transportation regulatory 

requirements. Because of the unique 

situations at some facilities and because 

some facilities may have more stringent 

requirements than is required by State or 

federal laws, you may have to develop 

procedures to conform to the plant health 

and safety requirements. 

6.0 Equipment and Supplies 

Figure 2 of Section 17 shows details of the 

combined cyclone heads used in this 

method. The sampling train is the same as 

Method 17 of appendix A–6 to part 60 with 

the exception of the PM10 and PM2.5 sizing 

devices. The following sections describe the 

sampling train’s primary design features in 

detail. 

6.1 Filterable Particulate Sampling Train 

Components. 

6.1.1 Nozzle. You must use stainless steel 

(316 or equivalent) or fluoropolymer-coated 

stainless steel nozzles with a sharp tapered 

leading edge. We recommend one of the 12 

nozzles listed in Figure 3 of Section 17 

because they meet design specifications 

when PM10 cyclones are used as part of the 

sampling train. We also recommend that you 

have a large number of nozzles in small 

diameter increments available to increase the 

likelihood of using a single nozzle for the 

entire traverse. We recommend one of the 

nozzles listed in Figure 4A or 4B of Section 

17 because they meet design specifications 

when PM2.5 cyclones are used without PM10

cyclones as part of the sampling train. 

6.1.2 PM10 and PM2.5 Sizing Device. 

6.1.2.1 Use stainless steel (316 or 

equivalent) or fluoropolymer-coated PM10

and PM2.5 sizing devices. You may use sizing 

devices constructed of high-temperature 

specialty metals such as Inconel, Hastelloy, 

or Haynes 230. (See also Section 8.6.1.) The 

sizing devices must be cyclones that meet the 

design specifications shown in Figures 3, 4A, 

4B, 5, and 6 of Section 17. Use a caliper to 

verify that the dimensions of the PM10 and 

PM2.5 sizing devices are within ± 0.02 cm of 

the design specifications. Example suppliers 

of PM10 and PM2.5 sizing devices include the 

following: 

(a) Environmental Supply Company, Inc., 

2142 E. Geer Street, Durham, North Carolina 

27704. Telephone No.: (919) 956–9688; Fax: 

(919) 682–0333. 

(b) Apex Instruments, 204 Technology Park 

Lane, Fuquay-Varina, North Carolina 27526. 

Telephone No.: (919) 557–7300 (phone); Fax: 

(919) 557–7110. 

6.1.2.2 You may use alternative particle 

sizing devices if they meet the requirements 

in Development and Laboratory Evaluation of 

a Five-Stage Cyclone System, EPA–600/7– 

78–008 (http://cfpub.epa.gov/ols). 

6.1.3 Filter Holder. Use a filter holder 

that is stainless steel (316 or equivalent). A 

heated glass filter holder may be substituted 

for the steel filter holder when filtration is 

performed out-of-stack. Commercial-size 

filter holders are available depending upon 

project requirements, including commercial 

stainless steel filter holders to support 25-, 

47-, 63-, 76-, 90-, 101-, and 110-mm diameter 

filters. Commercial size filter holders contain 

a fluoropolymer O-ring, a stainless steel 

screen that supports the particulate filter, and 

a final fluoropolymer O-ring. Screw the 

assembly together and attach to the outlet of 

cyclone IV. The filter must not be 

compressed between the fluoropolymer Oring and the filter housing. 

6.1.4 Pitot Tube. You must use a pitot 

tube made of heat resistant tubing. Attach the 

pitot tube to the probe with stainless steel 

fittings. Follow the specifications for the 

pitot tube and its orientation to the inlet 

nozzle given in Section 6.1.1.3 of Method 5 

of appendix A–3 to part 60. 

6.1.5 Probe Extension and Liner. The 

probe extension must be glass- or 

fluoropolymer-lined. Follow the 

specifications in Section 6.1.1.2 of Method 5 

of appendix A–3 to part 60. If the gas 

filtration temperature never exceeds 30 °C 

(85 °F), then the probe may be constructed 

of stainless steel without a probe liner and 

the extension is not recovered as part of the 

PM. 

6.1.6 Differential Pressure Gauge, 

Condensers, Metering Systems, Barometer, 

and Gas Density Determination Equipment. 

Follow the requirements in Sections 6.1.1.4 


jlentini on DSKJ8SOYB1PROD with RULES2
80136 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

through 6.1.3 of Method 5 of appendix A–3 

to part 60, as applicable. 

6.2 Sample Recovery Equipment. 

6.2.1 Filterable Particulate Recovery. Use 

the following equipment to quantitatively 

determine the amount of filterable PM 

recovered from the sampling train. 

(a) Cyclone and filter holder brushes. 

(b) Wash bottles. Two wash bottles are 

recommended. Any container material is 

acceptable, but wash bottles used for sample 

and blank recovery must not contribute more 

than 0.1 mg of residual mass to the CPM 

measurements. 

(c) Leak-proof sample containers. 

Containers used for sample and blank 

recovery must not contribute more than 0.05 

mg of residual mass to the CPM 

measurements. 

(d) Petri dishes. For filter samples; glass or 

polyethylene, unless otherwise specified by 

the Administrator. 

(e) Graduated cylinders. To measure 

condensed water to within 1 ml or 0.5 g. 

Graduated cylinders must have subdivisions 

not greater than 2 ml. 

(f) Plastic storage containers. Air-tight 

containers to store silica gel. 

6.2.2 Analysis Equipment. 

(a) Funnel. Glass or polyethylene, to aid in 

sample recovery. 

(b) Rubber policeman. To aid in transfer of 

silica gel to container; not necessary if silica 

gel is weighed in the field. 

(c) Analytical balance. Analytical balance 

capable of weighing at least 0.0001 g (0.1 

mg). 

(d) Balance. To determine the weight of the 

moisture in the sampling train components, 

use an analytical balance accurate to ± 0.5 g. 

(e) Fluoropolymer beaker liners. 

7.0 Reagents, Standards, and Sampling 

Media 

7.1 Sample Collection. To collect a 

sample, you will need a filter and silica gel. 

You must also have water and crushed ice. 

These items must meet the following 

specifications. 

7.1.1 Filter. Use a nonreactive, 

nondisintegrating glass fiber, quartz, or 

polymer filter that does not a have an organic 

binder. The filter must also have an 

efficiency of at least 99.95 percent (less than 

0.05 percent penetration) on 0.3 micrometer 

dioctyl phthalate particles. You may use test 

data from the supplier’s quality control 

program to document the PM filter efficiency. 

7.1.2 Silica Gel. Use an indicating-type 

silica gel of 6 to 16 mesh. You must obtain 

approval from the regulatory authority that 

established the requirement to use this test 

method to use other types of desiccants 

(equivalent or better) before you use them. 

Allow the silica gel to dry for two hours at 

175 °C (350 °F) if it is being reused. You do 

not have to dry new silica gel if the indicator 

shows the silica is active for moisture 

collection. 

7.1.3 Crushed Ice. Obtain from the best 

readily available source. 

7.1.4 Water. Use deionized, ultra-filtered 

water that contains 1.0 part per million by 

weight (1 milligram/liter) residual mass or 

less to recover and extract samples. 

7.2 Sample Recovery and Analytical 

Reagents. You will need acetone and 

anhydrous calcium sulfate for the sample 

recovery and analysis. Unless otherwise 

indicated, all reagents must conform to the 

specifications established by the Committee 

on Analytical Reagents of the American 

Chemical Society. If such specifications are 

not available, then use the best available 

grade. Additional information on each of 

these items is in the following paragraphs. 

7.2.1 Acetone. Use acetone that is stored 

in a glass bottle. Do not use acetone from a 

metal container because it will likely 

produce a high residue in the laboratory and 

field reagent blanks. You must use acetone 

with blank values less than 1 part per million 

by weight residue. Analyze acetone blanks 

prior to field use to confirm low blank 

values. In no case shall a blank value of 

greater than 0.0001 percent (1 part per 

million by weight) of the weight of acetone 

used in sample recovery be subtracted from 

the sample weight (i.e., the maximum blank 

correction is 0.1 mg per 100 ml of acetone 

used to recover samples). 

7.2.2 Particulate Sample Desiccant. Use 

indicating-type anhydrous calcium sulfate to 

desiccate samples prior to weighing. 

8.0 Sample Collection, Preservation, 

Storage, and Transport 

8.1 Qualifications. This is a complex test 

method. To obtain reliable results, you 

should be trained and experienced with instack filtration systems (such as cyclones, 

impactors, and thimbles) and impinger and 

moisture train systems. 

8.2 Preparations. Follow the pretest 

preparation instructions in Section 8.1 of 

Method 5 of appendix A–3 to part 60. 

8.3 Site Setup. You must complete the 

following to properly set up for this test: 

(a) Determine the sampling site location 

and traverse points. 

(b) Calculate probe/cyclone blockage. 

(c) Verify the absence of cyclonic flow. 

(d) Complete a preliminary velocity profile 

and select a nozzle(s) and sampling rate. 

8.3.1 Sampling Site Location and 

Traverse Point Determination. Follow the 

standard procedures in Method 1 of 

appendix A–1 to part 60 to select the 

appropriate sampling site. Choose a location 

that maximizes the distance from upstream 

and downstream flow disturbances. 

(a) Traverse points. The required maximum 

number of total traverse points at any 

location is 12, as shown in Figure 7 of 

Section 17. You must prevent the disturbance 

and capture of any solids accumulated on the 

inner wall surfaces by maintaining a 1-inch 

distance from the stack wall (0.5 inch for 

sampling locations less than 36.4 inches in 

diameter with the pitot tube and 32.4 inches 

without the pitot tube). During sampling, 

when the PM2.5 cyclone is used without the 

PM10, traverse points closest to the stack 

walls may not be reached because the inlet 

to a PM2.5 cyclone is located approximately 

2.75 inches from the end of the cyclone. For 

these cases, you may collect samples using 

the procedures in Section 11.3.2.2 of Method 

1 of appendix A–3 to part 60. You must use 

the traverse point closest to the unreachable 

sampling points as replacement for the 

unreachable points. You must extend the 

sampling time at the replacement sampling 

point to include the duration of the 

unreachable traverse points. 

(b) Round or rectangular duct or stack. If 

a duct or stack is round with two ports 

located 90° apart, use six sampling points on 

each diameter. Use a 3x4 sampling point 

layout for rectangular ducts or stacks. 

Consult with the Administrator to receive 

approval for other layouts before you use 

them. 

(c) Sampling ports. You must determine if 

the sampling ports can accommodate the instack cyclones used in this method. You may 

need larger diameter sampling ports than 

those used by Method 5 of appendix A–3 to 

part 60 or Method 17 of appendix A–6 to part 

60 for total filterable particulate sampling. 

When you use nozzles smaller than 0.16 inch 

in diameter and either a PM10 or a combined 

PM10 and PM2.5 sampling apparatus, the 

sampling port diameter may need to be six 

inches in diameter to accommodate the entire 

apparatus because the conventional 4-inch 

diameter port may be too small due to the 

combined dimension of the PM10 cyclone 

and the nozzle extending from the cyclone, 

which will likely exceed the internal 

diameter of the port. A 4-inch port should be 

adequate for the single PM2.5 sampling 

apparatus. However, do not use the 

conventional 4-inch diameter port in any 

circumstances in which the combined 

dimension of the cyclone and the nozzle 

extending from the cyclone exceeds the 

internal diameter of the port. (Note: If the 

port nipple is short, you may be able to 

‘‘hook’’ the sampling head through a smaller 

port into the duct or stack.) 

8.3.2 Probe/Cyclone Blockage 

Calculations. Follow the procedures in the 

next two sections, as appropriate. 

8.3.2.1 Ducts with diameters greater than 

36.4 inches. Based on commercially available 

cyclone assemblies for this procedure, ducts 

with diameters greater than 36.4 inches have 

blockage effects less than three percent, as 

illustrated in Figure 8 of Section 17. You 

must minimize the blockage effects of the 

combination of the in-stack nozzle/cyclones, 

pitot tube, and filter assembly that you use 

by keeping the cross-sectional area of the 

assembly at three percent or less of the crosssectional area of the duct. 

8.3.2.2 Ducts with diameters between 

25.7 and 36.4 inches. Ducts with diameters 

between 25.7 and 36.4 inches have blockage 

effects ranging from three to six percent, as 

illustrated in Figure 8 of Section 17. 

Therefore, when you conduct tests on these 

small ducts, you must adjust the observed 

velocity pressures for the estimated blockage 

factor whenever the combined sampling 

apparatus blocks more than three percent of 

the stack or duct (see Sections 8.7.2.2 and 

8.7.2.3 on the probe blockage factor and the 

final adjusted velocity pressure, 

respectively). (Note: Valid sampling with the 

combined PM2.5/PM10 cyclones cannot be 

performed with this method if the average 

stack blockage from the sampling assembly is 

greater than six percent, i.e., the stack 

diameter is less than 26.5 inches.) 

8.3.3 Cyclonic Flow. Do not use the 

combined cyclone sampling head at sampling 

locations subject to cyclonic flow. Also, you 

must follow procedures in Method 1 of 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80137 

appendix A–1 to part 60 to determine the 

presence or absence of cyclonic flow and 

then perform the following calculations: 

(a) As per Section 11.4 of Method 1 of 

appendix A–1 to part 60, find and record the 

angle that has a null velocity pressure for 

each traverse point using an S-type pitot 

tube. 

(b) Average the absolute values of the 

angles that have a null velocity pressure. Do 

not use the sampling location if the average 

absolute value exceeds 20°. (Note: You can 

minimize the effects of cyclonic flow 

conditions by moving the sampling location, 

placing gas flow straighteners upstream of 

the sampling location, or applying a modified 

sampling approach as described in EPA 

Guideline Document GD–008, Particulate 

Emissions Sampling in Cyclonic Flow. You 

may need to obtain an alternate method 

approval from the regulatory authority that 

established the requirement to use this test 

method prior to using a modified sampling 

approach.) 

8.3.4 Preliminary Velocity Profile. 

Conduct a preliminary velocity traverse by 

following Method 2 of appendix A–1 to part 

60 velocity traverse procedures. The purpose 

of the preliminary velocity profile is to 

determine all of the following: 

(a) The gas sampling rate for the combined 

probe/cyclone sampling head in order to 

meet the required particle size cut. 

(b) The appropriate nozzle to maintain the 

required gas sampling rate for the velocity 

pressure range and isokinetic range. If the 

isokinetic range cannot be met (e.g., batch 

processes, extreme process flow or 

temperature variation), void the sample or 

use methods subject to the approval of the 

Administrator to correct the data. The 

acceptable variation from isokinetic sampling 

is 80 to 120 percent and no more than 100 

± 29 percent (two out of 12 or five out of 24) 

sampling points outside of this criteria. 

(c) The necessary sampling duration to 

obtain sufficient particulate catch weights. 

8.3.4.1 Preliminary traverse. You must 

use an S-type pitot tube with a conventional 

thermocouple to conduct the traverse. 

Conduct the preliminary traverse as close as 

possible to the anticipated testing time on 

sources that are subject to hour-by-hour gas 

flow rate variations of approximately ± 20 

percent and/or gas temperature variations of 

approximately ± 10 °C (± 50 °F). (Note: You 

should be aware that these variations can 

cause errors in the cyclone cut diameters and 

the isokinetic sampling velocities.) 

8.3.4.2 Velocity pressure range. Insert the 

S-type pitot tube at each traverse point and 

record the range of velocity pressures 

measured on data form in Method 2 of 

appendix A–1 to part 60. You will use this 

later to select the appropriate nozzle. 

8.3.4.3 Initial gas stream viscosity and 

molecular weight. Determine the average gas 

temperature, average gas oxygen content, 

average carbon dioxide content, and 

estimated moisture content. You will use this 

information to calculate the initial gas stream 

viscosity (Equation 3) and molecular weight 

(Equations 1 and 2). (Note: You must follow 

the instructions outlined in Method 4 of 

appendix A–3 to part 60 or Alternative 

Moisture Measurement Method Midget 

Impingers (ALT–008) to estimate the 

moisture content. You may use a wet bulbdry bulb measurement or hand-held 

hygrometer measurement to estimate the 

moisture content of sources with gas 

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

8.3.4.4 Approximate PM concentration in 

the gas stream. Determine the approximate 

PM concentration for the PM2.5 and the PM2.5

to PM10 components of the gas stream 

through qualitative measurements or 

estimates from precious stack particulate 

emissions tests. Having an idea of the 

particulate concentration in the gas stream is 

not essential but will help you determine the 

appropriate sampling time to acquire 

sufficient PM weight for better accuracy at 

the source emission level. The collectable PM 

weight requirements depend primarily on the 

types of filter media and weighing 

capabilities that are available and needed to 

characterize the emissions. Estimate the 

collectable PM concentrations in the greater 

than 10 micrometer, less than or equal to 10 

micrometers and greater than 2.5 

micrometers, and less than or equal to 2.5 

micrometer size ranges. Typical PM 

concentrations are listed in Table 1 of 

Section 17. Additionally, relevant sections of 

AP–42, Compilation of Air Pollutant 

Emission Factors, may contain particle size 

distributions for processes characterized in 

those sections, and appendix B2 of AP–42 

contains generalized particle size 

distributions for nine industrial process 

categories (e.g., stationary internal 

combustion engines firing gasoline or diesel 

fuel, calcining of aggregate or unprocessed 

ores). The generalized particle size 

distributions can be used if source-specific 

particle size distributions are unavailable. 

Appendix B2 of AP–42 also contains typical 

collection efficiencies of various particulate 

control devices and example calculations 

showing how to estimate uncontrolled total 

particulate emissions, uncontrolled sizespecific emissions, and controlled sizespecific particulate emissions. (http:// 

www.epa.gov/ttnchie1/ap42.) 

8.4 Pre-test Calculations. You must 

perform pre-test calculations to help select 

the appropriate gas sampling rate through 

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

Choosing the appropriate sampling rate will 

allow you to maintain the appropriate 

particle cut diameters based upon 

preliminary gas stream measurements, as 

specified in Table 2 of Section 17. 

8.4.1 Gas Sampling Rate. The gas 

sampling rate is defined by the performance 

curves for both cyclones, as illustrated in 

Figure 10 of Section 17. You must use the 

calculations in Section 8.5 to achieve the 

appropriate cut size specification for each 

cyclone. The optimum gas sampling rate is 

the overlap zone defined as the range below 

the cyclone IV 2.25 micrometer curve down 

to the cyclone I 11.0 micrometer curve (area 

between the two dark, solid lines in Figure 

10 of Section 17). 

8.4.2 Choosing the Appropriate Sampling 

Rate. You must select a gas sampling rate in 

the middle of the overlap zone (discussed in 

Section 8.4.1), as illustrated in Figure 10 of 

Section 17, to maximize the acceptable 

tolerance for slight variations in flow 

characteristics at the sampling location. The 

overlap zone is also a weak function of the 

gas composition. (Note: The acceptable range 

is limited, especially for gas streams with 

temperatures less than approximately 100 °F. 

At lower temperatures, it may be necessary 

to perform the PM10 and PM2.5 separately in 

order to meet the necessary particle size 

criteria shown in Table 2 of Section 17.) 

8.5 Test Calculations. You must perform 

all of the calculations in Table 3 of Section 

17 and the calculations described in Sections 

8.5.1 through 8.5.5. 

8.5.1 Assumed Reynolds Number. You 

must select an assumed Reynolds number 

(Nre) using Equation 10 and an estimated 

sampling rate or from prior experience under 

the stack conditions determined using 

Methods 1 through 4 to part 60. You will 

perform initial test calculations based on an 

assumed Nre for the test to be performed. You 

must verify the assumed Nre by substituting 

the sampling rate (Qs) calculated in Equation 

7 into Equation 10. Then use Table 5 of 

Section 17 to determine if the Nre used in 

Equation 5 was correct. 

8.5.2 Final Sampling Rate. Recalculate 

the final Qs if the assumed Nre used in your 

initial calculation is not correct. Use 

Equation 7 to recalculate the optimum Qs. 

8.5.3 Meter Box DH. Use Equation 11 to 

calculate the meter box orifice pressure drop 

(DH) after you calculate the optimum 

sampling rate and confirm the Nre. (Note: The 

stack gas temperature may vary during the 

test, which could affect the sampling rate. If 

the stack gas temperature varies, you must 

make slight adjustments in the meter box DH 

to maintain the correct constant cut 

diameters. Therefore, use Equation 11 to 

recalculate the DH values for 50 °F above and 

below the stack temperature measured during 

the preliminary traverse (see Section 8.3.4.1), 

and document this information in Table 4 of 

Section 17.) 

8.5.4 Choosing a Sampling Nozzle. Select 

one or more nozzle sizes to provide for near 

isokinetic sampling rate (see Section 1.6). 

This will also minimize an isokinetic 

sampling error for the particles at each point. 

First calculate the mean stack gas velocity 

(vs) using Equation 13. See Section 8.7.2 for 

information on correcting for blockage and 

use of different pitot tube coefficients. Then 

use Equation 14 to calculate the diameter (D) 

of a nozzle that provides for isokinetic 

sampling at the mean vs at flow Qs. From the 

available nozzles one size smaller and one 

size larger than this diameter, D, select the 

most appropriate nozzle. Perform the 

following steps for the selected nozzle. 

8.5.4.1 Minimum/maximum nozzle/stack 

velocity ratio. Use Equation 15 to determine 

the velocity of gas in the nozzle. Use 

Equation 16 to calculate the minimum 

nozzle/stack velocity ratio (Rmin). Use 

Equation 17 to calculate the maximum 

nozzle/stack velocity ratio (Rmax). 

8.5.4.2 Minimum gas velocity. Use 

Equation 18 to calculate the minimum gas 

velocity (vmin) if Rmin is an imaginary number 

(negative value under the square root 

function) or if Rmin is less than 0.5. Use 

Equation 19 to calculate vmin if Rmin is ≥ 0.5. 

8.5.4.3 Maximum stack velocity. Use 

Equation 20 to calculate the maximum stack 


jlentini on DSKJ8SOYB1PROD with RULES2
80138 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

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

Equation 21 to calculate the stack velocity if 

Rmax is ≥ 1.5. 

8.5.4.4 Conversion of gas velocities to 

velocity pressure. Use Equation 22 to convert 

vmin to minimum velocity pressure, Dpmin. 

Use Equation 23 to convert vmax to maximum 

velocity pressure, Dpmax. 

8.5.4.5 Comparison to observed velocity 

pressures. Compare minimum and maximum 

velocity pressures with the observed velocity 

pressures at all traverse points during the 

preliminary test (see Section 8.3.4.2). 

8.5.5 Optimum Sampling Nozzle. The 

nozzle you selected is appropriate if all the 

observed velocity pressures during the 

preliminary test fall within the range of the 

Dpmin and Dpmax. Make sure the following 

requirements are met then follow the 

procedures in Sections 8.5.5.1 and 8.5.5.2. 

(a) Choose an optimum nozzle that 

provides for isokinetic sampling conditions 

as close to 100 percent as possible. This is 

prudent because even if there are slight 

variations in the gas flow rate, gas 

temperature, or gas composition during the 

actual test, you have the maximum assurance 

of satisfying the isokinetic criteria. Generally, 

one of the two candidate nozzles selected 

will be closer to optimum (see Section 8.5.4). 

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

allowed a 16 percent failure rate, rounded to 

the nearest whole number, of sampling 

points that are outside the range of the Dpmin

and Dpmax. If the coarse fraction for PM10

determination is included, you are allowed 

only an eight percent failure rate of the 

sampling points, rounded to the nearest 

whole number, outside the Dpmin and Dpmax. 

8.5.5.1 Precheck. Visually check the 

selected nozzle for dents before use. 

8.5.5.2 Attach the pre-selected nozzle. 

Screw the pre-selected nozzle onto the main 

body of cyclone I using fluoropolymer tape. 

Use a union and cascade adaptor to connect 

the cyclone IV inlet to the outlet of cyclone 

I (see Figure 2 of Section 17). 

8.6 Sampling Train Preparation. A 

schematic of the sampling train used in this 

method is shown in Figure 1 of Section 17. 

First, assemble the train and complete the 

leak check on the combined cyclone 

sampling head and pitot tube. Use the 

following procedures to prepare the sampling 

train. (Note: Do not contaminate the sampling 

train during preparation and assembly. Keep 

all openings, where contamination can occur, 

covered until just prior to assembly or until 

sampling is about to begin.) 

8.6.1 Sampling Head and Pitot Tube. 

Assemble the combined cyclone train. The 

O-rings used in the train have a temperature 

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

cyclones with stainless steel sealing rings for 

stack temperatures above 205 °C (400 °F) up 

to 260 °C (500 °F). You must also keep the 

nozzle covered to protect it from nicks and 

scratches. This method may not be suitable 

for sources with stack gas temperatures 

exceeding 260 °C (500 °F) because the 

threads of the cyclone components may gall 

or seize, thus preventing the recovery of the 

collected PM and rendering the cyclone 

unusable for subsequent use. You may use 

stainless steel cyclone assemblies 

constructed with bolt-together rather than 

screw-together assemblies at temperatures up 

to 538 °C (1,000 °F). You must use ‘‘breakaway’’ or expendable stainless steel bolts that 

can be over-torqued and broken if necessary 

to release cyclone closures, thus allowing 

you to recover PM without damaging the 

cyclone flanges or contaminating the 

samples. You may need to use specialty 

metals to achieve reliable particulate mass 

measurements above 538 °C (1,000 °F). The 

method can be used at temperatures up to 

1,371 °C (2,500 °F) using specially 

constructed high-temperature stainless steel 

alloys (Hastelloy or Haynes 230) with bolttogether closures using break-away bolts. 

8.6.2 Filterable Particulate Filter Holder 

and Pitot Tube. Attach the pre-selected filter 

holder to the end of the combined cyclone 

sampling head (see Figure 2 of Section 17). 

Attach the S-type pitot tube to the combined 

cyclones after the sampling head is fully 

attached to the end of the probe. (Note: The 

pitot tube tip must be mounted slightly 

beyond the combined head cyclone sampling 

assembly and at least one inch off the gas 

flow path into the cyclone nozzle. This is 

similar to the pitot tube placement in Method 

17 of appendix A–6 to part 60.) Securely 

fasten the sensing lines to the outside of the 

probe to ensure proper alignment of the pitot 

tube. Provide unions on the sensing lines so 

that you can connect and disconnect the 

S-type pitot tube tips from the combined 

cyclone sampling head before and after each 

run. Calibrate the pitot tube on the sampling 

head according to the most current ASTM 

International D3796 because the cyclone 

body is a potential source flow disturbance 

and will change the pitot coefficient value 

from the baseline (isolated tube) value. 

8.6.3 Filter. You must number and tare 

the filters before use. To tare the filters, 

desiccate each filter at 20 ± 5.6 °C (68 ± 

10 °F) and ambient pressure for at least 24 

hours and weigh at intervals of at least six 

hours to a constant weight. (See Section 3.0 

for a definition of constant weight.) Record 

results to the nearest 0.1 mg. During each 

weighing, the filter must not be exposed to 

the laboratory atmosphere for longer than 

two minutes and a relative humidity above 

50 percent. Alternatively, the filters may be 

oven-dried at 104 °C (220 °F) for two to three 

hours, desiccated for two hours, and 

weighed. Use tweezers or clean disposable 

surgical gloves to place a labeled (identified) 

and pre-weighed filter in the filter holder. 

You must center the filter and properly place 

the gasket so that the sample gas stream will 

not circumvent the filter. The filter must not 

be compressed between the gasket and the 

filter housing. Check the filter for tears after 

the assembly is completed. Then screw or 

clamp the filter housing together to prevent 

the seal from leaking. 

8.6.4 Moisture Trap. If you are measuring 

only filterable particulate (or you are sure 

that the gas filtration temperature will be 

maintained below 30 °C (85 °F)), then an 

empty modified Greenburg Smith impinger 

followed by an impinger containing silica gel 

is required. Alternatives described in Method 

5 of appendix A–3 to part 60 may also be 

used to collect moisture that passes through 

the ambient filter. If you are measuring 

condensable PM in combination with this 

method, then follow the procedures in 

Method 202 of appendix M of this part for 

moisture collection. 

8.6.5 Leak Check. Use the procedures 

outlined in Section 8.4 of Method 5 of 

appendix A–3 to part 60 to leak check the 

entire sampling system. Specifically perform 

the following procedures: 

8.6.5.1 Sampling train. You must pretest 

the entire sampling train for leaks. The 

pretest leak check must have a leak rate of 

not more than 0.02 actual cubic feet per 

minute or four percent of the average sample 

flow during the test run, whichever is less. 

Additionally, you must conduct the leak 

check at a vacuum equal to or greater than 

the vacuum anticipated during the test run. 

Enter the leak check results on the analytical 

data sheet (see Section 11.1) for the specific 

test. (Note: Do not conduct a leak check 

during port changes.) 

8.6.5.2 Pitot tube assembly. After you 

leak check the sample train, perform a leak 

check of the pitot tube assembly. Follow the 

procedures outlined in Section 8.4.1 of 

Method 5 of appendix A–3 to part 60. 

8.6.6 Sampling Head. You must preheat 

the combined sampling head to the stack 

temperature of the gas stream at the test 

location (± 10 °C, ± 50 °F). This will heat the 

sampling head and prevent moisture from 

condensing from the sample gas stream. 

8.6.6.1 Warmup. You must complete a 

passive warmup (of 30–40 min) within the 

stack before the run begins to avoid internal 

condensation. 

8.6.6.2 Shortened warmup. You can 

shorten the warmup time by thermostated 

heating outside the stack (such as by a heat 

gun). Then place the heated sampling head 

inside the stack and allow the temperature to 

equilibrate. 

8.7 Sampling Train Operation. Operate 

the sampling train the same as described in 

Section 4.1.5 of Method 5 of appendix A–3 

to part 60, but use the procedures in this 

section for isokinetic sampling and flow rate 

adjustment. Maintain the flow rate calculated 

in Section 8.4.1 throughout the run, provided 

the stack temperature is within 28 °C (50 °F) 

of the temperature used to calculate DH. If 

stack temperatures vary by more than 28 °C 

(50 °F), use the appropriate DH value 

calculated in Section 8.5.3. Determine the 

minimum number of traverse points as in 

Figure 7 of Section 17. Determine the 

minimum total projected sampling time 

based on achieving the data quality 

objectives or emission limit of the affected 

facility. We recommend that you round the 

number of minutes sampled at each point to 

the nearest 15 seconds. Perform the following 

procedures: 

8.7.1 Sample Point Dwell Time. You 

must calculate the flow rate-weighted dwell 

time (that is, sampling time) for each 

sampling point to ensure that the overall run 

provides a velocity-weighted average that is 

representative of the entire gas stream. Vary 

the dwell time at each traverse point 

proportionately with the point velocity. 

Calculate the dwell time at each of the 

traverse points using Equation 24. You must 

use the data from the preliminary traverse to 

determine the average velocity pressure 

(Dpavg). You must use the velocity pressure 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80139 

measured during the sampling run to 

determine the velocity pressure at each point 

(Dpn). Here, Ntp equals the total number of 

traverse points. Each traverse point must 

have a dwell time of at least two minutes. 

8.7.2 Adjusted Velocity Pressure. When 

selecting your sampling points using your 

preliminary velocity traverse data, your 

preliminary velocity pressures must be 

adjusted to take into account the increase in 

velocity due to blockage. Also, you must 

adjust your preliminary velocity data for 

differences in pitot tube coefficients. Use the 

following instructions to adjust the 

preliminary velocity pressure. 

8.7.2.1 Different pitot tube coefficient. 

You must use Equation 25 to correct the 

recorded preliminary velocity pressures if the 

pitot tube mounted on the combined cyclone 

sampling head has a different pitot tube 

coefficient than the pitot tube used during 

the preliminary velocity traverse (see Section 

8.3.4). 

8.7.2.2 Probe blockage factor. You must 

use Equation 26 to calculate an average probe 

blockage correction factor (bf) if the diameter 

of your stack or duct is between 25.7 and 

36.4 inches for the combined PM2.5/PM10

sampling head and pitot and between 18.8 

and 26.5 inches for the PM2.5 cyclone and 

pitot. A probe blockage factor is calculated 

because of the flow blockage caused by the 

relatively large cross-sectional area of the 

cyclone sampling head, as discussed in 

Section 8.3.2.2 and illustrated in Figures 8 

and 9 of Section 17. You must determine the 

cross-sectional area of the cyclone head you 

use and determine its stack blockage factor. 

(Note: Commercially-available sampling 

heads (including the PM10 cyclone, PM2.5

cyclone, pitot and filter holder) have a 

projected area of approximately 31.2 square 

inches when oriented into the gas stream. As 

the probe is moved from the most outer to 

the most inner point, the amount of blockage 

that actually occurs ranges from 

approximately 13 square inches to the full 

31.2 inches plus the blockage caused by the 

probe extension. The average cross-sectional 

area blocked is 22 square inches.) 

8.7.2.3 Final adjusted velocity pressure. 

Calculate the final adjusted velocity pressure 

(Dps2) using Equation 27. (Note: Figures 8 and 

9 of Section 17 illustrate that the blockage 

effect of the combined PM10, PM2.5 cyclone 

sampling head, and pitot tube increases 

rapidly below stack diameters of 26.5 inches. 

Therefore, the combined PM10, PM2.5 filter 

sampling head and pitot tube is not 

applicable for stacks with a diameter less 

than 26.5 inches because the blockage is 

greater than six percent. For stacks with a 

diameter less than 26.5 inches, PM2.5

particulate measurements may be possible 

using only a PM2.5 cyclone, pitot tube, and 

in-stack filter. If the blockage exceeds three 

percent but is less than six percent, you must 

follow the procedures outlined in Method 1A 

of appendix A–1 to part 60 to conduct tests. 

You must conduct the velocity traverse 

downstream of the sampling location or 

immediately before the test run. 

8.7.3 Sample Collection. Collect samples 

the same as described in Section 4.1.5 of 

Method 5 of appendix A–3 to part 60, except 

use the procedures in this section for 

isokinetic sampling and flow rate adjustment. 

Maintain the flow rate calculated in Section 

8.5 throughout the run, provided the stack 

temperature is within 28 °C (50 °F) of the 

temperature used to calculate DH. If stack 

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

use the appropriate DH value calculated in 

Section 8.5.3. Calculate the dwell time at 

each traverse point as in Equation 24. In 

addition to these procedures, you must also 

use running starts and stops if the static 

pressure at the sampling location is less than 

minus 5 inches water column. This prevents 

back pressure from rupturing the sample 

filter. If you use a running start, adjust the 

flow rate to the calculated value after you 

perform the leak check (see Section 8.4). 

8.7.3.1 Level and zero manometers. 

Periodically check the level and zero point of 

the manometers during the traverse. 

Vibrations and temperature changes may 

cause them to drift. 

8.7.3.2 Portholes. Clean the portholes 

prior to the test run. This will minimize the 

chance of collecting deposited material in the 

nozzle. 

8.7.3.3 Sampling procedures. Verify that 

the combined cyclone sampling head 

temperature is at stack temperature. You 

must maintain the temperature of the cyclone 

sampling head within ± 10 °C (± 18 °F) of the 

stack temperature. (Note: For many stacks, 

portions of the cyclones and filter will be 

external to the stack during part of the 

sampling traverse. Therefore, you must heat 

and/or insulate portions of the cyclones and 

filter that are not within the stack in order 

to maintain the sampling head temperature at 

the stack temperature. Maintaining the 

temperature will ensure proper particle 

sizing and prevent condensation on the walls 

of the cyclones.) To begin sampling, remove 

the protective cover from the nozzle. Position 

the probe at the first sampling point with the 

nozzle pointing directly into the gas stream. 

Immediately start the pump and adjust the 

flow to calculated isokinetic conditions. 

Ensure the probe/pitot tube assembly is 

leveled. (Note: When the probe is in position, 

block off the openings around the probe and 

porthole to prevent unrepresentative dilution 

of the gas stream. Take care to minimize 

contamination from material used to block 

the flow or insulate the sampling head during 

collection at the first sampling point.) 

(a) Traverse the stack cross-section, as 

required by Method 1 of appendix A–1 to 

part 60, with the exception that you are only 

required to perform a 12-point traverse. Do 

not bump the cyclone nozzle into the stack 

walls when sampling near the walls or when 

removing or inserting the probe through the 

portholes. This will minimize the chance of 

extracting deposited materials. 

(b) Record the data required on the field 

test data sheet for each run. Record the initial 

dry gas meter reading. Then take dry gas 

meter readings at the following times: the 

beginning and end of each sample time 

increment; when changes in flow rates are 

made; and when sampling is halted. Compare 

the velocity pressure measurements 

(Equations 22 and 23) with the velocity 

pressure measured during the preliminary 

traverse. Keep the meter box DH at the value 

calculated in Section 8.5.3 for the stack 

temperature that is observed during the test. 

Record all point-by-point data and other 

source test parameters on the field test data 

sheet. Do not leak check the sampling system 

during port changes. 

(c) Maintain flow until the sampling head 

is completely removed from the sampling 

port. You must restart the sampling flow 

prior to inserting the sampling head into the 

sampling port during port changes. 

(d) Maintain the flow through the sampling 

system at the last sampling point. At the 

conclusion of the test, remove the pitot tube 

and combined cyclone sampling head from 

the stack while the train is still operating 

(running stop). Make sure that you do not 

scrape the pitot tube or the combined cyclone 

sampling head against the port or stack walls. 

Then stop the pump and record the final dry 

gas meter reading and other test parameters 

on the field test data sheet. (Note: After you 

stop the pump, make sure you keep the 

combined cyclone head level to avoid tipping 

dust from the cyclone cups into the filter 

and/or down-comer lines.) 

8.7.4 Process Data. You must document 

data and information on the process unit 

tested, the particulate control system used to 

control emissions, any non-particulate 

control system that may affect particulate 

emissions, the sampling train conditions, and 

weather conditions. Record the site 

barometric pressure and stack pressure on 

the field test data sheet. Discontinue the test 

if the operating conditions may cause nonrepresentative particulate emissions. 

8.7.4.1 Particulate control system data. 

Use the process and control system data to 

determine whether representative operating 

conditions were maintained throughout the 

testing period. 

8.7.4.2 Sampling train data. Use the 

sampling train data to confirm that the 

measured particulate emissions are accurate 

and complete. 

8.7.5 Sample Recovery. First remove the 

sampling head (combined cyclone/filter 

assembly) from the train probe. After the 

sample head is removed, perform a post-test 

leak check of the probe and sample train. 

Then recover the components from the 

cyclone/filter. Refer to the following sections 

for more detailed information. 

8.7.5.1 Remove sampling head. After 

cooling and when the probe can be safely 

handled, wipe off all external surfaces near 

the cyclone nozzle and cap the inlet to the 

cyclone to prevent PM from entering the 

assembly. Remove the combined cyclone/ 

filter sampling head from the probe. Cap the 

outlet of the filter housing to prevent PM 

from entering the assembly. 

8.7.5.2 Leak check probe/sample train 

assembly (post-test). Leak check the 

remainder of the probe and sample train 

assembly (including meter box) after 

removing the combined cyclone head/filter. 

You must conduct the leak rate at a vacuum 

equal to or greater than the maximum 

vacuum achieved during the test run. Enter 

the results of the leak check onto the field 

test data sheet. If the leak rate of the sampling 

train (without the combined cyclone 

sampling head) exceeds 0.02 actual cubic feet 

per minute or four percent of the average 

sampling rate during the test run (whichever 


jlentini on DSKJ8SOYB1PROD with RULES2
80140 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

is less), the run is invalid and must be 

repeated. 

8.7.5.3 Weigh or measure the volume of 

the liquid collected in the water collection 

impingers and silica trap. Measure the liquid 

in the first impingers to within 1 ml using a 

clean graduated cylinder or by weighing it to 

within 0.5 g using a balance. Record the 

volume of the liquid or weight of the liquid 

present to be used to calculate the moisture 

content of the effluent gas. 

8.7.5.4 Weigh the silica impinger. If a 

balance is available in the field, weigh the 

silica impinger to within 0.5 g. Note the color 

of the indicating silica gel in the last 

impinger to determine whether it has been 

completely spent and make a notation of its 

condition. If you are measuring CPM in 

combination with this method, the weight of 

the silica gel can be determined before or 

after the post-test nitrogen purge is complete 

(See Section 8.5.3 of Method 202 of appendix 

M to this part). 

8.7.5.5 Recovery of PM. Recovery 

involves the quantitative transfer of particles 

in the following size range: greater than 10 

micrometers; less than or equal to 10 

micrometers but greater than 2.5 

micrometers; and less than or equal to 2.5 

micrometers. You must use a nylon or 

fluoropolymer brush and an acetone rinse to 

recover particles from the combined cyclone/ 

filter sampling head. Use the following 

procedures for each container: 

(a) Container #1, Less than or equal to 

PM2.5 micrometer filterable particulate. Use 

tweezers and/or clean disposable surgical 

gloves to remove the filter from the filter 

holder. Place the filter in the Petri dish that 

you labeled with the test identification and 

Container #1. Using a dry brush and/or a 

sharp-edged blade, carefully transfer any PM 

and/or filter fibers that adhere to the filter 

holder gasket or filter support screen to the 

Petri dish. Seal the container. This container 

holds particles less than or equal to 2.5 

micrometers that are caught on the in-stack 

filter. (Note: If the test is conducted for PM10

only, then Container #1 would be for less 

than or equal to PM2.5 micrometer filterable 

particulate.) 

(b) Container #2, Greater than PM10

micrometer filterable particulate. 

Quantitatively recover the PM from the 

cyclone I cup and brush cleaning and acetone 

rinses of the cyclone cup, internal surface of 

the nozzle, and cyclone I internal surfaces, 

including the outside surface of the 

downcomer line. Seal the container and mark 

the liquid level on the outside of the 

container you labeled with test identification 

and Container #2. You must keep any dust 

found on the outside of cyclone I and cyclone 

nozzle external surfaces out of the sample. 

This container holds PM greater than 10 

micrometers. 

(c) Container #3, Filterable particulate less 

than or equal to 10 micrometer and greater 

than 2.5 micrometers. Place the solids from 

cyclone cup IV and the acetone (and brush 

cleaning) rinses of the cyclone I turnaround 

cup (above inner downcomer line), inside of 

the downcomer line, and interior surfaces of 

cyclone IV into Container #3. Seal the 

container and mark the liquid level on the 

outside of the container you labeled with test 

identification and Container #3. This 

container holds PM less than or equal to 10 

micrometers but greater than 2.5 

micrometers. 

(d) Container #4, Less than or equal to 

PM2.5 micrometers acetone rinses of the exit 

tube of cyclone IV and front half of the filter 

holder. Place the acetone rinses (and brush 

cleaning) of the exit tube of cyclone IV and 

the front half of the filter holder in container 

#4. Seal the container and mark the liquid 

level on the outside of the container you 

labeled with test identification and Container 

#4. This container holds PM that is less than 

or equal to 2.5 micrometers. 

(e) Container #5, Cold impinger water. If 

the water from the cold impinger used for 

moisture collection has been weighed in the 

field, it can be discarded. Otherwise, 

quantitatively transfer liquid from the cold 

impinger that follows the ambient filter into 

a clean sample bottle (glass or plastic). Mark 

the liquid level on the bottle you labeled 

with test identification and Container #5. 

This container holds the remainder of the 

liquid water from the emission gases. If you 

collected condensable PM using Method 202 

of appendix M to this part in conjunction 

with using this method, you must follow the 

procedures in Method 202 of appendix M to 

this part to recover impingers and silica used 

to collect moisture. 

(f) Container #6, Silica gel absorbent. 

Transfer the silica gel to its original container 

labeled with test identification and Container 

#6 and seal. A funnel may make it easier to 

pour the silica gel without spilling. A rubber 

policeman may be used as an aid in removing 

the silica gel from the impinger. It is not 

necessary to remove the small amount of 

silica gel dust particles that may adhere to 

the impinger wall and are difficult to remove. 

Since the gain in weight is to be used for 

moisture calculations, do not use any water 

or other liquids to transfer the silica gel. If 

the silica gel has been weighed in the field 

to measure water content, it can be 

discarded. Otherwise, the contents of 

Container #6 are weighed during sample 

analysis. 

(g) Container #7, Acetone field reagent 

blank. Take approximately 200 ml of the 

acetone directly from the wash bottle you 

used and place it in Container #7 labeled 

‘‘Acetone Field Reagent Blank.’’ 

8.7.6 Transport Procedures. Containers 

must remain in an upright position at all 

times during shipping. You do not have to 

ship the containers under dry or blue ice. 

9.0 Quality Control 

9.1 Daily Quality Checks. You must 

perform daily quality checks of field log 

books and data entries and calculations using 

data quality indicators from this method and 

your site-specific test plan. You must review 

and evaluate recorded and transferred raw 

data, calculations, and documentation of 

testing procedures. You must initial or sign 

log book pages and data entry forms that 

were reviewed. 

9.2 Calculation Verification. Verify the 

calculations by independent, manual checks. 

You must flag any suspect data and identify 

the nature of the problem and potential effect 

on data quality. After you complete the test, 

prepare a data summary and compile all the 

calculations and raw data sheets. 

9.3 Conditions. You must document data 

and information on the process unit tested, 

the particulate control system used to control 

emissions, any non-particulate control 

system that may affect particulate emissions, 

the sampling train conditions, and weather 

conditions. Discontinue the test if the 

operating conditions may cause nonrepresentative particulate emissions. 

9.4 Field Analytical Balance Calibration 

Check. Perform calibration check procedures 

on field analytical balances each day that 

they are used. You must use National 

Institute of Standards and Technology 

(NIST)-traceable weights at a mass 

approximately equal to the weight of the 

sample plus container you will weigh. 

10.0 Calibration and Standardization 

Maintain a log of all filterable particulate 

sampling and analysis calibrations. Include 

copies of the relevant portions of the 

calibration and field logs in the final test 

report. 

10.1 Gas Flow Velocities. You must use 

an S-type pitot tube that meets the required 

EPA specifications (EPA Publication 600/4– 

77–0217b) during these velocity 

measurements. (Note: If, as specified in 

Section 8.7.2.3, testing is performed in stacks 

less than 26.5 inches in diameter, testers may 

use a standard pitot tube according to the 

requirements in Method 4A or 5 of appendix 

A–3 to part 60.) You must also complete the 

following: 

(a) Visually inspect the S-type pitot tube 

before sampling. 

(b) Leak check both legs of the pitot tube 

before and after sampling. 

(c) Maintain proper orientation of the Stype pitot tube while making measurements. 

10.1.1 S-type Pitot Tube Orientation. The 

S-type pitot tube is properly oriented when 

the yaw and the pitch axis are 90 degrees to 

the air flow. 

10.1.2 Average Velocity Pressure Record. 

Instead of recording either high or low 

values, record the average velocity pressure 

at each point during flow measurements. 

10.1.3 Pitot Tube Coefficient. Determine 

the pitot tube coefficient based on physical 

measurement techniques described in 

Method 2 of appendix A–1 to part 60. (Note: 

You must calibrate the pitot tube on the 

sampling head because of potential 

interferences from the cyclone body. Refer to 

Section 8.7.2 for additional information.) 

10.2 Thermocouple Calibration. You 

must calibrate the thermocouples using the 

procedures described in Section 10.3.1 of 

Method 2 of appendix A–1 to part 60 or 

Alternative Method 2 Thermocouple 

Calibration (ALT–011). Calibrate each 

temperature sensor at a minimum of three 

points over the anticipated range of use 

against a NIST-traceable thermometer. 

Alternatively, a reference thermocouple and 

potentiometer calibrated against NIST 

standards can be used. 

10.3 Nozzles. You may use stainless steel 

(316 or equivalent), high-temperature steel 

alloy, or fluoropolymer-coated nozzles for 

isokinetic sampling. Make sure that all 

nozzles are thoroughly cleaned, visually 

inspected, and calibrated according to the 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80141 

procedure outlined in Section 10.1 of Method 

5 of appendix A–3 to part 60. 

10.4 Dry Gas Meter Calibration. Calibrate 

your dry gas meter following the calibration 

procedures in Section 16.1 of Method 5 of 

appendix A–3 to part 60. Also, make sure 

you fully calibrate the dry gas meter to 

determine the volume correction factor prior 

to field use. Post-test calibration checks must 

be performed as soon as possible after the 

equipment has been returned to the shop. 

Your pre-test and post-test calibrations must 

agree within ± 5 percent. 

10.5 Glassware. Use class A volumetric 

glassware for titrations, or calibrate your 

equipment against NIST-traceable glassware. 

11.0 Analytical Procedures 

11.1 Analytical Data Sheet. Record all 

data on the analytical data sheet. Obtain the 

data sheet from Figure 5–6 of Method 5 of 

appendix A–3 to part 60. Alternatively, data 

may be recorded electronically using 

software applications such as the Electronic 

Reporting Tool located at http:// 

www.epa.gov/ttn/chief/ert/ert_tool.html. 

11.2 Dry Weight of PM. Determine the 

dry weight of particulate following 

procedures outlined in this section. 

11.2.1 Container #1, Less than or Equal to 

PM2.5 Micrometer Filterable Particulate. 

Transfer the filter and any loose particulate 

from the sample container to a tared 

weighing dish or pan that is inert to solvent 

or mineral acids. Desiccate for 24 hours in a 

dessicator containing anhydrous calcium 

sulfate. Weigh to a constant weight and 

report the results to the nearest 0.1 mg. (See 

Section 3.0 for a definition of Constant 

weight.) If constant weight requirements 

cannot be met, the filter must be treated as 

described in Section 11.2.1 of Method 202 of 

appendix M to this part. Extracts resulting 

from the use of this procedure must be 

filtered to remove filter fragments before the 

filter is processed and weighed. 

11.2.2 Container #2, Greater than PM10

Micrometer Filterable Particulate Acetone 

Rinse. Separately treat this container like 

Container #4. 

11.2.3 Container #3, Filterable Particulate 

Less than or Equal to 10 Micrometer and 

Greater than 2.5 Micrometers Acetone Rinse. 

Separately treat this container like Container 

#4. 

11.2.4 Container #4, Less than or Equal to 

PM2.5 Micrometers Acetone Rinse of the Exit 

Tube of Cyclone IV and Front Half of the 

Filter Holder. Note the level of liquid in the 

container and confirm on the analysis sheet 

whether leakage occurred during transport. If 

a noticeable amount of leakage has occurred, 

either void the sample or use methods 

(subject to the approval of the Administrator) 

to correct the final results. Quantitatively 

transfer the contents to a tared 250 ml beaker 

or tared fluoropolymer beaker liner, and 

evaporate to dryness at room temperature 

and pressure in a laboratory hood. Desiccate 

for 24 hours and weigh to a constant weight. 

Report the results to the nearest 0.1 mg. 

11.2.5 Container #5, Cold Impinger 

Water. If the amount of water has not been 

determined in the field, note the level of 

liquid in the container and confirm on the 

analysis sheet whether leakage occurred 

during transport. If a noticeable amount of 

leakage has occurred, either void the sample 

or use methods (subject to the approval of the 

Administrator) to correct the final results. 

Measure the liquid in this container either 

volumetrically to ± 1 ml or gravimetrically to 

± 0.5 g. 

11.2.6 Container #6, Silica Gel Absorbent. 

Weigh the spent silica gel (or silica gel plus 

impinger) to the nearest 0.5 g using a balance. 

This step may be conducted in the field. 

11.2.7 Container #7, Acetone Field 

Reagent Blank. Use 150 ml of acetone from 

the blank container used for this analysis. 

Transfer 150 ml of the acetone to a clean 250- 

ml beaker or tared fluoropolymer beaker 

liner. Evaporate the acetone to dryness at 

room temperature and pressure in a 

laboratory hood. Following evaporation, 

desiccate the residue for 24 hours in a 

desiccator containing anhydrous calcium 

sulfate. Weigh and report the results to the 

nearest 0.1 mg. 

12.0 Calculations and Data Analysis 

12.1 Nomenclature. Report results in 

International System of Units (SI units) 

unless the regulatory authority that 

established the requirement to use this test 

method specifies reporting in English units. 

The following nomenclature is used. 

A = Area of stack or duct at sampling 

location, square inches. 

An = Area of nozzle, square feet. 

bf = Average blockage factor calculated in 

Equation 26, dimensionless. 

Bws = Moisture content of gas stream, fraction 

(e.g., 10 percent H2O is Bws = 0.10). 

C = Cunningham correction factor for particle 

diameter, Dp, and calculated using the 

actual stack gas temperature, 

dimensionless. 

%CO2 = Carbon Dioxide content of gas 

stream, percent by volume. 

Ca = Acetone blank concentration, mg/mg. 

CfPM10 = Conc. of filterable PM10, gr/DSCF. 

CfPM2.5 = Conc. of filterable PM2.5, gr/DSCF. 

Cp = Pitot coefficient for the combined 

cyclone pitot, dimensionless. 

Cp′ = Coefficient for the pitot used in the 

preliminary traverse, dimensionless. 

Cr = Re-estimated Cunningham correction 

factor for particle diameter equivalent to 

the actual cut size diameter and 

calculated using the actual stack gas 

temperature, dimensionless. 

Ctf = Conc. of total filterable PM, gr/DSCF. 

C1 = -150.3162 (micropoise) 

C2 = 18.0614 (micropoise/K0.5) = 13.4622 

(micropoise/R0.5) 

C3 = 1.19183 × 106 (micropoise/K2) = 3.86153 

× 106 (micropoise/R2) 

C4 = 0.591123 (micropoise) 

C5 = 91.9723 (micropoise) 

C6 = 4.91705 × 10¥5 (micropoise/K2) = 

1.51761 × 10¥5 (micropoise/R2) 

D = Inner diameter of sampling nozzle 

mounted on Cyclone I, inches. 

Dp = Physical particle size, micrometers. 

D50 = Particle cut diameter, micrometers. 

D50–1 = Re-calculated particle cut diameters 

based on re-estimated Cr, micrometers. 

D50LL = Cut diameter for cyclone I 

corresponding to the 2.25 micrometer cut 

diameter for cyclone IV, micrometers. 

D50N = D50 value for cyclone IV calculated 

during the Nth iterative step, 

micrometers. 

D50(N∂1) = D50 value for cyclone IV calculated 

during the N+1 iterative step, 

micrometers. 

D50T = Cyclone I cut diameter corresponding 

to the middle of the overlap zone shown 

in Figure 10 of Section 17, micrometers. 

I = Percent isokinetic sampling, 

dimensionless. 

Kp = 85.49, ((ft/sec)/(pounds/mole -°R)). 

ma = Mass of residue of acetone after 

evaporation, mg. 

Md = Molecular weight of dry gas, pounds/ 

pound mole. 

mg = Milligram. 

mg/L = Milligram per liter. 

Mw = Molecular weight of wet gas, pounds/ 

pound mole. 

M1 = Milligrams of PM collected on the filter, 

less than or equal to 2.5 micrometers. 

M2 = Milligrams of PM recovered from 

Container #2 (acetone blank corrected), 

greater than 10 micrometers. 

M3 = Milligrams of PM recovered from 

Container #3 (acetone blank corrected), 

less than or equal to 10 and greater than 

2.5 micrometers. 

M4 = Milligrams of PM recovered from 

Container #4 (acetone blank corrected), 

less than or equal to 2.5 micrometers. 

Ntp = Number of iterative steps or total 

traverse points. 

Nre = Reynolds number, dimensionless. 

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

by volume of wet gas. 

(Note: The oxygen percentage used in 

Equation 3 is on a wet gas basis. That 

means that since oxygen is typically 

measured on a dry gas basis, the 

measured percent O2 must be multiplied 

by the quantity (1–Bws) to convert to the 

actual volume fraction. Therefore, 

%O2,wet = (1–Bws) * %O2, dry) 

Pbar = Barometric pressure, inches Hg. 

Ps = Absolute stack gas pressure, inches Hg. 

Qs = Sampling rate for cyclone I to achieve 

specified D50. 

QsST = Dry gas sampling rate through the 

sampling assembly, DSCFM. 

QI = Sampling rate for cyclone I to achieve 

specified D50. 

Rmax = Nozzle/stack velocity ratio parameter, 

dimensionless. 

Rmin = Nozzle/stack velocity ratio parameter, 

dimensionless. 

Tm = Meter box and orifice gas temperature, 

°R. 

tn = Sampling time at point n, min. 

tr = Total projected run time, min. 

Ts = Absolute stack gas temperature, °R. 

t1 = Sampling time at point 1, min. 

vmax = Maximum gas velocity calculated from 

Equations 18 or 19, ft/sec. 

vmin = Minimum gas velocity calculated from 

Equations 16 or 17, ft/sec. 

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

vs = Velocity of stack gas, ft/sec. 

Va = Volume of acetone blank, ml. 

Vaw = Volume of acetone used in sample 

recovery wash, ml. 

Vc = Quantity of water captured in impingers 

and silica gel, ml. 

Vm = Dry gas meter volume sampled, ACF. 

Vms = Dry gas meter volume sampled, 

corrected to standard conditions, DSCF. 


jlentini on DSKJ8SOYB1PROD with RULES2
80142 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

Vws = Volume of water vapor, SCF. 

Vb = Volume of aliquot taken for IC analysis, 

ml. 

Vic = Volume of impinger contents sample, 

ml. 

Wa = Weight of blank residue in acetone used 

to recover samples, mg. 

W2,3,4 = Weight of PM recovered from 

Containers #2, #3, and #4, mg. 

Z = Ratio between estimated cyclone IV D50

values, dimensionless. 

DH = Meter box orifice pressure drop, inches 

W.C. 

DH@ = Pressure drop across orifice at flow 

rate of 0.75 SCFM at standard 

conditions, inches W.C. 

(Note: Specific to each orifice and meter box.) 

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

velocity pressures measured during the 

preliminary traverse, inches W.C. 

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

inches W.C. 

Dpavg = Average velocity pressure, inches 

W.C. 

Dpmax = Maximum velocity pressure, inches 

W.C. 

Dpmin = Minimum velocity pressure, inches 

W.C. 

Dpn = Velocity pressure measured at point n 

during the test run, inches W.C. 

Dps = Velocity pressure calculated in 

Equation 25, inches W.C. 

Dps1 = Velocity pressure adjusted for 

combined cyclone pitot tube, inches 

W.C. 

Dps2 = Velocity pressure corrected for 

blockage, inches W.C. 

Dp1 = Velocity pressure measured at point 1, 

inches W.C. 

g = Dry gas meter gamma value, 

dimensionless. 

μ = Gas viscosity, micropoise. 

q = Total run time, min. 

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

bottle). 

12.0 = Constant calculated as 60 percent of 

20.5 square inch cross-sectional area of 

combined cyclone head, square inches. 

12.2 Calculations. Perform all of the 

calculations found in Table 6 of Section 17. 

Table 6 of Section 17 also provides 

instructions and references for the 

calculations. 

12.3 Analyses. Analyze D50 of cyclone IV 

and the concentrations of the PM in the 

various size ranges. 

12.3.1 D50 of Cyclone IV. To determine 

the actual D50 for cyclone IV, recalculate the 

Cunningham correction factor and the 

Reynolds number for the best estimate of 

cyclone IV D50. The following sections 

describe additional information on how to 

recalculate the Cunningham correction factor 

and determine which Reynolds number to 

use. 

12.3.1.1 Cunningham correction factor. 

Recalculate the initial estimate of the 

Cunningham correction factor using the 

actual test data. Insert the actual test run data 

and D50 of 2.5 micrometers into Equation 4. 

This will give you a new Cunningham 

correction factor based on actual data. 

12.3.1.2 Initial D50 for cyclone IV. 

Determine the initial estimate for cyclone IV 

D50 using the test condition Reynolds number 

calculated with Equation 10 as indicated in 

Table 3 of Section 17. Refer to the following 

instructions. 

(a) If the Reynolds number is less than 

3,162, calculate the D50 for cyclone IV with 

Equation 34, using actual test data. 

(b) If the Reynolds number is greater than 

or equal to 3,162, calculate the D50 for 

cyclone IV with Equation 35 using actual test 

data. 

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

either Equation 34 or 35 into Equation 36 to 

re-establish the Cunningham Correction 

Factor (Cr). (Note: Use the test condition 

calculated Reynolds number to determine the 

most appropriate equation (Equation 34 or 

35).) 

12.3.1.3 Re-establish cyclone IV D50. Use 

the re-established Cunningham correction 

factor (calculated in the previous step) and 

the calculated Reynolds number to determine 

D50–1. 

(a) Use Equation 37 to calculate the reestablished cyclone IV D50–1 if the Reynolds 

number is less than 3,162. 

(b) Use Equation 38 to calculate the reestablished cyclone IV D50–1 if the Reynolds 

number is greater than or equal to 3,162. 

12.3.1.4 Establish ‘‘Z’’ values. The ‘‘Z’’ 

value is the result of an analysis that you 

must perform to determine if the Cr is 

acceptable. Compare the calculated cyclone 

IV D50 (either Equation 34 or 35) to the reestablished cyclone IV D50–1 (either Equation 

36 or 37) values based upon the test 

condition calculated Reynolds number 

(Equation 39). Follow these procedures. 

(a) Use Equation 39 to calculate the ‘‘Z’’ 

values. If the ‘‘Z’’ value is between 0.99 and 

1.01, the D50–1 value is the best estimate of 

the cyclone IV D50 cut diameter for your test 

run. 

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

less than 0.99, re-establish a Cr based on the 

D50–1 value determined in either Equations 36 

or 37, depending upon the test condition 

Reynolds number. 

(c) Use the second revised Cr to re-calculate 

the cyclone IV D50. 

(d) Repeat this iterative process as many 

times as necessary using the prescribed 

equations until you achieve the criteria 

documented in Equation 40. 

12.3.2 Particulate Concentration. Use the 

particulate catch weights in the combined 

cyclone sampling train to calculate the 

concentration of PM in the various size 

ranges. You must correct the concentrations 

for the acetone blank. 

12.3.2.1 Acetone blank concentration. 

Use Equation 42 to calculate the acetone 

blank concentration (Ca). 

12.3.2.2 Acetone blank residue weight. 

Use Equation 44 to calculate the acetone 

blank weight (Wa (2,3,4)). Subtract the weight 

of the acetone blank from the particulate 

weight catch in each size fraction. 

12.3.2.3 Particulate weight catch per size 

fraction. Correct each of the PM weights per 

size fraction by subtracting the acetone blank 

weight (i.e., M2,3,4–Wa). (Note: Do not subtract 

a blank value of greater than 0.1 mg per 100 

ml of the acetone used from the sample 

recovery.) Use the following procedures. 

(a) Use Equation 45 to calculate the PM 

recovered from Containers #1, #2, #3, and #4. 

This is the total collectable PM (Ctf). 

(b) Use Equation 46 to determine the 

quantitative recovery of PM10 (CfPM10) from 

Containers #1, #3, and #4. 

(c) Use Equation 47 to determine the 

quantitative recovery of PM2.5 (CfPM2.5) 

recovered from Containers #1 and #4. 

12.4 Reporting. You must prepare a test 

report following the guidance in EPA 

Guidance Document 043, Preparation and 

Review of Test Reports (December 1998). 

12.5 Equations. Use the following 

equations to complete the calculations 

required in this test method. 

Molecular Weight of Dry Gas. Calculate the 

molecular weight of the dry gas using 

Equation 1. 

Molecular Weight of Wet Gas. Calculate the 

molecular weight of the stack gas on a wet 

basis using Equation 2. 

Gas Stream Viscosity. Calculate the gas 

stream viscosity using Equation 3. This 

equation uses constants for gas temperatures 

in °R. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.000</GPH> ER21DE10.001</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80143 

Cunningham Correction Factor. The 

Cunningham correction factor is calculated 

for a 2.25 micrometer diameter particle. 

Lower Limit Cut Diameter for Cyclone I for 

Nre Less than 3,162. The Cunningham 

correction factor is calculated for a 2.25 

micrometer diameter particle. 

Cut Diameter for Cyclone I for the Middle 

of the Overlap Zone. 

Sampling Rate Using Both PM10 and PM2.5

Cyclones. 

Sampling Rate Using Only PM2.5 Cyclone. For Nre Less than 3,162: 

For Nre greater than or equal to 3,162: 

Reynolds Number. 

Meter Box Orifice Pressure Drop. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.002</GPH> ER21DE10.003</GPH> ER21DE10.004</GPH> ER21DE10.005</GPH> ER21DE10.006</GPH> ER21DE10.007</GPH> ER21DE10.008</GPH> ER21DE10.009</GPH>
80144 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

Lower Limit Cut Diameter for Cyclone I for 

Nre Greater than or Equal to 3,162. The 

Cunningham correction factor is calculated 

for a 2.25 micrometer diameter particle. 

Velocity of Stack Gas. Correct the mean 

preliminary velocity pressure for Cp and 

blockage using Equations 25, 26, and 27. 

Calculated Nozzle Diameter for Acceptable 

Sampling Rate. 

Velocity of Gas in Nozzle. 

Minimum Nozzle/Stack Velocity Ratio 

Parameter. 

Maximum Nozzle/Stack Velocity Ratio 

Parameter. 

Minimum Gas Velocity for Rmin Less than 

0.5. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.010</GPH> ER21DE10.011</GPH> ER21DE10.012</GPH> ER21DE10.013</GPH> ER21DE10.014</GPH> ER21DE10.015</GPH> ER21DE10.016</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80145 

Minimum Gas Velocity for Rmin Greater 

than or Equal to 0.5. 

Maximum Gas Velocity for Rmax Less than 

to 1.5. 

Maximum Gas Velocity for Rmax Greater 

than or Equal to 1.5. 

Minimum Velocity Pressure. 

Maximum Velocity Pressure. 

Sampling Dwell Time at Each Point. Ntp is 

the total number of traverse points. You must 

use the preliminary velocity traverse data. 

Adjusted Velocity Pressure. 

Average Probe Blockage Factor. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.017</GPH> ER21DE10.018</GPH> ER21DE10.019</GPH> ER21DE10.020</GPH> ER21DE10.021</GPH> ER21DE10.022</GPH> ER21DE10.023</GPH> ER21DE10.024</GPH> ER21DE10.025</GPH>
80146 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

Velocity Pressure. 

Dry Gas Volume Sampled at Standard 

Conditions. 

Sample Flow Rate at Standard Conditions. 

Volume of Water Vapor. 

Moisture Content of Gas Stream. 

Sampling Rate. 

(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. 

Particle Cut Diameter for Nre Less than 

3,162 for Cyclone IV. C must be recalculated 

using the actual test data and a D50 for 2.5 

micrometer diameter particle size. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.026</GPH> ER21DE10.027</GPH> ER21DE10.028</GPH> ER21DE10.029</GPH> ER21DE10.030</GPH> ER21DE10.031</GPH> ER21DE10.032</GPH> ER21DE10.033</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80147 

Particle Cut Diameter for Nre Greater than 

or Equal to 3,162 for Cyclone IV. C must be 

recalculated using the actual test run data 

and a D50 for 2.5 micrometer diameter 

particle size. 

Re-estimated Cunningham Correction 

Factor. You must use the actual test run 

Reynolds Number (Nre) value and select the 

appropriate D50 from Equation 33 or 34 (or 

Equation 37 or 38 if reiterating). 

Re-calculated Particle Cut Diameter for Nre

Less than 3,162. 

Re-calculated Particle Cut Diameter for N 

Greater than or Equal to 3,162. 

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

Acceptance Criteria for Z Values. The 

number of iterative steps is represented by N. 

Percent Isokinetic Sampling. 

Acetone Blank Concentration. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.034</GPH> ER21DE10.035</GPH> ER21DE10.036</GPH> ER21DE10.037</GPH> ER21DE10.038</GPH> ER21DE10.039</GPH> ER21DE10.040</GPH> ER21DE10.041</GPH>
80148 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

Acetone Blank Correction Weight. 

Acetone Blank Weight. 

Concentration of Total Filterable PM. 

Concentration of Filterable PM10.

Concentration of Filterable PM2.5.

13.0 Method Performance 

13.1 Field evaluation of PM10 and total 

PM showed that the precision of constant 

sampling rate method was the same 

magnitude as Method 17 of appendix A–6 to 

part 60 (approximately five percent). 

Precision in PM10 and total PM between 

multiple trains showed standard deviations 

of four to five percent and total mass 

compared to 4.7 percent observed for Method 

17 in simultaneous test runs at a Portland 

cement clinker cooler exhaust. The accuracy 

of the constant sampling rate PM10 method 

for total mass, referenced to Method 17, was 

¥2 ± 4.4 percent (Farthing, 1988a). 

13.2 Laboratory evaluation and guidance 

for PM10 cyclones were designed to limit 

error due to spatial variations to 10 percent. 

The maximum allowable error due to an 

isokinetic sampling was limited to ± 20 

percent for 10 micrometer particles in 

laboratory tests (Farthing, 1988b). 

13.3 A field evaluation of the revised 

Method 201A by EPA showed that the 

detection limit was 2.54 mg for total filterable 

PM, 1.44 mg for filterable PM10, and 1.35 mg 

for PM2.5. The precision resulting from 10 

quadruplicate tests (40 test runs) conducted 

for the field evaluation was 6.7 percent 

relative standard deviation. The field 

evaluation also showed that the blank 

expected from Method 201A was less than 

0.9 mg (EPA, 2010). 

14.0 Alternative Procedures 

Alternative methods for estimating the 

moisture content (ALT–008) and 

thermocouple calibration (ALT–011) can be 

found at http://www.epa.gov/ttn/emc/ 

approalt.html. 

15.0 Waste Management 

[Reserved] 

16.0 References 

(1) Dawes, S.S., and W.E. Farthing. 1990. 

‘‘Application Guide for Measurement of PM2.5

at Stationary Sources,’’ U.S. Environmental 

Protection Agency, Atmospheric Research 

and Exposure Assessment Laboratory, 

Research Triangle Park, NC, 27511, EPA– 

600/3–90/057 (NTIS No.: PB 90–247198). 

(2) Farthing, et al. 1988a. ‘‘PM10 Source 

Measurement Methodology: Field Studies,’’ 

EPA 600/3–88/055, NTIS PB89–194278/AS, 

U.S. Environmental Protection Agency, 

Research Triangle Park, NC 27711. 

(3) Farthing, W.E., and S.S. Dawes. 1988b. 

‘‘Application Guide for Source PM10

Measurement with Constant Sampling Rate,’’ 

EPA/600/3–88–057, U.S. Environmental 

Protection Agency, Research Triangle Park, 

NC 27711. 

(4) Richards, J.R. 1996. ‘‘Test protocol: PCA 

PM10/PM2.5 Emission Factor Chemical 

Characterization Testing,’’ PCA R&D Serial 

No. 2081, Portland Cement Association. 

(5) U.S. Environmental Protection Agency, 

Federal Reference Methods 1 through 5 and 

Method 17, 40 CFR part 60, Appendix A–1 

through A–3 and A–6. 

(6) U.S. Environmental Protection Agency. 

2010. ‘‘Field Evaluation of an Improved 

Method for Sampling and Analysis of 

Filterable and Condensable Particulate 

Matter.’’ Office of Air Quality Planning and 

Standards, Sector Policy and Program 

Division Monitoring Policy Group. Research 

Triangle Park, NC 27711. 

17.0 Tables, Diagrams, Flowcharts, and 

Validation Data 

You must use the following tables, 

diagrams, flowcharts, and data to complete 

this test method successfully. 

TABLE 1—TYPICAL PM CONCENTRATIONS

Particle size range Concentration and % by weight 

Total collectable particulate .............................................................................................................................. 0.015 gr/DSCF. 

Less than or equal to 10 and greater than 2.5 micrometers ............................................................................ 40% of total collectable PM. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.042</GPH> ER21DE10.043</GPH> ER21DE10.044</GPH> ER21DE10.045</GPH> ER21DE10.046</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80149 

TABLE 1—TYPICAL PM CONCENTRATIONS—Continued 

Particle size range Concentration and % by weight 

≤ 2.5 micrometers ............................................................................................................................................. 20% of total collectable PM. 

TABLE 2—REQUIRED CYCLONE CUT DIAMETERS (D50) 

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—TEST 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 less than 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. 

D50 for PM2.5 cyclone and Nre less than 3,162 ......................... Final sampling rate for cyclone IV, QIV .................................... Equation 8. 

D50 for PM2.5 cyclone and Nre greater than or equal to 3,162 Final sampling rate for cyclone IV, QIV .................................... Equation 9. 

QI(Qs) from Equation 7 .............................................................. Verify the assumed Reynolds number, Nre ............................. Equation 10. 

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

estimate moisture content of sources with gas temperature less than 160 °F. 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 11. 

TABLE 4—DH VALUES BASED ON PRELIMINARY TRAVERSE DATA

Stack Temperature (°R) Ts—50° Ts Ts + 50° 

DH, (inches W.C.) a a a 

aThese values are to be filled in by the stack tester. 

TABLE 5—VERIFICATION OF THE ASSUMED REYNOLDS NUMBER

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

Less than 3,162 ....................................................................................... Calculate DH for the meter box ..... Assume original D50LL is correct 

Greater than or equal to 3,162 ............................................................... Recalculate D50LL using Equation 

12.

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 28 to correct the sample volume measured by the dry 

gas meter to standard conditions (20 °C, 760 mm Hg or 68 °F, 29.92 

inches Hg). 

Dry gas sampling rate (QsST) ................................................................... Must be calculated using Equation 29. 

Volume of water condensed (Vws) ........................................................... Use Equation 30 to determine the water condensed in the impingers 

and silica gel combination. Determine the total moisture catch by 

measuring the change in volume or weight in the impingers and 

weighing the silica gel. 

Moisture content of gas stream (Bws) ...................................................... Calculate this using Equation 31. 

Sampling rate (Qs) .................................................................................... Calculate this using Equation 32. 

Test condition Reynolds numbera ............................................................ Use Equation 10 to calculate the actual Reynolds number during test

conditions. 


jlentini on DSKJ8SOYB1PROD with RULES2
80150 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

TABLE 6—CALCULATIONS FOR RECOVERY OF PM10 AND PM2.5—Continued 

Calculations Instructions and References 

Actual D50 of cyclone I ............................................................................. Calculate this using Equation 33. This calculation is based on the average temperatures and pressures measured during the test run. 

Stack gas velocity (vs) .............................................................................. Calculate this using Equation 13. 

Percent isokinetic rate (%I) ...................................................................... Calculate this using Equation 41. 

a Calculate the Reynolds number at the cyclone IV inlet during the test based on: (1) The sampling rate for the combined cyclone head, (2) the 

actual gas viscosity for the test, and (3) the dry and wet gas stream molecular weights. 

BILLING CODE 6560–50–P 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80151 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.047</GPH>
80152 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.048</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80153 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.049</GPH>
80154 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.050</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80155 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.051</GPH>
80156 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.052</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80157 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.053</GPH>
80158 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.054</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80159 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.055</GPH> ER21DE10.056</GPH>
80160 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

BILLING CODE 6560–50–C 

Method 202—Dry Impinger Method for 

Determining Condensable Particulate 

Emissions From Stationary Sources 

1.0 Scope and Applicability 

1.1 Scope. The U.S. Environmental 

Protection Agency (U.S. EPA or ‘‘we’’) 

developed this method to describe the 

procedures that the stack tester (‘‘you’’) must 

follow to measure condensable particulate 

matter (CPM) emissions from stationary 

sources. This method includes procedures for 

measuring both organic and inorganic CPM. 

1.2 Applicability. This method addresses 

the equipment, preparation, and analysis 

necessary to measure only CPM. You can use 

this method only for stationary source 

emission measurements. You can use this 

method to measure CPM from stationary 

source emissions after filterable particulate 

matter (PM) has been removed. CPM is 

measured in the emissions after removal from 

the stack and after passing through a filter. 

(a) If the gas filtration temperature exceeds 

30 °C (85 °F) and you must measure both the 

filterable and condensable (material that 

condenses after passing through a filter) 

components of total primary (direct) PM 

emissions to the atmosphere, then you must 

combine the procedures in this method with 

the procedures in Method 201A of appendix 

M to this part for measuring filterable PM. 

However, if the gas filtration temperature 

never exceeds 30 °C (85 °F), then use of this 

method is not required to measure total 

primary PM. 

(b) If Method 17 of appendix A–6 to part 

60 is used in conjunction with this method 

and constant weight requirements for the instack filter cannot be met, the Method 17 

filter and sampling nozzle rinse must be 

treated as described in Sections 8.5.4.4 and 

11.2.1 of this method. (See Section 3.0 for a 

definition of constant weight.) Extracts 

resulting from the use of this procedure must 

be filtered to remove filter fragments before 

the filter is processed and weighed. 

1.3 Responsibility. You are responsible 

for obtaining the equipment and supplies you 

will need to use this method. You should 

also develop your own procedures for 

following this method and any additional 

procedures to ensure accurate sampling and 

analytical measurements. 

1.4 Additional Methods. To obtain 

reliable results, you should have a thorough 

knowledge of the following test methods that 

are found in appendices A–1 through A–3 

and A–6 to part 60, and in appendix M to 

this part: 

(a) Method 1—Sample and velocity 

traverses for stationary sources. 

(b) Method 2—Determination of stack gas 

velocity and volumetric flow rate (Type S 

pitot tube). 

(c) Method 3—Gas analysis for the 

determination of dry molecular weight. 

(d) Method 4—Determination of moisture 

content in stack gases. 

(e) Method 5—Determination of particulate 

matter emissions from stationary sources. 

(f) Method 17—Determination of 

particulate matter emissions from stationary 

sources (in-stack filtration method). 

(g) Method 201A—Determination of PM10

and PM2.5 emissions from stationary sources 

(Constant sampling rate procedure). 

(h) You will need additional test methods 

to measure filterable PM. You may use 

Method 5 (including Method 5A, 5D and 5I 

but not 5B, 5E, 5F, 5G, or 5H) of appendix 

A–3 to part 60, or Method 17 of appendix 

A–6 to part 60, or Method 201A of appendix 

M to this part to collect filterable PM from 

stationary sources with temperatures above 

30 °C (85 °F) in conjunction with this 

method. However, if the gas filtration 

temperature never exceeds 30 °C (85 °F), then 

use of this method is not required to measure 

total primary PM. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.057</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80161 

1.5 Limitations. You can use this method 

to measure emissions in stacks that have 

entrained droplets only when this method is 

combined with a filterable PM test method 

that operates at high enough temperatures to 

cause water droplets sampled through the 

probe to become vaporous. 

1.6 Conditions. You must maintain 

isokinetic sampling conditions to meet the 

requirements of the filterable PM test method 

used in conjunction with this method. You 

must sample at the required number of 

sampling points specified in Method 5 of 

appendix A–3 to part 60, Method 17 of 

appendix A–6 to part 60, or Method 201A of 

appendix M to this part. Also, if you are 

using this method as an alternative to a 

required performance test method, you must 

receive approval from the regulatory 

authority that established the requirement to 

use this test method prior to conducting the 

test. 

2.0 Summary of Method 

2.1 Summary. The CPM is collected in 

dry impingers after filterable PM has been 

collected on a filter maintained as specified 

in either Method 5 of appendix A–3 to part 

60, Method 17 of appendix A–6 to part 60, 

or Method 201A of appendix M to this part. 

The organic and aqueous fractions of the 

impingers and an out-of-stack CPM filter are 

then taken to dryness and weighed. The total 

of the impinger fractions and the CPM filter 

represents the CPM. Compared to the version 

of Method 202 that was promulgated on 

December 17, 1991, this method eliminates 

the use of water as the collection media in 

impingers and includes the addition of a 

condenser followed by a water dropout 

impinger immediately after the final in-stack 

or heated filter. This method also includes 

the addition of one modified Greenburg 

Smith impinger (backup impinger) and a 

CPM filter following the water dropout 

impinger. Figure 1 of Section 18 presents the 

schematic of the sampling train configured 

with these changes. 

2.1.1 Condensable PM. CPM is collected 

in the water dropout impinger, the modified 

Greenburg Smith impinger, and the CPM 

filter of the sampling train as described in 

this method. The impinger contents are 

purged with nitrogen immediately after 

sample collection to remove dissolved sulfur 

dioxide (SO2) gases from the impinger. The 

CPM filter is extracted with water and 

hexane. The impinger solution is then 

extracted with hexane. The organic and 

aqueous fractions are dried and the residues 

are weighed. The total of the aqueous and 

organic fractions represents the CPM. 

2.1.2 Dry Impinger and Additional Filter. 

The potential artifacts from SO2 are reduced 

using a condenser and water dropout 

impinger to separate CPM from reactive 

gases. No water is added to the impingers 

prior to the start of sampling. To improve the 

collection efficiency of CPM, an additional 

filter (the ‘‘CPM filter’’) is placed between the 

second and third impingers. 

3.0 Definitions 

3.1 Condensable PM (CPM) means 

material that is vapor phase at stack 

conditions, but condenses and/or reacts upon 

cooling and dilution in the ambient air to 

form solid or liquid PM immediately after 

discharge from the stack. Note that all 

condensable PM is assumed to be in the 

PM2.5 size fraction. 

3.2 Constant weight means a difference of 

no more than 0.5 mg or one percent of total 

weight less tare weight, whichever is greater, 

between two consecutive weighings, with no 

less than six hours of desiccation time 

between weighings. 

3.3 Field Train Proof Blank. A field train 

proof blank is recovered on site from a clean, 

fully-assembled sampling train prior to 

conducting the first emissions test. 

3.4 Filterable PM means particles that are 

emitted directly by a source as a solid or 

liquid at stack or release conditions and 

captured on the filter of a stack test train. 

3.5 Primary PM (also known as direct 

PM) means particles that enter the 

atmosphere as a direct emission from a stack 

or an open source. Primary PM comprises 

two components: filterable PM and 

condensable PM. These two PM components 

have no upper particle size limit. 

3.6 Primary PM2.5 (also known as direct 

PM2.5, total PM2.5, PM2.5, or combined 

filterable PM2.5 and condensable PM) means 

PM with an aerodynamic diameter less than 

or equal to 2.5 micrometers. These solid 

particles are emitted directly from an air 

emissions source or activity, or are the 

gaseous emissions or liquid droplets from an 

air emissions source or activity that condense 

to form PM at ambient temperatures. Direct 

PM2.5 emissions include elemental carbon, 

directly emitted organic carbon, directly 

emitted sulfate, directly emitted nitrate, and 

other inorganic particles (including but not 

limited to crustal material, metals, and sea 

salt). 

3.7 Primary PM10 (also known as direct 

PM10, total PM10, PM10, or the combination 

of filterable PM10 and condensable PM) 

means PM with an aerodynamic diameter 

equal to or less than 10 micrometers. 

4.0 Interferences 

[Reserved] 

5.0 Safety 

Disclaimer. Because the performance of 

this method may require the use of hazardous 

materials, operations, and equipment, you 

should develop a health and safety plan to 

ensure the safety of your employees who are 

on site conducting the particulate emission 

test. Your plan should conform with all 

applicable Occupational Safety and Health 

Administration, Mine Safety and Health 

Administration, and Department of 

Transportation regulatory requirements. 

Because of the unique situations at some 

facilities and because some facilities may 

have more stringent requirements than is 

required by State or federal laws, you may 

have to develop procedures to conform to the 

plant health and safety requirements. 

6.0 Equipment and Supplies 

The equipment used in the filterable 

particulate portion of the sampling train is 

described in Methods 5 and 17 of appendix 

A–1 through A–3 and A–6 to part 60 and 

Method 201A of appendix M to this part. The 

equipment used in the CPM portion of the 

train is described in this section. 

6.1 Condensable Particulate Sampling 

Train Components. The sampling train for 

this method is used in addition to filterable 

particulate collection using Method 5 of 

appendix A–3 to part 60, Method 17 of 

appendix A–6 to part 60, or Method 201A of 

appendix M to this part. This method 

includes the following exceptions or 

additions: 

6.1.1 Probe Extension and Liner. The 

probe extension between the filterable 

particulate filter and the condenser must be 

glass- or fluoropolymer-lined. Follow the 

specifications for the probe liner specified in 

Section 6.1.1.2 of Method 5 of appendix A– 

3 to part 60. 

6.1.2 Condenser and Impingers. You must 

add the following components to the 

filterable particulate sampling train: A 

Method 23 type condenser as described in 

Section 2.1.2 of Method 23 of appendix A– 

8 to part 60, followed by a water dropout 

impinger or flask, followed by a modified 

Greenburg-Smith impinger (backup 

impinger) with an open tube tip as described 

in Section 6.1.1.8 of Method 5 of appendix 

A–3 to part 60. 

6.1.3 CPM Filter Holder. The modified 

Greenburg-Smith impinger is followed by a 

filter holder that is either glass, stainless steel 

(316 or equivalent), or fluoropolymer-coated 

stainless steel. Commercial size filter holders 

are available depending on project 

requirements. Use a commercial filter holder 

capable of supporting 47 mm or greater 

diameter filters. Commercial size filter 

holders contain a fluoropolymer O-ring, 

stainless steel, ceramic or fluoropolymer 

filter support and a final fluoropolymer Oring. A filter that meets the requirements 

specified in Section 7.1.1 may be placed 

behind the CPM filter to reduce the pressure 

drop across the CPM filter. This support filter 

is not part of the PM sample and is not 

recovered with the CPM filter. At the exit of 

the CPM filter, install a fluoropolymer-coated 

or stainless steel encased thermocouple that 

is in contact with the gas stream. 

6.1.4 Long Stem Impinger Insert. You will 

need a long stem modified Greenburg Smith 

impinger insert for the water dropout 

impinger to perform the nitrogen purge of the 

sampling train. 

6.2 Sample Recovery Equipment. 

6.2.1 Condensable PM Recovery. Use the 

following equipment to quantitatively 

determine the amount of CPM recovered 

from the sampling train. 

(a) Nitrogen purge line. You must use inert 

tubing and fittings capable of delivering at 

least 14 liters/min of nitrogen gas to the 

impinger train from a standard gas cylinder 

(see Figures 2 and 3 of Section 18). You may 

use standard 0.6 centimeters (1⁄4 inch) tubing 

and compression fittings in conjunction with 

an adjustable pressure regulator and needle 

valve. 

(b) Rotameter. You must use a rotameter 

capable of measuring gas flow up to 20 L/ 

min. The rotameter must be accurate to five 

percent of full scale. 

(c) Nitrogen gas purging system. 

Compressed ultra-pure nitrogen, regulator, 

and filter must be capable of providing at 


jlentini on DSKJ8SOYB1PROD with RULES2
80162 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

least 14 L/min purge gas for one hour 

through the sampling train. 

(d) Amber glass bottles (500 ml). 

6.2.2 Analysis Equipment. The following 

equipment is necessary for CPM sample 

analysis: 

(a) Separatory Funnel. Glass, 1 liter. 

(b) Weighing Tins. 50 ml. Glass 

evaporation vials, fluoropolymer beaker 

liners, or aluminum weighing tins can be 

used. 

(c) Glass Beakers. 300 to 500 ml. 

(d) Drying Equipment. A desiccator 

containing anhydrous calcium sulfate that is 

maintained below 10 percent relative 

humidity, and a hot plate or oven equipped 

with temperature control. 

(e) Glass Pipets. 5 ml. 

(f) Burette. Glass, 0 to 100 ml in 0.1 ml 

graduations. 

(g) Analytical Balance. Analytical balance 

capable of weighing at least 0.0001 g (0.1 

mg). 

(h) pH Meter or Colormetric pH Indicator. 

The pH meter or colormetric pH indicator 

(e.g., phenolphthalein) must be capable of 

determining the acidity of liquid within 0.1 

pH units. 

(i) Sonication Device. The device must 

have a minimum sonication frequency of 20 

kHz and be approximately four to six inches 

deep to accommodate the sample extractor 

tube. 

(j) Leak-Proof Sample Containers. 

Containers used for sample and blank 

recovery must not contribute more than 0.05 

mg of residual mass to the CPM 

measurements. 

(k) Wash bottles. Any container material is 

acceptable, but wash bottles used for sample 

and blank recovery must not contribute more 

than 0.1 mg of residual mass to the CPM 

measurements. 

7.0 Reagents and Standards 

7.1 Sample Collection. To collect a 

sample, you will need a CPM filter, crushed 

ice, and silica gel. You must also have water 

and nitrogen gas to purge the sampling train. 

You will find additional information on each 

of these items in the following summaries. 

7.1.1 CPM Filter. You must use a 

nonreactive, nondisintegrating polymer filter 

that does not have an organic binder and 

does not contribute more than 0.5 mg of 

residual mass to the CPM measurements. The 

CPM filter must also have an efficiency of at 

least 99.95 percent (less than 0.05 percent 

penetration) on 0.3 micrometer dioctyl 

phthalate particles. You may use test data 

from the supplier’s quality control program 

to document the CPM filter efficiency. 

7.1.2 Silica Gel. Use an indicating-type 

silica gel of six to 16 mesh. You must obtain 

approval of the Administrator for other types 

of desiccants (equivalent or better) before you 

use them. Allow the silica gel to dry for two 

hours at 175 °C (350 °F) if it is being reused. 

You do not have to dry new silica gel if the 

indicator shows the silica gel is active for 

moisture collection. 

7.1.3 Water. Use deionized, ultra-filtered 

water that contains 1.0 parts per million by 

weight (ppmw) (1 mg/L) residual mass or less 

to recover and extract samples. 

7.1.4 Crushed Ice. Obtain from the best 

readily available source. 

7.1.5 Nitrogen Gas. Use Ultra-High Purity 

compressed nitrogen or equivalent to purge 

the sampling train. The compressed nitrogen 

you use to purge the sampling train must 

contain no more than 1 parts per million by 

volume (ppmv) oxygen, 1 ppmv total 

hydrocarbons as carbon, and 2 ppmv 

moisture. The compressed nitrogen must not 

contribute more than 0.1 mg of residual mass 

per purge. 

7.2 Sample Recovery and Analytical 

Reagents. You will need acetone, hexane, 

anhydrous calcium sulfate, ammonia 

hydroxide, and deionized water for the 

sample recovery and analysis. Unless 

otherwise indicated, all reagents must 

conform to the specifications established by 

the Committee on Analytical Reagents of the 

American Chemical Society. If such 

specifications are not available, then use the 

best available grade. Additional information 

on each of these items is in the following 

paragraphs: 

7.2.1 Acetone. Use acetone that is stored 

in a glass bottle. Do not use acetone from a 

metal container because it normally produces 

a high residual mass in the laboratory and 

field reagent blanks. You must use acetone 

that has a blank value less than 1.0 ppmw 

(0.1 mg/100 ml) residue. 

7.2.2 Hexane, American Chemical Society 

grade. You must use hexane that has a blank 

residual mass value less than 1.0 ppmw (0.1 

mg/100 ml) residue. 

7.2.3 Water. Use deionized, ultra-filtered 

water that contains 1 ppmw (1 mg/L) residual 

mass or less to recover material caught in the 

impinger. 

7.2.4 Condensable Particulate Sample 

Desiccant. Use indicating-type anhydrous 

calcium sulfate to desiccate water and 

organic extract residue samples prior to 

weighing. 

7.2.5 Ammonium Hydroxide. Use 

National Institute of Standards and 

Technology-traceable or equivalent (0.1 N) 

NH4OH. 

7.2.6 Standard Buffer Solutions. Use one 

buffer solution with a neutral pH and a 

second buffer solution with an acid pH of no 

less than 4. 

8.0 Sample Collection, Preservation, 

Storage, and Transport 

8.1 Qualifications. This is a complex test 

method. To obtain reliable results, you 

should be trained and experienced with instack filtration systems (such as, cyclones, 

impactors, and thimbles) and impinger and 

moisture train systems. 

8.2 Preparations. You must clean all 

glassware used to collect and analyze 

samples prior to field tests as described in 

Section 8.4 prior to use. Cleaned glassware 

must be used at the start of each new source 

category tested at a single facility. Analyze 

laboratory reagent blanks (water, acetone, 

and hexane) before field tests to verify low 

blank concentrations. Follow the pretest 

preparation instructions in Section 8.1 of 

Method 5. 

8.3 Site Setup. You must follow the 

procedures required in Methods 5, 17, or 

201A, whichever is applicable to your test 

requirements including: 

(a) Determining the sampling site location 

and traverse points. 

(b) Calculating probe/cyclone blockage (as 

appropriate). 

(c) Verifying the absence of cyclonic flow. 

(d) Completing a preliminary velocity 

profile, and selecting a nozzle(s) and 

sampling rate. 

8.3.1 Sampling Site Location. Follow the 

standard procedures in Method 1 of 

appendix A–1 to part 60 to select the 

appropriate sampling site. Choose a location 

that maximizes the distance from upstream 

and downstream flow disturbances. 

8.3.2 Traverse points. Use the required 

number of traverse points at any location, as 

found in Methods 5, 17, or 201A, whichever 

is applicable to your test requirements. You 

must prevent the disturbance and capture of 

any solids accumulated on the inner wall 

surfaces by maintaining a 1-inch distance 

from the stack wall (0.5 inch for sampling 

locations less than 24 inches in diameter). 

8.4 Sampling Train Preparation. A 

schematic of the sampling train used in this 

method is shown in Figure 1 of Section 18. 

All glassware that is used to collect and 

analyze samples must be cleaned prior to the 

test with soap and water, and rinsed using 

tap water, deionized water, acetone, and 

finally, hexane. It is important to completely 

remove all silicone grease from areas that 

will be exposed to the hexane rinse during 

sample recovery. After cleaning, you must 

bake glassware at 300 °C for six hours prior 

to beginning tests at each source category 

sampled at a facility. As an alternative to 

baking glassware, a field train proof blank, as 

specified in Section 8.5.4.10, can be 

performed on the sampling train glassware 

that is used to collect CPM samples. Prior to 

each sampling run, the train glassware used 

to collect condensable PM must be rinsed 

thoroughly with deionized, ultra-filtered 

water that that contains 1 ppmw (1 mg/L) 

residual mass or less. 

8.4.1 Condenser and Water Dropout 

Impinger. Add a Method 23 type condenser 

and a condensate dropout impinger without 

bubbler tube after the final probe extension 

that connects the in-stack or out-of-stack hot 

filter assembly with the CPM sampling train. 

The Method 23 type stack gas condenser is 

described in Section 2.1.2 of Method 23. The 

condenser must be capable of cooling the 

stack gas to less than or equal to 30 °C (85 

°F). 

8.4.2 Backup Impinger. The water 

dropout impinger is followed by a modified 

Greenburg Smith impinger (backup impinger) 

with no taper (see Figure 1 of Section 18). 

Place the water dropout and backup 

impingers in an insulated box with water at 

less than or equal to 30 °C (less than or equal 

to 85 °F). At the start of the tests, the water 

dropout and backup impingers must be 

clean, without any water or reagent added. 

8.4.3 CPM Filter. Place a filter holder 

with a filter meeting the requirements in 

Section 7.1.1 after the backup impinger. The 

connection between the CPM filter and the 

moisture trap impinger must include a 

thermocouple fitting that provides a leak-free 

seal between the thermocouple and the stack 

gas. (Note: A thermocouple well is not 

sufficient for this purpose because the 

fluoropolymer- or steel-encased 

thermocouple must be in contact with the 

sample gas.) 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80163 

8.4.4 Moisture Traps. You must use a 

modified Greenburg-Smith impinger 

containing 100 ml of water, or the alternative 

described in Method 5 of appendix A–3 to 

part 60, followed by an impinger containing 

silica gel to collect moisture that passes 

through the CPM filter. You must maintain 

the gas temperature below 20 °C (68 °F) at the 

exit of the moisture traps. 

8.4.5 Silica Gel Trap. Place 200 to 300 g 

of silica gel in each of several air-tight 

containers. Weigh each container, including 

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

weight on the filterable particulate data 

sheet. As an alternative, the silica gel need 

not be preweighed, but may be weighed 

directly in its impinger or sampling holder 

just prior to train assembly. 

8.4.6 Leak-Check (Pretest). Use the 

procedures outlined in Method 5 of appendix 

A–3 to part 60, Method 17 of appendix A– 

6 to part 60, or Method 201A of appendix M 

to this part as appropriate to leak check the 

entire sampling system. Specifically, perform 

the following procedures: 

8.4.6.1 Sampling train. You must pretest 

the entire sampling train for leaks. The 

pretest leak-check must have a leak rate of 

not more than 0.02 actual cubic feet per 

minute or 4 percent of the average sample 

flow during the test run, whichever is less. 

Additionally, you must conduct the leakcheck at a vacuum equal to or greater than 

the vacuum anticipated during the test run. 

Enter the leak-check results on the field test 

data sheet for the filterable particulate 

method. (Note: Conduct leak-checks during 

port changes only as allowed by the filterable 

particulate method used with this method.) 

8.4.6.2 Pitot tube assembly. After you 

leak-check the sample train, perform a leakcheck of the pitot tube assembly. Follow the 

procedures outlined in Section 8.4.1 of 

Method 5. 

8.5 Sampling Train Operation. Operate 

the sampling train as described in the 

filterable particulate sampling method (i.e., 

Method 5 of appendix A–3 to part 60, 

Method 17 of appendix A–6 to part 60, or 

Method 201A of appendix M to this part) 

with the following additions or exceptions: 

8.5.1 CPM Filter Assembly. On the field 

data sheet for the filterable particulate 

method, record the CPM filter temperature 

readings at the beginning of each sample time 

increment and when sampling is halted. 

Maintain the CPM filter greater than 20 °C 

(greater than 65 °F) but less than or equal to 

30 °C (less than or equal to 85 °F) during 

sample collection. (Note: Maintain the 

temperature of the CPM filter assembly as 

close to 30 °C (85 °F) as feasible.) 

8.5.2 Leak-Check Probe/Sample Train 

Assembly (Post-Test). Conduct the leak rate 

check according to the filterable particulate 

sampling method used during sampling. If 

required, conduct the leak-check at a vacuum 

equal to or greater than the maximum 

vacuum achieved during the test run. If the 

leak rate of the sampling train exceeds 0.02 

actual cubic feet per minute or four percent 

of the average sampling rate during the test 

run (whichever is less), then the run is 

invalid and you must repeat it. 

8.5.3 Post-Test Nitrogen Purge. As soon 

as possible after the post-test leak-check, 

detach the probe, any cyclones, and in-stack 

or hot filters from the condenser and 

impinger train. If no water was collected 

before the CPM filter, then you may skip the 

remaining purge steps and proceed with 

sample recovery (see Section 8.5.4). You may 

purge the CPM sampling train using the 

sampling system meter box and vacuum 

pump or by passing nitrogen through the 

train under pressure. For either type of purge, 

you must first attach the nitrogen supply line 

to a purged inline filter. 

8.5.3.1 If you choose to conduct a 

pressurized nitrogen purge on the complete 

CPM sampling train, you must quantitatively 

transfer the water collected in the condenser 

and the water dropout impinger to the 

backup impinger. You must measure the 

water combined in the backup impinger and 

record the volume or weight as part of the 

moisture collected during sampling as 

specified in Section 8.5.3.4. 

(a) You must conduct the purge on the 

condenser, backup impinger, and CPM filter. 

If the tip of the backup impinger insert does 

not extend below the water level (including 

the water transferred from the first impinger), 

you must add a measured amount of 

degassed, deionized ultra-filtered water that 

contains 1 ppmw (1 mg/L) residual mass or 

less until the impinger tip is at least 1 

centimeter below the surface of the water. 

You must record the amount of water added 

to the water dropout impinger (Vp) (see 

Figure 4 of Section 18) to correct the 

moisture content of the effluent gas. (Note: 

Prior to use, water must be degassed using a 

nitrogen purge bubbled through the water for 

at least 15 minutes to remove dissolved 

oxygen). 

(b) To perform the nitrogen purge using 

positive pressure nitrogen flow, you must 

start with no flow of gas through the clean 

purge line and fittings. Connect the filter 

outlet to the input of the impinger train and 

disconnect the vacuum line from the exit of 

the silica moisture collection impinger (see 

Figure 3 of Section 18). You may purge only 

the CPM train by disconnecting the moisture 

train components if you measure moisture in 

the field prior to the nitrogen purge. You 

must increase the nitrogen flow gradually to 

avoid over-pressurizing the impinger array. 

You must purge the CPM train at a minimum 

of 14 liters per minute for at least one hour. 

At the conclusion of the purge, turn off the 

nitrogen delivery system. 

8.5.3.2 If you choose to conduct a 

nitrogen purge on the complete CPM 

sampling train using the sampling system 

meter box and vacuum pump, replace the 

short stem impinger insert with a modified 

Greenberg Smith impinger insert. The 

impinger tip length must extend below the 

water level in the impinger catch. 

(a) You must conduct the purge on the 

complete CPM sampling train starting at the 

inlet of the condenser. If insufficient water 

was collected, you must add a measured 

amount of degassed, deionized ultra-filtered 

water that contains 1 ppmw (1 mg/L) residual 

mass or less until the impinger tip is at least 

1 centimeter below the surface of the water. 

You must record the amount of water added 

to the water dropout impinger (Vp) (see 

Figure 4 of Section 18) to correct the 

moisture content of the effluent gas. (Note: 

Prior to use, water must be degassed using a 

nitrogen purge bubbled through the water for 

at least 15 minutes to remove dissolved 

oxygen). 

(b) You must start the purge using the 

sampling train vacuum pump with no flow 

of gas through the clean purge line and 

fittings. Connect the filter outlet to the input 

of the impinger train (see Figure 2 of Section 

18). To avoid over- or under-pressurizing the 

impinger array, slowly commence the 

nitrogen gas flow through the line while 

simultaneously opening the meter box pump 

valve(s). Adjust the pump bypass and/or 

nitrogen delivery rates to obtain the 

following conditions: 14 liters/min or DH@ 

and a positive overflow rate through the 

rotameter of less than 2 liters/min. The 

presence of a positive overflow rate 

guarantees that the nitrogen delivery system 

is operating at greater than ambient pressure 

and prevents the possibility of passing 

ambient air (rather than nitrogen) through the 

impingers. Continue the purge under these 

conditions for at least one hour, checking the 

rotameter and DH@ value(s) at least every 15 

minutes. At the conclusion of the purge, 

simultaneously turn off the delivery and 

pumping systems. 

8.5.3.3 During either purge procedure, 

continue operation of the condenser 

recirculation pump, and heat or cool the 

water surrounding the first two impingers to 

maintain the gas temperature measured at the 

exit of the CPM filter greater than 20 °C 

(greater than 65 °F), but less than or equal to 

30 °C (less than or equal to 85 °F). If the 

volume of liquid collected in the moisture 

traps has not been determined prior to 

conducting the nitrogen purge, maintain the 

temperature of the moisture traps following 

the CPM filter to prevent removal of moisture 

during the purge. If necessary, add more ice 

during the purge to maintain the gas 

temperature measured at the exit of the silica 

gel impinger below 20 °C (68 °F). Continue 

the purge under these conditions for at least 

one hour, checking the rotameter and DH@ 

value(s) periodically. At the conclusion of 

the purge, simultaneously turn off the 

delivery and pumping systems. 

8.5.3.4 Weigh the liquid, or measure the 

volume of the liquid collected in the dropout, 

impingers, and silica trap if this has not been 

done prior to purging the sampling train. 

Measure the liquid in the water dropout 

impinger to within 1 ml using a clean 

graduated cylinder or by weighing it to 

within 0.5 g using a balance. Record the 

volume or weight of liquid present to be used 

to calculate the moisture content of the 

effluent gas in the field log notebook. 

8.5.3.5 If a balance is available in the 

field, weigh the silica impinger to within 0.5 

g. Note the color of the indicating silica gel 

in the last impinger to determine whether it 

has been completely spent, and make a 

notation of its condition in the field log 

notebook. 

8.5.4 Sample Recovery. 

8.5.4.1 Recovery of filterable PM. 

Recovery of filterable PM involves the 

quantitative transfer of particles according to 

the filterable particulate sampling method 

(i.e., Method 5 of appendix A–3 to part 60, 


jlentini on DSKJ8SOYB1PROD with RULES2
80164 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

Method 17 of appendix A–6 to part 60, or 

Method 201A of appendix M to this part). 

8.5.4.2 CPM Container #1, Aqueous 

liquid impinger contents. Quantitatively 

transfer liquid from the dropout and the 

backup impingers prior to the CPM filter into 

a clean, leak-proof container labeled with test 

identification and ‘‘CPM Container #1, 

Aqueous Liquid Impinger Contents.’’ Rinse 

all sampling train components including the 

back half of the filterable PM filter holder, 

the probe extension, condenser, each 

impinger and the connecting glassware, and 

the front half of the CPM filter housing twice 

with water. Recover the rinse water, and add 

it to CPM Container #1. Mark the liquid level 

on the container. 

8.5.4.3 CPM Container #2, Organic rinses. 

Follow the water rinses of the probe 

extension, condenser, each impinger and all 

of the connecting glassware and front half of 

the CPM filter with an acetone rinse. Recover 

the acetone rinse into a clean, leak-proof 

container labeled with test identification and 

‘‘CPM Container #2, Organic Rinses.’’ Then 

repeat the entire rinse procedure with two 

rinses of hexane, and save the hexane rinses 

in the same container as the acetone rinse 

(CPM Container #2). Mark the liquid level on 

the jar. 

8.5.4.4 CPM Container #3, CPM filter 

sample. Use tweezers and/or clean 

disposable surgical gloves to remove the filter 

from the CPM filter holder. Place the filter in 

the Petri dish labeled with test identification 

and ‘‘CPM Container #3, Filter Sample.’’ 

8.5.4.5 CPM Container #4, Cold impinger 

water. You must weigh or measure the 

volume of the contents of CPM Container #4 

either in the field or during sample analysis 

(see Section 11.2.4). If the water from the 

cold impinger has been weighed in the field, 

it can be discarded. Otherwise, quantitatively 

transfer liquid from the cold impinger that 

follows the CPM filter into a clean, leak-proof 

container labeled with test identification and 

‘‘CPM Container #4, Cold Water Impinger.’’ 

Mark the liquid level on the container. CPM 

Container #4 holds the remainder of the 

liquid water from the emission gases. 

8.5.4.6 CPM Container #5, Silica gel 

absorbent. You must weigh the contents of 

CPM Container #5 in the field or during 

sample analysis (see Section 11.2.5). If the 

silica gel has been weighed in the field to 

measure water content, then it can be 

discarded or recovered for reuse. Otherwise, 

transfer the silica gel to its original container 

labeled with test identification and ‘‘CPM 

Container #5, Silica Gel Absorbent’’ and seal. 

You may use a funnel to make it easier to 

pour the silica gel without spilling. You may 

also use a rubber policeman as an aid in 

removing the silica gel from the impinger. It 

is not necessary to remove the small amount 

of silica gel dust particles that may adhere to 

the impinger wall and are difficult to remove. 

Since the gain in weight is to be used for 

moisture calculations, do not use any water 

or other liquids to transfer the silica gel. 

8.5.4.7 CPM Container #6, Acetone field 

reagent blank. Take approximately 200 ml of 

the acetone directly from the wash bottle you 

used for sample recovery and place it in a 

clean, leak-proof container labeled with test 

identification and ‘‘CPM Container #6, 

Acetone Field Reagent Blank’’ (see Section 

11.2.6 for analysis). Mark the liquid level on 

the container. Collect one acetone field 

reagent blank from the lot(s) of solvent used 

for the test. 

8.5.4.8 CPM Container #7, Water field 

reagent blank. Take approximately 200 ml of 

the water directly from the wash bottle you 

used for sample recovery and place it in a 

clean, leak-proof container labeled with test 

identification and ‘‘CPM Container #7, Water 

Field Reagent Blank’’ (see Section 11.2.7 for 

analysis). Mark the liquid level on the 

container. Collect one water field reagent 

blank from the lot(s) of water used for the 

test. 

8.5.4.9 CPM Container #8, Hexane field 

reagent blank. Take approximately 200 ml of 

the hexane directly from the wash bottle you 

used for sample recovery and place it in a 

clean, leak-proof container labeled with test 

identification and ‘‘CPM Container #8, 

Hexane Field Reagent Blank’’ (see Section 

11.2.8 for analysis). Mark the liquid level on 

the container. Collect one hexane field 

reagent blank from the lot(s) of solvent used 

for the test. 

8.5.4.10 Field train proof blank. If you 

did not bake the sampling train glassware as 

specified in Section 8.4, you must conduct a 

field train proof blank as specified in 

Sections 8.5.4.11 and 8.5.4.12 to demonstrate 

the cleanliness of sampling train glassware. 

8.5.4.11 CPM Container #9, Field train 

proof blank, inorganic rinses. Prior to 

conducting the emission test, rinse the probe 

extension, condenser, each impinger and the 

connecting glassware, and the front half of 

the CPM filter housing twice with water. 

Recover the rinse water and place it in a 

clean, leak-proof container labeled with test 

identification and ‘‘CPM Container #9, Field 

Train Proof Blank, Inorganic Rinses.’’ Mark 

the liquid level on the container. 

8.5.4.12 CPM Container #10, Field train 

proof blank, organic rinses. Follow the water 

rinse of the probe extension, condenser, each 

impinger and the connecting glassware, and 

the front half of the CPM filter housing with 

an acetone rinse. Recover the acetone rinse 

into a clean, leak-proof container labeled 

with test identification and ‘‘CPM Container 

#10, Field Train Proof Blank, Organic 

Rinses.’’ Then repeat the entire rinse 

procedure with two rinses of hexane and 

save the hexane rinses in the same container 

as the acetone rinse (CPM Container #10). 

Mark the liquid level on the container. 

8.5.5 Transport procedures. Containers 

must remain in an upright position at all 

times during shipping. You do not have to 

ship the containers under dry or blue ice. 

However, samples must be maintained at or 

below 30 °C (85 °F) during shipping. 

9.0 Quality Control 

9.1 Daily Quality Checks. You must 

perform daily quality checks of field log 

notebooks and data entries and calculations 

using data quality indicators from this 

method and your site-specific test plan. You 

must review and evaluate recorded and 

transferred raw data, calculations, and 

documentation of testing procedures. You 

must initial or sign log notebook pages and 

data entry forms that were reviewed. 

9.2 Calculation Verification. Verify the 

calculations by independent, manual checks. 

You must flag any suspect data and identify 

the nature of the problem and potential effect 

on data quality. After you complete the test, 

prepare a data summary and compile all the 

calculations and raw data sheets. 

9.3 Conditions. You must document data 

and information on the process unit tested, 

the particulate control system used to control 

emissions, any non-particulate control 

system that may affect particulate emissions, 

the sampling train conditions, and weather 

conditions. Discontinue the test if the 

operating conditions may cause nonrepresentative particulate emissions. 

9.4 Field Analytical Balance Calibration 

Check. Perform calibration check procedures 

on field analytical balances each day that 

they are used. You must use National 

Institute of Standards and Technology 

(NIST)-traceable weights at a mass 

approximately equal to the weight of the 

sample plus container you will weigh. 

9.5 Glassware. Use class A volumetric 

glassware for titrations, or calibrate your 

equipment against NIST-traceable glassware. 

9.6 Laboratory Analytical Balance 

Calibration Check. Check the calibration of 

your laboratory analytical balance each day 

that you weigh CPM samples. You must use 

NIST Class S weights at a mass 

approximately equal to the weight of the 

sample plus container you will weigh. 

9.7 Laboratory Reagent Blanks. You 

should run blanks of water, acetone, and 

hexane used for field recovery and sample 

analysis. Analyze at least one sample (150 ml 

minimum) of each lot of reagents that you 

plan to use for sample recovery and analysis 

before you begin testing. These blanks are not 

required by the test method, but running 

blanks before field use is advisable to verify 

low blank concentrations, thereby reducing 

the potential for a high field blank on test 

samples. 

9.8 Field Reagent Blanks. You should run 

at least one field reagent blank of water, 

acetone, and hexane you use for field 

recovery. These blanks are not required by 

the test method, but running independent 

field reagent blanks is advisable to verify that 

low blank concentrations were maintained 

during field solvent use and demonstrate that 

reagents have not been contaminated during 

field tests. 

9.9 Field Train Proof Blank. If you are not 

baking glassware as specified in Section 8.4, 

you must recover a minimum of one field 

train proof blank for the sampling train used 

for testing each new source category at a 

single facility. You must assemble the 

sampling train as it will be used for testing. 

You must recover the field train proof blank 

samples as described in Section 8.5.4.11 and 

8.5.4.12. 

9.10 Field Train Recovery Blank. You 

must recover a minimum of one field train 

blank for each source category tested at the 

facility. You must recover the field train 

blank after the first or second run of the test. 

You must assemble the sampling train as it 

will be used for testing. Prior to the purge, 

you must add 100 ml of water to the first 

impinger and record this data on Figure 4. 

You must purge the assembled train as 


jlentini on DSKJ8SOYB1PROD with RULES2
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80165 

described in Sections 8.5.3.2 and 8.5.3.3. You 

must recover field train blank samples as 

described in Section 8.5.4. From the field 

sample weight, you will subtract the 

condensable particulate mass you determine 

with this blank train or 0.002 g (2.0 mg), 

whichever is less. 

10.0 Calibration and Standardization 

Maintain a field log notebook of all 

condensable particulate sampling and 

analysis calibrations. Include copies of the 

relevant portions of the calibration and field 

logs in the final test report. 

10.1 Thermocouple Calibration. You 

must calibrate the thermocouples using the 

procedures described in Section 10.3.1 of 

Method 2 of appendix A–1 to part 60 or 

Alternative Method 2, Thermocouple 

Calibration (ALT–011) (http://www.epa.gov/ 

ttn/emc). Calibrate each temperature sensor 

at a minimum of three points over the 

anticipated range of use against a NISTtraceable thermometer. Alternatively, a 

reference thermocouple and potentiometer 

calibrated against NIST standards can be 

used. 

10.2 Ammonium Hydroxide. The 0.1 N 

NH4OH used for titrations in this method is 

made as follows: Add 7 ml of concentrated 

(14.8 M) NH4OH to l liter of water. 

Standardize against standardized 0.1 

N H2SO4, and calculate the exact normality 

using a procedure parallel to that described 

in Section 10.5 of Method 6 of appendix A– 

4 to 40 CFR part 60. Alternatively, purchase 

0.1 N NH4OH that has been standardized 

against a NIST reference material. Record the 

normality on the CPM Work Table (see 

Figure 6 of Section 18). 

11.0 Analytical Procedures 

11.1 Analytical Data Sheets. (a) Record 

the filterable particulate field data on the 

appropriate (i.e., Method 5, 17, or 201A) 

analytical data sheets. Alternatively, data 

may be recorded electronically using 

software applications such as the Electronic 

Reporting Tool available at http:// 

www.epa.gov/ttn/chief/ert/ert_tool.html. 

Record the condensable particulate data on 

the CPM Work Table (see Figure 6 of Section 

18). 

(b) Measure the liquid in all containers 

either volumetrically to ± 1 ml or 

gravimetrically to ± 0.5 g. Confirm on the 

filterable particulate analytical data sheet 

whether leakage occurred during transport. If 

a noticeable amount of leakage has occurred, 

either void the sample or use methods 

(subject to the approval of the Administrator) 

to correct the final results. 

11.2 Condensable PM Analysis. See the 

flow chart in Figure 7 of Section 18 for the 

steps to process and combine fractions from 

the CPM train. 

11.2.1 Container #3, CPM Filter Sample. 

If the sample was collected by Method 17 or 

Method 201A with a stack temperature below 

30 °C (85 °F) and the filter can be brought 

to a constant weight, transfer the filter and 

any loose PM from the sample container to 

a tared glass weighing dish. (See Section 3.0 

for a definition of constant weight.) Desiccate 

the sample for 24 hours in a desiccator 

containing anhydrous calcium sulfate. Weigh 

to a constant weigh and report the results to 

the nearest 0.1 mg. If the filter cannot be 

brought to constant weight using this 

procedure, you must follow the extraction 

and weighing procedures in this section. (See 

Section 3.0 for a definition of constant 

weight.) Extract the filter recovered from the 

low-temperature portion of the train, and 

combine the extracts with the organic and 

inorganic fractions resulting from the 

aqueous impinger sample recovery in 

Containers 1 and 2, respectively. Extract the 

CPM filter as follows: 

11.2.1.1 Extract the water soluble 

(aqueous or inorganic) CPM from the CPM 

filter by folding the filter in quarters and 

placing it into a 50-ml extraction tube. Add 

sufficient deionized, ultra-filtered water to 

cover the filter (e.g., 10 ml of water). Place 

the extractor tube into a sonication bath and 

extract the water-soluble material for a 

minimum of two minutes. Combine the 

aqueous extract with the contents of 

Container #1. Repeat this extraction step 

twice for a total of three extractions. 

11.2.1.2 Extract the organic soluble CPM 

from the CPM filter by adding sufficient 

hexane to cover the filter (e.g., 10 ml of 

hexane). Place the extractor tube into a 

sonication bath and extract the organic 

soluble material for a minimum of two 

minutes. Combine the organic extract with 

the contents of Container #2. Repeat this 

extraction step twice for a total of three 

extractions. 

11.2.2 CPM Container #1, Aqueous 

Liquid Impinger Contents. Analyze the water 

soluble CPM in Container 1 as described in 

this section. Place the contents of Container 

#1 into a separatory funnel. Add 

approximately 30 ml of hexane to the funnel, 

mix well, and drain off the lower organic 

phase. Repeat this procedure twice with 30 

ml of hexane each time combining the 

organic phase from each extraction. Each 

time, leave a small amount of the organic/ 

hexane phase in the separatory funnel, 

ensuring that no water is collected in the 

organic phase. This extraction should yield 

about 90 ml of organic extract. Combine the 

organic extract from Container #1 with the 

organic train rinse in Container 2. 

11.2.2.1 Determine the inorganic fraction 

weight. Transfer the aqueous fraction from 

the extraction to a clean 500-ml or smaller 

beaker. Evaporate to no less than 10 ml liquid 

on a hot plate or in the oven at 105 °C and 

allow to dry at room temperature (not to 

exceed 30 °C (85 °F)). You must ensure that 

water and volatile acids have completely 

evaporated before neutralizing nonvolatile 

acids in the sample. Following evaporation, 

desiccate the residue for 24 hours in a 

desiccator containing anhydrous calcium 

sulfate. Weigh at intervals of at least six 

hours to a constant weight. (See Section 3.0 

for a definition of Constant weight.) Report 

results to the nearest 0.1 mg on the CPM 

Work Table (see Figure 6 of Section 18) and 

proceed directly to Section 11.2.3. If the 

residue can not be weighed to constant 

weight, redissolve the residue in 100 ml of 

deionized distilled ultra-filtered water that 

contains 1 ppmw (1 mg/L) residual mass or 

less and continue to Section 11.2.2.2. 

11.2.2.2 Use titration to neutralize acid in 

the sample and remove water of hydration. 

If used, calibrate the pH meter with the 

neutral and acid buffer solutions. Then titrate 

the sample with 0.1N NH4OH to a pH of 7.0, 

as indicated by the pH meter or colorimetric 

indicator. Record the volume of titrant used 

on the CPM Work Table (see Figure 6 of 

Section 18). 

11.2.2.3 Using a hot plate or an oven at 

105 °C, evaporate the aqueous phase to 

approximately 10 ml. Quantitatively transfer 

the beaker contents to a clean, 50-ml pretared weighing tin and evaporate to dryness 

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

°F)) and pressure in a laboratory hood. 

Following evaporation, desiccate the residue 

for 24 hours in a desiccator containing 

anhydrous calcium sulfate. Weigh at 

intervals of at least six hours to a constant 

weight. (See Section 3.0 for a definition of 

Constant weight.) Report results to the 

nearest 0.1 mg on the CPM Work Table (see 

Figure 6 of Section 18). 

11.2.2.4 Calculate the correction factor to 

subtract the NH4

+ retained in the sample 

using Equation 1 in Section 12. 

11.2.3 CPM Container #2, Organic 

Fraction Weight Determination. Analyze the 

organic soluble CPM in Container #2 as 

described in this section. Place the organic 

phase in a clean glass beaker. Evaporate the 

organic extract at room temperature (not to 

exceed 30 °C (85 °F)) and pressure in a 

laboratory hood to not less than 10 ml. 

Quantitatively transfer the beaker contents to 

a clean 50-ml pre-tared weighing tin and 

evaporate to dryness at room temperature 

(not to exceed 30 °C (85 °F)) and pressure in 

a laboratory hood. Following evaporation, 

desiccate the organic fraction for 24 hours in 

a desiccator containing anhydrous calcium 

sulfate. Weigh at intervals of at least six 

hours to a constant weight (i.e., less than or 

equal to 0.5 mg change from previous 

weighing), and report results to the nearest 

0.1 mg on the CPM Work Table (see Figure 

6 of Section 18). 

11.2.4 CPM Container #4, Cold Impinger 

Water. If the amount of water has not been 

determined in the field, note the level of 

liquid in the container, and confirm on the 

filterable particulate analytical data sheet 

whether leakage occurred during transport. If 

a noticeable amount of leakage has occurred, 

either void the sample or use methods 

(subject to the approval of the Administrator) 

to correct the final results. Measure the liquid 

in Container #4 either volumetrically to ± 1 

ml or gravimetrically to ± 0.5 g, and record 

the volume or weight on the filterable 

particulate analytical data sheet of the 

filterable PM test method. 

11.2.5 CPM Container #5, Silica Gel 

Absorbent. Weigh the spent silica gel (or 

silica gel plus impinger) to the nearest 0.5 g 

using a balance. This step may be conducted 

in the field. Record the weight on the 

filterable particulate analytical data sheet of 

the filterable PM test method. 

11.2.6 Container #6, Acetone Field 

Reagent Blank. Use 150 ml of acetone from 

the blank container used for this analysis. 

Transfer 150 ml of the acetone to a clean 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 


jlentini on DSKJ8SOYB1PROD with RULES2
80166 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

the beaker contents to a clean 50-ml pre-tared 

weighing tin, and evaporate to dryness at 

room temperature (not to exceed 30 °C (85 

°F)) and pressure in a laboratory hood. 

Following evaporation, desiccate the residue 

for 24 hours in a desiccator containing 

anhydrous calcium sulfate. Weigh at 

intervals of at least six hours to a constant 

weight (i.e., less than or equal to 0.5 mg 

change from previous weighing), and report 

results to the nearest 0.1 mg on Figure 4 of 

Section 19. 

11.2.7 Water Field Reagent Blank, 

Container #7. Use 150 ml of the water from 

the blank container for this analysis. Transfer 

the water to a clean 250-ml beaker, and 

evaporate to approximately 10 ml liquid in 

the oven at 105 °C. Quantitatively transfer the 

beaker contents to a clean 50 ml pre-tared 

weighing tin and evaporate to dryness at 

room temperature (not to exceed 30 °C (85 

°F)) and pressure in a laboratory hood. 

Following evaporation, desiccate the residue 

for 24 hours in a desiccator containing 

anhydrous calcium sulfate. Weigh at 

intervals of at least six hours to a constant 

weight (i.e., less than or equal to 0.5 mg 

change from previous weighing) and report 

results to the nearest 0.1 mg on Figure 4 of 

Section 18. 

11.2.8 Hexane Field Reagent Blank, 

Container #8. Use 150 ml of hexane from the 

blank container for this analysis. Transfer 

150 ml of the hexane to a clean 250-ml 

beaker. Evaporate the hexane at room 

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

pressure in a laboratory hood to 

approximately 10 ml. Quantitatively transfer 

the beaker contents to a clean 50-ml pre-tared 

weighing tin and evaporate to dryness at 

room temperature (not to exceed 30 °C (85 

°F)) and pressure in a laboratory hood. 

Following evaporation, desiccate the residue 

for 24 hours in a desiccator containing 

anhydrous calcium sulfate. Weigh at 

intervals of at least six hours to a constant 

weight (i.e., less than or equal to 0.5 mg 

change from previous weighing), and report 

results to the nearest 0.1 mg on Figure 4 of 

Section 18. 

12.0 Calculations and Data Analysis 

12.1 Nomenclature. Report results in 

International System of Units (SI units) 

unless the regulatory authority for testing 

specifies English units. The following 

nomenclature is used. 

DH@ = Pressure drop across orifice at flow 

rate of 0.75 SCFM at standard conditions, 

inches of water column (Note: Specific to 

each orifice and meter box). 

17.03 = mg/milliequivalents for ammonium 

ion. 

ACFM = Actual cubic feet per minute. 

Ccpm = Concentration of the condensable PM 

in the stack gas, dry basis, corrected to 

standard conditions, milligrams/dry 

standard cubic foot. 

mc = Mass of the NH4

+ added to sample to 

form ammonium sulfate, mg. 

mcpm = Mass of the total condensable PM, mg. 

mfb = Mass of total CPM in field train 

recovery blank, mg. 

mg = Milligrams. 

mg/L = Milligrams per liter. 

mi = Mass of inorganic CPM, mg. 

mib = Mass of inorganic CPM in field train 

recovery blank, mg. 

mo = Mass of organic CPM, mg. 

mob = Mass of organic CPM in field train 

blank, mg. 

mr = Mass of dried sample from inorganic 

fraction, mg. 

N = Normality of ammonium hydroxide 

titrant. 

ppmv = Parts per million by volume. 

ppmw = Parts per million by weight. 

Vm(std) = Volume of gas sample measured by 

the dry gas meter, corrected to standard 

conditions, dry standard cubic meter 

(dscm) or dry standard cubic foot (dscf) 

as defined in Equation 5–1 of Method 5. 

Vt = Volume of NH4OH titrant, ml. 

Vp = Volume of water added during train 

purge. 

12.2 Calculations. Use the following 

equations to complete the calculations 

required in this test method. Enter the 

appropriate results from these calculations 

on the CPM Work Table (see Figure 6 of 

Section 18). 

12.2.1 Mass of ammonia correction. 

Correction for ammonia added during 

titration of 100 ml aqueous CPM sample. 

This calculation assumes no waters of 

hydration. 

12.2.2 Mass of the Field Train Recovery 

Blank (mg). Per Section 9.10, the mass of the 

field train recovery blank, mfb, shall not 

exceed 2.0 mg. 

12.2.3 Mass of Inorganic CPM (mg). 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.058</GPH> ER21DE10.059</GPH> ER21DE10.060</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80167 

12.2.4 Total Mass of CPM (mg). 

12.2.5 Concentration of CPM (mg/dscf). 

12.3 Emissions Test Report. You must 

prepare a test report following the guidance 

in EPA Guidance Document 043 (Preparation 

and Review of Test Reports. December 1998). 

13.0 Method Performance 

An EPA field evaluation of the revised 

Method 202 showed the following precision 

in the results: approximately 4 mg for total 

CPM, approximately 0.5 mg for organic CPM, 

and approximately 3.5 mg for inorganic CPM. 

14.0 Pollution Prevention 

[Reserved] 

15.0 Waste Management 

Solvent and water are evaporated in a 

laboratory hood during analysis. No liquid 

waste is generated in the performance of this 

method. Organic solvents used to clean 

sampling equipment should be managed as 

RCRA organic waste. 

16.0 Alternative Procedures 

Alternative Method 2, Thermocouple 

Calibration (ALT–011) for the thermocouple 

calibration can be found at http:// 

www.epa.gov/ttn/emc/approalt.html. 

17.0 References 

(1) Commonwealth of Pennsylvania, 

Department of Environmental Resources. 

1960. Chapter 139, Sampling and Testing 

(Title 25, Rules and Regulations, part I, 

Department of Environmental Resources, 

Subpart C, Protection of Natural Resources, 

Article III, Air Resources). January 8, 1960. 

(2) DeWees, W.D. and K.C. Steinsberger. 

1989. ‘‘Method Development and Evaluation 

of Draft Protocol for Measurement of 

Condensable Particulate Emissions.’’ Draft 

Report. November 17, 1989. 

(3) DeWees, W.D., K.C. Steinsberger, G.M. 

Plummer, L.T. Lay, G.D. McAlister, and R.T. 

Shigehara. 1989. ‘‘Laboratory and Field 

Evaluation of EPA Method 5 Impinger Catch 

for Measuring Condensable Matter from 

Stationary Sources.’’ Paper presented at the 

1989 EPA/AWMA International Symposium 

on Measurement of Toxic and Related Air 

Pollutants. Raleigh, North Carolina. May 

1–5, 1989. 

(4) Electric Power Research Institute 

(EPRI). 2008. ‘‘Laboratory Comparison of 

Methods to Sample and Analyze 

Condensable PM.’’ EPRI Agreement EP– 

P24373/C11811 Condensable Particulate 

Methods: EPRI Collaboration with EPA, 

October 2008. 

(5) Nothstein, Greg. Masters Thesis. 

University of Washington. Department of 

Environmental Health. Seattle, Washington. 

(6) Richards, J., T. Holder, and D. Goshaw. 

2005. ‘‘Optimized Method 202 Sampling 

Train to Minimize the Biases Associated with 

Method 202 Measurement of Condensable 

PM Emissions.’’ Paper presented at Air & 

Waste Management Association Hazardous 

Waste Combustion Specialty Conference. St. 

Louis, Missouri. November 2–3, 2005. 

(7) Texas Air Control Board, Laboratory 

Division. 1976. ‘‘Determination of Particulate 

in Stack Gases Containing Sulfuric Acid and/ 

or Sulfur Dioxide.’’ Laboratory Methods for 

Determination of Air Pollutants. Modified 

December 3, 1976. 

(8) Puget Sound Air Pollution Control 

Agency, Engineering Division. 1983. 

‘‘Particulate Source Test Procedures Adopted 

by Puget Sound Air Pollution Control Agency 

Board of Directors.’’ Seattle, Washington. 

August 11, 1983. 

(9) U.S. Environmental Protection Agency, 

Federal Reference Methods 1 through 5 and 

Method 17, 40 CFR 60, appendix A–1 

through A–3 and A–6. 

(10) U.S. Environmental Protection 

Agency. 2008. ‘‘Evaluation and Improvement 

of Condensable PM Measurement,’’ EPA 

Contract No. EP–D–07–097, Work 

Assignment 2–03, October 2008. 

(11) U.S. Environmental Protection 

Agency. 2005. ‘‘Laboratory Evaluation of 

Method 202 to Determine Fate of SO2 in 

Impinger Water,’’ EPA Contract No. 68–D– 

02–061, Work Assignment 3–14, September 

30, 2005. 

(12) U.S. Environmental Protection 

Agency. 2010. Field valuation of an 

Improved Method for Sampling and Analysis 

of Filterable and Condensable Particulate 

Matter. Office of Air Quality Planning and 

Standards, Sector Policy and Program 

Division Monitoring Policy Group. Research 

Triangle Park, NC 27711. 

(13) Wisconsin Department of Natural 

Resources. 1988. Air Management Operations 

Handbook, Revision 3. January 11, 1988. 

18.0 Tables, Diagrams, Flowcharts, and 

Validation Data 

BILLING CODE 6560–50–P 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.061</GPH> ER21DE10.062</GPH>
80168 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.063</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80169 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.064</GPH>
80170 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

BILLING CODE 6560–50–C FIGURE 4—FIELD TRAIN RECOVERY

BLANK CONDENSABLE PARTICULATE

CALCULATIONS

Field Train Recovery Blank Condensable 

Particulate Calculations 

Plant 

FIGURE 4—FIELD TRAIN RECOVERY

BLANK CONDENSABLE PARTICULATE

CALCULATIONS—Continued 

Date 

Blank No. 

CPM Filter No. 


jlentini on DSKJ8SOYB1PROD with RULES2ER21DE10.065</GPH>
Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 80171 

FIGURE 4—FIELD TRAIN RECOVERY

BLANK CONDENSABLE PARTICULATE

CALCULATIONS—Continued 

Water volume added to purge train (Vp) ml 

Field Reagent Blank Massa

Water (Section 11.2.7) ............................ mg 

Acetone (Section 11.2.6) ........................ mg 

Hexane (Section 11.2.8) ......................... mg 

Field Train Recovery Blank Mass 

Mass of Organic CPM (mob) (Section 

11.2.3).

mg 

Mass of Inorganic CPM (mib) (Equation 

3).

mg 

FIGURE 4—FIELD TRAIN RECOVERY

BLANK CONDENSABLE PARTICULATE

CALCULATIONS—Continued 

Mass of the Field Train Recovery Blank 

(not to exceed 2.0 mg) (Equation 2).

mg 

aField reagent blanks are optional and intended to provide the testing contractor with 

information they can use to implement corrective actions, if necessary, to reduce the residual mass contribution from reagents used in 

the field. Field reagent blanks are not used to 

correct the CPM measurement results. 

FIGURE 5—OTHER FIELD TRAIN SAMPLE CONDENSABLE PARTICULATE

DATA

Other Field Train Sample Condensable 

Particulate Data 

Plant 

Date 

Run No. 

FIGURE 5—OTHER FIELD TRAIN SAMPLE CONDENSABLE PARTICULATE

DATA—Continued 

CPM Filter No. 

Water volume added to purge train (max 

50 ml) (Vp).

ml 

Date 

Run No. 

CPM Filter No. 

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 6—CPM WORK TABLE

Calculations for Recovery of Condensable PM (CPM) 

Plant 

Date 

Run No. 

Sample Preparation—CPM Containers No. 1 and 2 (Section 11.1): 

Was significant volume of water lost during transport? Yes or No ..............................

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

Estimate the volume lost during transport .............................. ml 

Plant 

Date 

Run No. 

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

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

Estimate the volume lost during transport. .............................. ml 

For Titration: 

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

Volume of titrant (Vt) (Section 11.2.2.2) .............................. ml 

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

For CPM Blank Weights: 

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

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

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

For CPM Train Weights: 

Mass of Organic CPM (mo) (Section 11.2.3) .............................. mg 

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

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

BILLING CODE 6560–50–P 


jlentini on DSKJ8SOYB1PROD with RULES2
80172 Federal Register / Vol. 75, No. 244 / Tuesday, December 21, 2010 / Rules and Regulations 

[FR Doc. 2010–30847 Filed 12–20–10; 8:45 am] 

BILLING CODE 6560–50–C 


jlentini on DSKJ8SOYB1PROD with RULES2er21de10.066</GPH>