76642 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

B. Revising paragraph (a) to read as 

follows:

§ 663.21 What criteria does the Secretary 

use to evaluate an application for a 

fellowship? 

(a) General. The Secretary evaluates 

an application for a fellowship on the 

basis of the criteria in this section. The 

Secretary informs applicants of the 

maximum possible score for each 

criterion in the application package or 

in a notice published in the Federal 

Register.

* * * * *

PART 664—FULBRIGHT-HAYS GROUP 

PROJECTS ABROAD FELLOWSHIP 

PROGRAM 

44. The authority citation for part 664 

continues to read as follows:

Authority: 22 U.S.C. 2452(b)(6), unless 

otherwise noted.

45. Section 664.30 is amended by—

A. Revising paragraph (a); 

B. Removing paragraph (b); and 

C. Redesignating paragraphs (c) and 

(d) as paragraphs (b) and (c), 

respectively. 

The revision reads as follows:

§ 664.30 How does the Secretary evaluate 

an application? 

(a) The Secretary evaluates an 

application for a Group Project Abroad 

on the basis of the criteria in § 664.31. 

The Secretary informs applicants of the 

maximum possible score for each 

criterion in the application package or 

in a notice published in the Federal 

Register.

* * * * *

46. Section 664.31 is amended by—

A. Removing all of the parentheticals 

that end in ‘‘points).’’ and removing the 

parenthetical that ends in ‘‘points)’’; and 

B. Revising the introductory text to 

read as follows:

§ 664.31 What selection criteria does the 

Secretary use? 

The Secretary uses the criteria in this 

section to evaluate applications for the 

purpose of recommending to the J. 

William Fulbright Foreign Scholarship 

Board Group Projects Abroad for 

funding under this part.

* * * * *

PART 669—LANGUAGE RESOURCE 

CENTERS PROGRAM 

47. The authority citation for part 669 

continues to read as follows:

Authority: 20 U.S.C. 1123, unless 

otherwise noted.

48. Section 669.20 is revised to read 

as follows:

§ 669.20 How does the Secretary evaluate 

an application? 

The Secretary evaluates an 

application for an award on the basis of 

the criteria contained in §§ 669.21 and 

669.22. The Secretary informs 

applicants of the maximum possible 

score for each criterion in the 

application package or in a notice 

published in the Federal Register.

(Authority: 20 U.S.C. 1123.)

49. Section 669.21 is amended by—

A. Removing all of the parentheticals 

that end in ‘‘points)’’; 

B. In paragraph (c), removing the 

symbol ‘‘§ ’’; and 

C. Revising the introductory text to 

read as follows:

§ 669.21 What selection criteria does the 

Secretary use? 

The Secretary evaluates an 

application on the basis of the criteria 

in this section.

* * * * *

[FR Doc. 04–28021 Filed 12–21–04; 8:45 am] 

BILLING CODE 4000–01–P

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 63 

[OAR–2004–0080, FRL–7851–9] 

RIN 2060–AF00 

National Emission Standards for 

Hazardous Air Pollutants: Appendix 

A—Test Methods; Method 301 for the 

Field Validation of Pollutant 

Measurement Methods From Various 

Waste Media

AGENCY: Environmental Protection 

Agency (EPA).

ACTION: Proposed rule.

SUMMARY: This action proposes to 

amend procedures for validating 

alternative emissions test methods, to 

rewrite the EPA’s Method 301 in plain 

language, reorganize the method for 

clarity, correct technical errors, and 

revise the technical procedures. The 

revisions to the technical procedures 

include replacing quantitation limits 

with detection limits, revising the bias 

acceptance criteria and eliminating the 

correction factors, revising the precision 

acceptance criteria, and allowing 

analyte spiking as an option even when 

there is an existing test method.

DATES: Comments. Comments must be 

received on or before February 22, 2005. 

Public Hearing. If anyone contacts the 

EPA requesting a public hearing by 

January 11, 2005, a public hearing will 

be held on January 21, 2005.

ADDRESSES: Comments. Submit your 

comments, identified by Docket ID No. 

OAR–2004–0080, by one of the 

following methods. 

• Federal eRulemaking Portal: http://

/www.regulations.gov. Follow the online instructions for submitting 

comments. 

• Agency Web site: http://

www.epa.gov/edocket. EDOCKET, EPA’s 

electronic public docket and comment 

system, is EPA’s preferred method for 

receiving comments. Follow the on-line 

instructions for submitting comments. 

• Mail: Air and Radiation Docket and 

Information Center (Mail Code 6102T), 

Attention Docket Number OAR–2004–

0080, Room B108, U.S. EPA, 1301 

Constitution Avenue, NW., Washington, 

DC 20460. The EPA requests that a 

separate copy also be sent to the contact 

person listed below (see FOR FURTHER

INFORMATION CONTACT). Send 

submissions containing such 

proprietary or confidential business 

information (CBI) directly to the 

following address, and not to the public 

docket, to ensure that proprietary or CBI 

is not inadvertently placed in the public 

docket: Attention: Mr. Roberto Morales, 

U.S. Environmental Protection Agency, 

OAQPS Document Control Officer, 109 

TW Alexander Drive, Room C404–02, 

RTP, NC, 27711. 

• Hand Delivery: Air and Radiation 

Docket and Information Center (Mail 

Code 6102T), Attention Docket Number 

OAR–2004–0080, Room B102, U.S. EPA, 

1301 Constitution Avenue, NW., 

Washington, DC 20460. Such deliveries 

are only accepted during the Docket’s 

normal hours of operation, and special 

arrangements should be made for 

deliveries of boxed information. The 

EPA requests a separate copy also be 

sent to the contact person listed below 

(see FOR FURTHER INFORMATION CONTACT). 

Instructions. Direct your comments to 

Docket ID No. OAR–2004–0080. The 

EPA’s policy is that all comments 

received will be included in the public 

docket without change and may be 

made available online at http://

www.epa.gov/edocket, including any 

personal information provided, unless 

the comment includes information 

claimed to be Confidential Business 

Information (CBI) or other information 

whose disclosure is restricted by statute. 

Do not submit information that you 

consider to be CBI or otherwise 

protected through EDOCKET, 

regulations.gov Web sites, or e-mail. The 

EPA EDOCKET and the Federal 

regulations.gov Web sites are 

‘‘anonymous access’’ systems, which 

means the EPA will not know your 

identity or contact information unless 

you provide it in the body of your 

Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 76643

comment. If you send an e-mail 

comment directly to the EPA without 

going through EDOCKET OR 

regulations.gov, your e-mail address 

will be automatically captured and 

included as part of the comment that is 

placed in the public docket and made 

available on the Internet. If you submit 

an electronic comment, the EPA 

recommends that you include your 

name and other contact information in 

the body of your comment and with any 

disk or CD–ROM you submit. If the EPA 

cannot read your comment due to 

technical difficulties and cannot contact 

you for clarification, the EPA may not 

be able to consider your comment. 

Electronic files should avoid the use of 

special characters, any form of 

encryption, and be free of any defects or 

viruses. For additional information 

about EPA’s public docket visit 

EDOCKET on-line or see the Federal 

Register of May 31, 2002 (67 FR 38102). 

Docket. All documents in the docket 

are listed in the EDOCKET index at 

http://www.epa.gov/edocket. Although 

listed in the index, some information is 

not publicly available, i.e., CBI or other 

information whose disclosure is 

restricted by statute. Certain other 

material, such as copyrighted material, 

is not placed on the Internet and will be 

publicly available only in hardcopy 

form. Publicly available docket 

materials are available either 

electronically in EDOCKET or in hard 

copy at the EPA Docket Center (Air 

Docket), EPA West, Room B–108, 1301 

Constitution Avenue, NW., Washington, 

DC 20004. The Docket Center is open 

from 8:30 a.m. to 4:30 p.m., Monday 

through Friday, excluding legal 

holidays. The telephone number for the 

Public Reading Room is (202) 566–1744, 

and the telephone number for the Air 

Docket is (202) 566–1742. 

Public Hearing. People interested in 

presenting oral testimony or inquiring 

as to whether a hearing is to be held 

should contact Ms. Corlis McCormick, 

Source Measurement Technology 

Group, Emission Measurement Center 

(D243–02), U.S. Environmental 

Protection Agency, Research Triangle 

Park, NC 27711, telephone number: 

(919) 541–5545, at least 2 days in 

advance of the public hearing. People 

interested in attending the public 

hearing must also call Ms. McCormick 

to verify the time, date, and location of 

the hearing. The public hearing will 

provide interested parties the 

opportunity to present data, views, or 

arguments concerning the proposed 

changes to Method 301. If a public 

hearing is held, it will be held at 10 a.m. 

in the EPA’s Auditorium in Research 

Triangle Park, North Carolina, or at an 

alternate site nearby.

FOR FURTHER INFORMATION CONTACT: For 

information concerning the proposed 

standards, contact Mr. Gary McAlister, 

Source Measurement Technology 

Group, Emission Measurement Center 

(D243–02), U.S. Environmental 

Protection Agency, Research Triangle 

Park, North Carolina 27711, telephone 

number: (919) 541–1062, electronic mail 

address: mcalister.gary@epa.gov.

SUPPLEMENTARY INFORMATION:

Preamble Outline 

The information in this preamble is 

organized as follows.

I. General Information 

A. Does This Action Apply to Me? 

B. What Should I Consider as I Prepare My 

Comments for the EPA? 

C. Availability of the Proposed Rule 

II. Introduction 

III. What Changes Are We Proposing? 

A. Use Plain Language 

B. Reorganize Method 301 

C. Correct Technical Errors 

D. Make Technical Revisions 

IV. What Are the Administrative 

Requirements? 

A. Executive Order 12866—Regulatory 

Planning and Review 

B. Paperwork Reduction Act 

C. Regulatory Flexibility Act (RFA) 

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 

Risks 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 of 1995

I. General Information 

A. Does This Action Apply to Me? 

Method 301 affects/applies to you if 

you want to propose a test method to 

meet an EPA requirement in absence of 

a validated method. 

B. What Should I Consider as I Prepare 

My Comments for the EPA? 

1. Submitting CBI. Do not submit this 

information to the EPA through 

EDOCKET, regulations.gov, or e-mail. 

Clearly mark the part or all of the 

information that you claim to be CBI. 

For CBI information in a disk or CD 

ROM that you mail to the EPA, mark the 

outside of the disk or CD ROM as CBI 

and then identify electronically within 

the disk or CD ROM the specific 

information that is claimed as CBI. In 

addition to one complete version of the 

comment that includes information 

claimed as CBI, a copy of the comment 

that does not contain the information 

claimed as CBI must be submitted for 

inclusion in the public docket. 

Information so marked will not be 

disclosed except in accordance with 

procedures set forth in 40 CFR part 2. 

2. Tips for Preparing Your Comments.

When submitting comments, remember 

to: 

i. Identify the rulemaking by docket 

number and other identifying 

information (e.g., subject heading, 

Federal Register proposal publication 

date and reference page number(s)). 

ii. Follow directions.—The EPA may 

ask you to respond to specific questions 

or organize comments by referencing a 

Code of Federal Regulations (CFR) part 

or section number. 

iii. Explain why you agree or disagree; 

suggest alternatives and provide 

substitute language for your requested 

changes. 

iv. Describe any assumptions and 

provide any technical information and/

or data that you used. 

v. If you estimate potential costs or 

burdens, explain how you arrived at 

your estimate in sufficient detail to 

allow for it to be reproduced. 

vi. Provide specific examples to 

illustrate your concerns, and suggest 

alternatives. 

vii. Explain your views as clearly as 

possible, avoiding the use of profanity 

or personal threats. 

viii. Make sure to submit your 

comments by the specified comment 

period deadline. 

Commenters wishing to submit 

proprietary information for 

consideration must clearly distinguish 

such information from other comments 

and clearly label it as CBI. Send 

submissions containing such 

proprietary information directly to the 

following address, and not to the public 

docket, to ensure that proprietary 

information is not inadvertently placed 

in the docket: Attention: Mr. Roberto 

Morales, U.S. Environmental Protection 

Agency, OAQPS Document Control 

Officer, 109 TW Alexander Drive, Room 

C404–02, RTP, NC 27711. The EPA will 

disclose information identified as CBI 

only to the extent allowed by the 

procedures set forth in 40 CFR part 2. 

If no claim of confidentiality 

accompanies a submission when it is 

received by the EPA, the information 

may be made available to the public 

without further notice to the 

commenter. 

C. Availability of the Proposed Rule 

In addition to being available in the 

docket, an electronic copy of the 

proposed changes to Method 301 is also

76644 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

available on the Internet through the 

Technology Transfer Network (TTN). 

Following signature, a copy of Method 

301 will be posted on the TTN’s policy 

and guidance page for newly proposed 

or promulgated rules http://

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

provides information and technology 

exchange in various areas of air 

pollution control. If more information 

regarding the TTN is needed, call the 

TTN HELP line at (919) 541–5384. 

II. Introduction 

Today’s action proposes to amend 

EPA’s Method 301; Field Validation of 

Pollutant Measurement Methods from 

Various Waste Media. Method 301 can 

be found in Appendix A of 40 CFR part 

63 (Test Methods). Method 301 was 

promulgated with 40 CFR part 63 

subpart D (Regulations Governing 

Compliance Extensions for Early 

Reductions of Hazardous Air Pollutants) 

(58 FR 27338, June 13, 1991) pursuant 

to section 112 of the Clean Air Act (as 

amended in 1990). You would use 

Method 301 whenever you propose to 

use a test method to meet an EPA 

requirement in absence of a validated 

method. The method specifies 

procedures for determining and 

documenting the precision and bias of 

measured concentrations from various 

media (e.g., sludge, exhaust gas, 

wastewater) at the level of an applicable 

standard for a source. Bias (or systemic 

error) is established by comparing your 

proposed method against a reference 

value. A correction factor is employed 

to eliminate/minimize bias. This 

correction factor is established from 

data obtained during your validation 

test. Methods that have bias correction 

factors outside a specified range are 

considered unacceptable. Method 

precision (or random error) at the level 

of the standard must be demonstrated to 

be as precise as the validated method for 

acceptance. 

Today’s action proposes to amend 

those provisions by correcting technical 

errors, and simplifying and clarifying 

procedures. Section II of this preamble 

discusses the proposed Method 301 

rule, and section III presents the 

administrative requirements for this 

action.

III. What Changes Are We Proposing? 

A. Use Plain Language 

In compliance with President 

Clinton’s June 1, 1998, Executive 

Memorandum on Plain Language in 

government writing, Method 301 has 

been rewritten in plain language. The 

use of plain language clarifies the 

requirements of Method 301, thus, 

reducing the burden (time) associated 

with understanding the Method. When 

Method 301 refers to ‘‘you,’’ it means 

the owner or operator of the affected 

source. 

B. Reorganize Method 301 

We have reorganized the information 

in Method 301 to make it easier to 

follow the requirements and to 

understand the relationships among the 

various requirements. The 

reorganization did not create new 

requirements, but it does incorporate 

various corrections to technical errors 

and technical revisions. These 

corrections and revisions, as well as the 

rationale for the changes, are discussed 

in sections III C and D of this preamble. 

Section 17.0 of today’s rule (What 

detection limits must I use?) shall apply 

instead of section 9.0 (Practical 

Quantitation Limits) of the promulgated 

Method 301 rule. We have retained all 

other sections from the promulgated 

Method 301, but you will find them in 

new places. Where necessary for clarity, 

we have put the information from one 

section of Promulgated Method 301 into 

several new sections. Some information 

has been put into tables at the end of the 

Method. Section 2.0 presents new 

information. It has been added to 

explain when you must use Method 301 

and to identify the requirement for 

receiving written approval from the 

Administrator before using the 

alternative test method. Table 1 of this 

preamble specifies where the sections in 

the promulgated Method 301 are found 

in the proposed Method 301 rule. 

The equations of the promulgated 

Method 301 have also been amended. 

Some of the promulgated equations 

have been modified; some have been 

replaced by other equations, and some 

have simply been renumbered or 

reordered. The technical reasons for the 

changes to the equations are discussed 

in section III. D of this preamble. Table 

2 indicates whether each equation in the 

proposed amended rule has changed 

from the promulgated rule. Equations 

301–5 and 301–10 (correction factors 

when using isotopic spiking and paired 

sampling systems with a validated test 

method comparison) of promulgated 

Method 301 rule have been removed for 

the reasons discussed in section III D of 

this preamble.

TABLE 1.—COMPARISON OF SECTIONS IN PROPOSED METHOD 301 TO THOSE IN PROMULGATED METHOD 301 

Proposed new section Promulgated method section 

Using Method 301

1.0 What is the purpose of Method 301? .............................................. 1.1 Applicability. 

2.0 When must I use Method 301? ........................................................ None. 

3.0 What does Method 301 include? ..................................................... 1.1.2. 

4.0 How do I perform Method 301? ....................................................... 1.2 Principle.

Reference Materials and Performance Audits

5.0 What reference materials must I use? ............................................. 3.0 Reference Materials. 

6.0 How do I conduct the performance audit? ....................................... 4.0 EPA Performance Audit Materials. 

Sampling Procedures

7.0 What sampling procedures must I use? .......................................... 5.0 Procedure for Determination of Bias and Precision in the Field. 

8.0 How do I ensure sample stability? ................................................... 8 Procedure for Sample Stability in Bias and Precision Evaluations. 

Bias and Precision

9.0 What are the requirements for bias? ............................................... 1.2.1 Bias. 

10.0 What are the requirements for precision? ..................................... 1.2.2 Precision. 

11.0 What calculations must I perform for isotopic sampling? 6.1 Isotopic Sampling. 

Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 76645

TABLE 1.—COMPARISON OF SECTIONS IN PROPOSED METHOD 301 TO THOSE IN PROMULGATED METHOD 301—

Continued

Proposed new section Promulgated method section 

12.0 What calculations must I perform for comparison with a validated 

method if I am using paired sampling systems? 

6.2.1 Comparison with a validated method: Paired Sampling Systems. 

13.0 What calculations must I perform for comparison with a validated 

method if I am using quadruplet replicate sampling systems? 

6.2.2 Comparison with a validated method: Quadruplet Replicate 

Sampling Systems. 

14.0 What calculations must I perform for analyte spiking? 6.3 Analyte Spiking. 

15.0 How do I conduct followup tests? .................................................. 11 Followup Testing. 

Optional Requirements

16.0 How do I use and conduct ruggedness testing? 7 Ruggedness Testing. 

17.0 What detection limits must I use? 9 Practical Limit of Quantitation. 

Other Requirements and Information

18.0 How do I apply for approval to use an alternative method? 10 Field Validation Report Requirements. 

19.0 How do I request a waiver? ........................................................... 1.1.1 and 12 Procedure for Obtaining a Waiver. 

20.0 What definitions apply to this method? .......................................... 12 Definitions. 

21.0 Where can I find additional information? ....................................... 13 Bibliography. 

TABLE 2.—EQUATIONS IN PROPOSED METHOD 301 

The following equation in proposed method 301 . . . is . . . 

The following equation in 

promulgated method 

301 . . . 

301–1 Difference in Sample Results .......................................................................... New.

301–7 Relative Magnitude of Bias .............................................................................. New.

301–9 Relative Magnitude of Bias for Comparing Against Validated Methods Using 

Paired Sampling Systems.

New.

Equations When Using Isotopic Spiking

301–4 Numerical Value of Bias .................................................................................. A revision of ....................... 301–1. 

301–5 Standard Deviation ........................................................................................... The same as ...................... 301–2. 

301–6 t Test ................................................................................................................ A replacement for ............... 301–3 and 301–4. 

301–8 Relative Standard Deviation ............................................................................ A revision of ....................... 301–6. 

Equations When Comparing Against Validated Method Using Paired Sampling Systems

301–2 Standard Deviation ........................................................................................... For paired sampling systems, a replacement for.301–2. 

301–3 t Test ................................................................................................................ The same as ...................... 301–9. 

301–10 Variance ......................................................................................................... A replacement for ............... 301–7. 

301–11 Pooled Variance ............................................................................................. New.

301–12 Alternative Test Method Variance .................................................................. A replacement for ............... 301–9a. 

301–13 F test .............................................................................................................. The same as ...................... 301–8. 

Equations When Comparing Against Validated Method Using Quadruplet Replicate Sampling Systems

301–14 Bias ................................................................................................................ The same as ...................... 301–12. 

301–15 Alternative Test Method Variance .................................................................. The same as ...................... 301–11. 

Equations When Using Analyte Spiking

301–16 Bias ................................................................................................................ The same as ...................... 301–14. 

301–17 t Test .............................................................................................................. A replacement for ............... 301–4. 

301–18 Standard Deviation for Spiked Samples ........................................................ A revision of ....................... 301–13 

301–19 Standard Deviation for Unspiked Samples .................................................... A replacement for ............... 301–13 and 301–6. 

301–20 F test .............................................................................................................. New.

301–21 Pooled Standard Deviation ............................................................................ A replacement for ............... 301–15. 

C. Correct Technical Errors 

Some of the equations in promulgated 

Method 301 are incorrect. We are 

proposing to correct these equations 

with today’s action. For a discussion of 

new equations due to technical 

revisions, see section III D of this 

preamble. We revised several equations 

to clarify their intent. Under the new 

numbering system, the revised 

equations are 301–4 (numerical value of 

bias), 301–6 (t Test), 301–8 (relative 

standard deviation), 301–18 (standard 

deviation for spiked samples), and 301–

19 (standard deviation for unspiked 

samples). These changes were editorial/

defining changes and not technical 

changes. For example, we added or 

changed subscripts or redefined a 

variable.

76646 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

We added Equations 301–1, 301–7, 

and 301–9. Equation 301–1 is used to 

calculate the difference in minimum 

and maximum storage times under the 

new sample stability procedures. 

Equation 301–7 is used to calculate 

relative magnitude of bias for isotopic 

spiking. This new equation was needed 

when we dropped the use of correction 

factors. Likewise, Equation 301–9 was 

needed for calculating relative 

magnitude of bias when comparing 

against a validated method using paired 

sampling systems. 

We also added Equation 301–11 and 

changed Equations 301–12, 301–17, 

301–18, and 301–19 to correct technical 

errors in promulgated Method 301. 

Equations 301–11 (Pooled Variance) and 

301–12 (Alternative Test Method 

Variance) are being proposed to correct 

a technical error in the promulgated 

method. Addition and subtraction can 

only be performed on the variance. It 

cannot be performed on the standard 

deviation. The proposed Equation 301–

11 is a new equation that calculates the 

pooled variance of both methods when 

comparing against validated methods 

using paired sampling systems. The 

proposed Equation 301–12 replaces the 

standard deviation with the variance. 

Equations 301–17 (calculation of the 

test ‘‘t-statistic’’) and 301–21 

(calculation of the pooled standard 

deviation) were changed because the 

divisor was wrong. Equation 301–20 (F 

test) was added so that the tester could 

determine if the spiked and unspiked 

samples had the same precision, thereby 

allowing them to be pooled to calculate 

the overall precision. 

The proposed Equation 301–2 

(Standard Deviation) replaces the 

promulgated Equation 301–2 when 

comparing against validated methods 

using paired sampling systems. The text 

in promulgated 6.2.1.4 directs the 

analyst to determine the mean of the 

paired sample differences by 

substituting dm (mean of the paired 

sample differences) and di (standard 

deviation of the differences) for Si and 

Sm in the proposed Equation 301–2. We 

created the proposed Equation 301–2 to 

incorporate these changes. 

D. Make Technical Revisions 

We are proposing five major technical 

changes to Method 301. These technical 

changes include the following: 

(1) Replacing the Practical Limit of 

Quantitation (PLQ) with a procedure to 

determine the Limit of Detection, 

(2) Revising the bias acceptance 

criteria and eliminating correction 

factors, 

(3) Revising precision acceptance 

criteria when using analyte spiking, 

(4) Allowing analyte spiking even 

when there is an existing test method, 

and 

(5) Establishing new procedures for 

ensuring sample stability. 

1. Practical Limit of Quantitation. We 

are proposing to replace the 

determination of the PLQ with a 

procedure to determine the Limit of 

detection (LOD). The purpose of 

establishing a measurement limit is to 

ensure that a test method is appropriate 

for its intended use. The LOD is a better 

parameter for this purpose. 

The PLQ is defined as the level or 

concentration at which the precision of 

a test method reaches an acceptable 

value. There are several problems with 

this concept. The first is the idea that 

there is an absolute value for acceptable 

precision. To a certain extent, a tester 

can compensate for imprecision by 

collecting additional data so there is no 

absolute level at which the imprecision 

of a test method becomes so great that 

the method is no longer useful. This 

concept works best when the precision 

of the test method is independent of the 

concentration of the analyte being 

measured. As the concentration of the 

analyte increases, the imprecision of the 

method as a percentage of the measured 

quantity decreases. In this case, the 

relative imprecision will actually 

decrease as the quantity measured 

increases. 

However, for most environmental 

measurements, it appears that the 

precision is a function of the 

concentration of the analyte being 

measured. Thus, the relative 

imprecision will not decrease as the 

quantity measured increases. In this 

case, the PLQ has no meaning. 

The LOD is the minimum level or 

concentration of an analyte that 

produces a signal or response that is 

distinguishable from the signal or 

response produced when no analyte is 

present. This is a measurable quantity 

that can be determined regardless of the 

method’s precision or whether that 

precision varies with the level of the 

analyte. For all of these reasons, we 

believe that the LOD is a more useful 

parameter to characterize a test 

method’s performance. 

2. Bias Acceptance Criteria. We are 

also proposing to change the acceptance 

criteria for the bias in a proposed 

alternative method from ± 30% to ±

10% and concurrently to eliminate the 

requirement for correcting all data 

collected with the method. We believe 

that twelve pairs of results from a single 

source are not sufficient to allow us to 

establish a correction factor that can or 

should be applied to all future uses of 

the method. In addition, keeping track 

of correction factors to ensure that they 

are applied to future uses of the method 

is a huge administrative burden both for 

the users of the method and the 

regulatory agencies who oversee its use. 

If we do not use correction factors, 

method biases of up to 30 percent are 

undesirably large. Therefore, we are 

proposing to reduce the acceptable bias 

to + 10% and eliminate the requirement 

to correct the data. With this change, the 

bias of alternative methods will be 

acceptable; the criteria for using the 

alternative test method at similar 

sources will be clear, and the 

administrative burden will be reduced. 

3. Precision Acceptance Criteria. We 

are proposing to change the acceptance 

criteria for method precision when 

using analyte spiking from ± 50% to ±

20%. In addition, we are proposing to 

eliminate the requirement for different 

numbers of replicate samples depending 

on the method’s relative precision. All 

future testing using an alternative test 

method at similar sources will require 

only three replicate samples. The 

requirement in the existing procedure 

was an attempt to compensate for the 

poorer precision of some candidate 

alternative test methods by increasing 

the amount of data that the user was 

required to collect. While more data 

does compensate for the imprecision of 

any future data collected with the 

method, allowing candidate alternative 

test methods with poor precision creates 

other problems. One problem is that 

poor precision makes it more difficult to 

detect potential bias in a test method. 

For this reason, we are proposing to 

tighten the acceptance criteria for the 

precision of candidate alternative test 

methods.

4. Analyte Spiking. We are also 

proposing to allow the tester to use 

analyte spiking to evaluate an 

alternative test method even when there 

is an existing compliance test method. 

If the NESHAP specifies a test method, 

promulgated Method 301 requires the 

tester to evaluate an alternative method 

by direct comparison. We believe that 

this is too restrictive in some cases. For 

example, a change in process 

technology may cause a previously 

unbiased test method to develop an 

interference that biases its results. If the 

tester is required to compare the 

alternative test method to the existing 

test method, the alternative method 

could never demonstrate acceptable 

performance if it were unbiased. We 

believe that it is sufficient for an 

alternative method to demonstrate 

acceptable performance by using the 

analyte spiking procedure and that this 

is a reasonable alternative to direct 

comparison. 

Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 76647

5. Sample Stability. Finally, we are 

proposing procedures for sample 

stability. Method 301 previously lacked 

specific procedures for ensuring that 

samples collected under proposed 

alternative methods were analyzed 

within an appropriate time. New 

Section 8.4 includes a requirement to 

calculate the difference in the sampling 

results at the minimum and maximum 

storage times, determine the standard 

deviation of the differences, and test the 

difference in the results for statistical 

significance by calculating the t-statistic 

and determining if the mean of the 

differences between the initial results 

and the results after storage is 

significant at the 95 percent confidence 

level. We have also added Table 1 to 

compare the calculated t-statistic with 

the critical value of the t-statistic. These 

procedures are necessary to ensure 

sample stability and should have been 

included in promulgated Method 301. 

IV. What Are the Administrative 

Requirements? 

A. Executive Order 12866—Regulatory 

Planning and Review 

Under Executive Order 12866 (58 FR 

51735, October 4, 1993), the EPA must 

determine whether the regulatory action 

is ‘‘significant’’ and, therefore, subject to 

review by the Office of Management and 

Budget (OMB) and the requirements of 

the Executive Order. The Executive 

Order defines ‘‘significant regulatory 

action’’ as one that is likely to result in 

a rule that may: 

(1) Have an annual effect on the 

economy of $100 million or more or 

adversely affect in a material way the 

economy, a sector of the economy, 

productivity, competition, jobs, the 

environment, public health or safety, or 

State, local, or tribal governments or 

communities; 

(2) Create a serious inconsistency or 

otherwise interfere with an action taken 

or planned by another agency; 

(3) Materially alter the budgetary 

impact of entitlements, grants, user fees, 

or loan programs, or the rights and 

obligation of recipients thereof; or 

(4) Raise novel legal or policy issues 

arising out of legal mandates, the 

President’s priorities, or the principles 

set forth in the Executive Order. 

It has been determined that this 

proposed regulatory action is not a 

‘‘significant regulatory action’’ under 

the terms of Executive Order 12866 and 

is, therefore, not subject to OMB review. 

B. Paperwork Reduction Act 

This action does not impose or change 

the information collection burden under 

the provisions of the Paperwork 

Reduction Act 44 U.S.C. 3501, et seq.

Burden means the total time, effort, or 

financial resources expended by persons 

to generate, maintain, retain, or disclose 

or provide information to or for a 

Federal agency. This includes the time 

needed to review instructions; develop, 

acquire, install, and utilize technology 

and systems for the purposes of 

collecting, validating, and verifying 

information, processing and 

maintaining information, and disclosing 

and providing information; adjust the 

existing ways to comply with any 

previously applicable instructions and 

requirements; train personnel to be able 

to respond to a collection of 

information; search data sources; 

complete and review the collection of 

information; and transmit or otherwise 

disclose the collection of information. 

An agency may not conduct or 

sponsor, and a person is not required to 

respond to a collection of information 

unless it displays a currently valid OMB 

control number. The OMB control 

numbers for EPA’s regulations are listed 

in 40 CFR part 9 and 48 CFR chapter 15. 

C. Regulatory Flexibility Act (RFA) 

The 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 the purposes of assessing the 

impacts of today’s proposed rule on 

small entities, small entity is defined as: 

(1) A small business that meets the 

definitions for small business based on 

the Small Business Association (SBA) 

size standards which, for this proposed 

action, are operations that have fewer 

than 1,000 employees; (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-forprofit enterprise which is independently 

owned and operated and is not 

dominant in its field.

After considering the economic 

impacts of today’s proposed rule on 

small entities, I certify that this 

proposed action will not have a 

significant economic impact on a 

substantial number of small entities. In 

determining whether a rule has 

significant economic impact on a 

substantial number of small entities, the 

impact of concern is any significant 

adverse economic impact on small 

entities since the primary purpose of the 

regulatory flexibility analysis is to 

identify and address regulatory 

alternatives ‘‘which minimize any 

significant economic impact of the 

proposed rule on small entities,’’ (5 

U.S.C. 603 and 604). Thus, an agency 

may certify that a rule will not have a 

significant economic impact on a 

substantial number of small entities if 

the rule relieves regulatory burden, or 

otherwise has a positive economic effect 

on all of the small entities subject to the 

rule. This proposed rule will not impose 

any requirements on small entities. This 

rule establishes procedures for using 

alternative methods. As such, small 

entities and other sources are not 

required to comply with this proposed 

rule, but may elect to use Method 301. 

The proposed rule offers additional 

flexibility to all sources, including small 

entities that may be subject to 

requirements under the CAA. 

Additionally, this proposed amended 

rule clarifies and simplifies the 

procedures for using alternative 

methods. We continue to be interested 

in the potential impacts of the proposed 

rule on small entities and welcome 

comments on issues related to such 

impacts. 

D. Unfunded Mandates Reform Act 

Title II of the Unfunded Mandates 

Reform Act of 1995 (UMRA), Public 

Law 1044, establishes requirements for 

Federal agencies to assess the effects of 

their regulatory actions on State, local, 

and tribal governments and the private 

sector. Under section 202 of the UMRA, 

the EPA generally must prepare a 

written statement, including cost-benefit 

analysis, for proposed and final rules 

with ‘‘Federal mandates’’ that may 

result in expenditures to State, local, 

and tribal governments, in the aggregate, 

or to the private sector, of $100 million 

or more in any one year. Before 

promulgating an EPA rule for which a 

written statement is needed, section 205 

of the UMRA generally requires the EPA 

to identify and consider a reasonable 

number of regulatory alternatives and 

adopt the least costly, most costeffective, or least burdensome 

alternative if the Administrator 

publishes with the final rule an 

explanation why that alternative was 

not adopted. Before EPA establishes any 

regulatory requirements that may 

significantly or uniquely affect small 

governments, including tribal 

governments, it must have developed 

under section 203 of the UMRA a small 

government agency plan. The plan must 

provide for notifying potentially 

affected small governments, enabling 

76648 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

official of affected small governments to 

have meaningful and timely input in the 

development of EPA regulatory 

proposals with significant Federal 

intergovernmental mandates, and 

informing, educating, and advising 

small governments on compliance with 

the regulatory requirements. 

We have determined that today’s 

proposed amended rule does not 

contain Federal mandates for State, 

local, or tribal governments or the 

private sector. Therefore, this proposed 

amended rule is not subject to the 

requirements of sections 202 and 205 of 

the UMRA. 

E. Executive Order 13132—Federalism 

Executive Order 13132, entitled 

‘‘Federalism’’ (64 FR 43255, August 10, 

1999), requires the EPA to develop an 

accountable process to ensure 

‘‘meaningful and timely input by State 

and local officials in the development of 

regulatory policies that have federalism 

implications.’’ ‘‘Policies that have 

federalism implications’’ is defined in 

the Executive Order to include 

regulations that have ‘‘substantial direct 

effects on the States, on the relationship 

between the National Government and 

the States, or on the distribution of 

power and responsibilities among the 

various levels of government.’’

Under Executive Order 13132, the 

EPA may not issue a regulation that has 

federalism implications, that imposes 

substantial direct compliance costs, and 

that is not required by statute, unless 

the Federal Government provides the 

funds necessary to pay the direct 

compliance costs incurred by State and 

local governments, or the EPA consults 

with State and local officials early in the 

process of developing the proposed 

regulation. The EPA also may not issue 

a regulation that has federalism 

implications and that preempts State 

law unless the Agency consults with 

State and local officials early in the 

process of developing the proposed 

regulation.

Today’s proposed amended rule will 

not have federalism implications. They 

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. 

Today’s proposed amended rule 

clarifies and simplifies the procedures 

for using alternative methods. Thus, the 

requirements of section 6 of the 

Executive Order do not apply. 

F. Executive Order 13175—Consultation 

and Coordination With Indian Tribal 

Governments 

Executive Order 13175, entitled 

‘‘Consultation and Coordination with 

Indian Tribal Governments’’ (65 FR 

67249, November 9, 2000), requires EPA 

to develop an accountable process to 

ensure ‘‘meaningful and timely input by 

tribal officials in the development of 

regulatory policies that have tribal 

implications.’’ The proposed amended 

rule does not have tribal implications, 

as specified in Executive Order 13175. 

The proposed action serves to clarify 

and simplify procedures for using 

alternative methods. Therefore, 

Executive Order 13175 does not apply 

to the proposed amended rule. 

G. Executive Order 13045—Protection of 

Children From Environmental Health 

Risks and Safety Risks 

Executive Order 13045, ‘‘Protection of 

Children from Environmental Health 

Risks and Safety Risks’’ (62 FR 19885, 

April 23, 1997), applies to any rule that 

the EPA determines is: (1) 

‘‘Economically significant’’ as defined 

under E.O. 12866; and (2) concerns an 

environmental health or safety risk that 

the EPA has reason to believe may have 

a disproportionate effect on children. If 

the regulatory action meets both criteria, 

the EPA must evaluate the 

environmental health or safety effects of 

the planned rule on children and 

explain why the planned regulation is 

preferable to other potentially effective 

and reasonable alternatives considered 

by the EPA. 

The EPA interprets Executive Order 

13045 as applying only to those 

regulatory actions that are based on 

health or safety risks, such that the 

analysis required under section 5–501 of 

the Executive Order has the potential to 

influence the regulation. The proposed 

amended rule is not subject to Executive 

Order 13045 because it is not 

economically significant as defined in 

Executive Order 12866, and because this 

proposed amended rule is not based on 

health or safety risks. Thus, Executive 

Order 13045 does not apply to this 

proposed amended rule. 

H. Executive Order 13211, Actions 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution, or Use 

This rule is not subject to Executive 

Order 13211, ‘‘Actions Concerning 

Regulations That Significantly Affect 

Energy Supply, Distribution, or Use’’ (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 of 1995 

Section 112(d) of the National 

Technology Transfer and Advancement 

Act of 1995 (NTTAA), Public Law No. 

104–113, section 12(d) 915 U.S.C. 272 

note), directs all Federal agencies to use 

voluntary consensus standards instead 

of government unique standards in their 

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, etc.) 

that are developed or adopted by one or 

more voluntary consensus standards 

bodies. Examples of organizations, 

generally regarded as voluntary 

consensus standards bodies, include the 

American Society for Testing and 

Materials (ASTM), the National Fire 

Protection Association (NFPA), and the 

Society of Automotive Engineers (SAE). 

The NTTAA requires Federal agencies 

like EPA to provide Congress through 

OMB with explanations when an agency 

decides not to use available and 

applicable voluntary consensus 

standards. This proposed amended rule 

clarifies and simplifies, already 

promulgated, procedures for use of 

alternative standards. The intent of the 

Method 301 is to allow owners and 

operators of sources regulated by Part 63 

standards the flexibility and option to 

use alternative standards. Today’s 

proposed amended rule is intended to 

simplify and clarify the procedures for 

using alternative standards. Therefore, 

the EPA is not considering the use of 

any voluntary consensus standards with 

today’s proposed action.

List of Subjects in 40 CFR Part 63 

Environmental protection, Alternative 

test method, Air pollution control, Field 

validation, Hazardous air pollutants.

Dated: December 16, 2004. 

Michael O. Leavitt, 

Administrator.

For the reasons stated in the 

preamble, title 40, chapter I, part 63, of 

the Code of the Federal Regulations is 

proposed to be amended as follows:

PART 63—[AMENDED] 

1. The authority citation for part 63 

continues to read as follows:

Authority: 42 U.S.C. 7401, et seq.

2. Appendix A is amended by revising 

Method 301 to read as follows:

Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 76649

Appendix A to Part 63—Test Methods 

Method 301—Field Validation of Pollutant 

Measurement Methods From Various Waste 

Media

Sec. 

Using Method 301 

1.0 What Is the Purpose of Method 301? 

2.0 When Must I Use Method 301? 

3.0 What Does Method 301 Include? 

4.0 How Do I Perform Method 301? 

Reference Materials and Performance Audits 

5.0 What Reference Materials Must I Use? 

6.0 How do I conduct the performance 

audit? 

Sampling Procedures 

7.0 What Sampling Procedures Must I Use? 

8.0 How Do I Ensure Sample Stability? 

Bias and Precision 

9.0 What Are the Requirements for Bias? 

10.0 What Are the Requirements for 

Precision? 

11.0 What Calculations Must I Perform for 

Isotopic Spiking? 

12.0 What Calculations Must I Perform for 

Comparison With a Validated Method If 

I Am Using Paired Sampling Systems? 

13.0 What Calculations Must I Perform for 

Comparison With a Validated Method If 

I Am Using Quadruplet Replicate 

Sampling Systems? 

14.0 What Calculations Must I Perform for 

Analyte Spiking? 

15.0 How Do I Conduct Tests at Similar 

Sources? 

Optional Requirements 

16.0 How Do I Use and Conduct 

Ruggedness Testing? 

17.0 What Detection Limits Must I Use? 

Other Requirements and Information 

18.0 How Do I Apply for Approval To Use 

an Alternative Test Method? 

19.0 How Do I Request a Waiver? 

20.0 What Definitions Apply to This 

Method? 

21.0 Where Can I Find Additional 

Information? 

Using Method 301 

1.0 What Is the Purpose of Method 301? 

This method describes the minimum 

procedures that you, the owner or operator of 

an affected source subject to requirements 

under 40 CFR part 63, must use to validate 

an alternative test method to a test method 

required in 40 CFR part 63. 

2.0 When Must I Use Method 301? 

If you want to request to use an alternative 

test method to meet requirements in a 

subpart of 40 CFR part 63, you must use 

Method 301 to validate the alternative test 

method. You must request approval to use 

the alternative test method according to the 

procedures in section 18 and § 63.7(f). You 

must receive the Administrator’s written 

approval to use the alternative test method 

before you use the alternative test method to 

meet requirements under 40 CFR part 63. In 

some cases, the Administrator may decide to 

waive the requirement to use Method 301. 

Section 19 describes the requirements for 

obtaining a waiver. 

3.0 What Does Method 301 Include? 

This method includes minimum 

procedures to determine and document 

systematic error (bias) and random error 

(precision) of measured concentrations from 

exhaust gases, wastewater, sludge, and other 

media. It contains procedures for ensuring 

sample stability if such procedures are not 

included in the test method. This method 

also includes optional procedures for 

ruggedness and detection limits. 

4.0 How Do I Perform Method 301? 

First, you introduce a known concentration 

of an analyte or compare the alternative test 

method against a validated test method to 

determine the alternative test method’s bias. 

Then, you collect multiple, collocated 

simultaneous samples to determine the 

alternative test method’s precision. Sections 

5.0 through 17.0 describe these procedures in 

detail. 

Reference Materials and Performance Audits 

5.0 What Reference Materials Must I Use? 

You must use reference materials (that is, 

analytes) at the level of the applicable 

emission limitation or standard that the 

subpart in 40 CFR part 63 requires. If you 

want to expand the applicable range of the 

method, you must conduct additional runs 

with higher and lower analyte 

concentrations. The additional runs must be 

conducted according to the ruggedness 

procedures in 16.0. You must use the 

analytes according to the procedures in 5.1 

through 5.4. 

5.1 Exhaust Gas Tests. You must get a 

known concentration of each analyte from an 

independent source such as a speciality gas 

manufacturer, specialty chemical company, 

or chemical laboratory. You must also get the 

manufacturer’s stability data for the analyte 

concentration and recommendations for 

recertification. 

5.2 Tests for Other Waste Media. You 

must get the pure liquid components of each 

analyte from an independent manufacturer. 

The manufacturer must certify the purity and 

shelf life of the pure liquid components. You 

must dilute the pure liquid components in 

the same type medium as the waste from the 

affected source. You must verify the accuracy 

of the concentration of each diluted analyte 

by comparing its response to the pure liquid 

components. 

5.3 Surrogate Analytes. If you 

demonstrate to the Administrator’s 

satisfaction that a surrogate compound 

behaves as the analyte does, then you may 

use surrogate compounds for highly toxic or 

reactive compounds. A surrogate may be an 

isotope or one that contains a unique element 

(for example, chlorine) that is not present in 

the source or a derivation of the toxic or 

reactive compound, if the derivative 

formation is part of the method’s procedure. 

You may use laboratory experiments or 

literature data to show behavioral 

acceptability. 

5.4 Isotopically Labeled Materials.

Isotope mixtures may contain the isotope and 

the natural analyte. The isotope labeled 

analyte concentration must be more than five 

times the natural concentration of the 

analyte. 

6.0 How Do I Conduct the Performance 

Audit? 

6.1 Getting Performance Audit Material.

If EPA has performance audit material for the 

analytes that you are testing, you must use 

it to assess method bias. You can get a list 

of performance audit materials at http://

www.epa.gov/ttn/emc/email.html#audit or by 

contacting EMC at (919) 541–5545. You must 

request the performance audit material at 

least 30 days before the validation test.

6.2 Sampling and Analyzing Performance 

Audit Material. You must sample and 

analyze the performance audit material three 

times according to the instructions provided 

with the audit sample. You must submit the 

three results with the field validation report. 

Although there are no acceptance criteria for 

these performance audit results, you and the 

Administrator may use them to assess the 

relative error of sample recovery, sample 

preparation, and analytical procedures and 

then consider the relative error in evaluating 

the measured emissions. 

Sampling Procedures 

7.0 What Sampling Procedures Must I Use? 

You may determine bias and precision by 

comparing against a validated test method, 

using isotopic sampling, or using analyte 

spiking. Isotopic sampling can only be used 

for procedures requiring mass spectrometry. 

You must collect samples according to the 

requirements in Table 1. You must perform 

the sampling according to the procedures in 

sections 7.1 through 7.5. 

7.1 Comparison Against a Validated Test 

Method. If you are comparing the results 

from the validated test method, it is 

recommended that you conduct a 

performance audit according to the 

procedures in section 6. 

7.2 Isotopic Spiking. Spike all 12 samples 

with the analyte at the concentration in the 

applicable emission limitation or standard in 

the subpart of 40 CFR part 63. If there is no 

applicable emission limitation or standard, 

spike at the expected level of the samples. 

Follow the appropriate spiking procedures in 

7.4.1 through 7.4.2 for the applicable waste 

medium. 

7.3 Analyte Spiking. In each quadruplet 

set, spike half of the samples (two out of the 

four) with the analyte according to the 

applicable procedure in Section 7.4. 

7.4 Spiking Procedure.

7.4.1 Gaseous Analyte with Sorbent or 

Impinger Sampling Trains. Sample the 

analyte (in the laboratory or in the field) at 

a concentration that is close to the 

concentration in the applicable emission 

limitation or standard in the subpart of 40 

CFR part 63 (or the expected sample 

concentration where there is no standard) for 

the time required by the method, and then 

sample the gas stream for an equal amount 

of time. The time for sampling both the 

analyte and gas stream should be equal; 

however, the time should be adjusted to 

avoid sorbent breakthrough. The stack gas 

and the gaseous analyte may be sampled at 

the same time. The analyte must be 

76650 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

introduced as close to the tip of the sampling 

train as possible. 

7.4.2 Gaseous Analyte with Sample 

Container (Bag or Canister). Spike the sample 

containers after completion of each test run 

with an amount equal to the concentration in 

the applicable emission limitation or 

standard in the subpart of 40 CFR part 63 (or 

the expected sample concentration where 

there is no standard). The final concentration 

of the analyte shall approximate the level of 

the emission concentration in the stack. The 

volume amount of analyte shall be less than 

10 percent of the sample volume. 

7.4.3 Liquid and Solid Analyte with 

Sorbent or Impinger Trains. Spike the trains 

with an amount equal to the concentration in 

the applicable emission limitation or 

standard in the subpart of 40 CFR part 63 (or 

the expected sample concentration where 

there is no standard) before sampling the 

stack gas. If possible, do the spiking in the 

field. If it is not possible to do the spiking 

in the field, you can do it in the laboratory. 

7.4.4 Liquid and Solid Analyte with 

Sample Container (Bag or Canister). Spike 

the containers at the completion of each test 

run with an amount equal to the 

concentration in the applicable emission 

limitation or standard in the subpart of 40 

CFR part 63 (or the expected sample 

concentration where there is no standard).

7.5 Probe Placement and Arrangement 

for Stationary Source Stack or Duct 

Sampling. To sample a stationary source as 

defined in 40 CFR 63.2, you must place the 

probe according to the procedures in 7.5. You 

must place the probes in the same horizontal 

plane. 

7.5.1 For Paired Sample Probes, the 

sample probe tip should be 2.5 cm from the 

outside edge of the other sample probe, with 

a pitot tube on the outside of each probe. The 

Administrator may approve a validation 

request where other paired arrangements for 

the pitot tube are used. 

7.5.2 For Quadruplet Sampling Probes,

the tips should be in a 6.0 cm × 6.0 cm square 

area measured from the center line of the 

opening of the probe tip with a single pitot 

tube in the center or two pitot tubes with 

their location on either side of the probe tip 

configuration. You must propose an 

alternative arrangement whenever the crosssectional area of the probe tip configuration 

is approximately 5 percent or more of the 

stack or duct cross-sectional area. 

8.0 How Do I Ensure Sample Stability? 

8.1 Developing Storage and Analysis 

Procedures. If the alternative test method 

includes well-established procedures 

supported by experimental data for sample 

storage and the time within which the 

collected samples must be analyzed, you 

must store the samples according to the 

procedures in the alternative test method. 

You are not required to conduct the 

procedures in section 8.2 or 8.3. If the 

alternative test method does not include such 

procedures, you must propose procedures for 

storing and analyzing samples to ensure 

sample stability. At a minimum, your 

proposed procedures must meet the 

requirements in section 8.2 or 8.3. The 

minimum storage time should be as soon as 

possible, but no longer than 24 hours after 

collection of the sample. The maximum 

storage time should be four weeks or less. 

8.2 Storage and Sampling Procedures for 

Stack Test Emissions. You must store and 

analyze samples of stack test emissions 

according to Table 3. If you are using analyte 

spiking procedures, you must include equal 

numbers of spiked and unspiked samples. 

8.3 Storage and Sampling Procedures for 

Testing Other Waste Media. You must 

analyze half of the replicate samples at the 

proposed minimum storage time and the 

other half at the proposed maximum storage 

time to identify the effect of storage times on 

analyte samples. The minimum storage time 

should be as soon as possible, but no longer 

than 24 hours after collection of the sample. 

The maximum storage time should be two 

weeks or less. 

8.4 Sample Stability. After you have 

conducted sampling and analysis according 

to 8.2 or 8.3, compare the results at the 

minimum and maximum storage times. 

Calculate the difference in the results using 

Equation 301–1.

dR R i = − mini maxi Eq. 301-1

Where:

di = difference between the results of the ith 

sample. 

Rmini = results from the ith sample at the 

minimum storage time. 

Rmaxi = results from the ith sample at the 

maximum storage time.

8.4.1 Standard Deviation. Determine the 

standard deviation, SDd, of the differences, 

di’s, of the paired samples using Equation 

301–2.

SD

d d

n

d

i m

i

N

=

( ) −

−

∑ 2

1 Eq. 301-2

Where:

Vm = validated method. 

Pm = proposed alternative test method. 

di = The difference between the i–th pair of 

samples, Vm¥Pm. 

dm = The mean of the paired sample 

differences. 

n = total number of paired samples.

8.4.2 t Test. Test the difference in the 

results for statistical significance by 

calculating the t-statistic and determining if 

the mean of the differences between the 

initial results and the results after storage is 

significant at the 95 percent confidence level. 

Calculate the value of the t-statistic using 

Equation 301–3.

t

d

SD

n

m

d

= Eq. 301-3

Where:

n is the total number of paired samples.

Compare the calculated t-statistic with the 

critical value of the t-statistic from Table 2. 

If the calculated t-value is less than the 

critical value, the difference is not 

statistically significant, thus, the sampling 

and analysis procedure ensures stability, and 

you may submit a request for validation of 

the proposed alternative test method. If the 

calculated t-value is greater than the critical 

value, the difference is statistically 

significant and you must repeat the 

procedures in 8.2 or 8.3 with new samples 

using shorter proposed maximum storage 

times. 

Bias and Precision

9.0 What Are the Requirements for Bias? 

You must establish bias by comparing the 

results of the sampling using the alternative 

test method against a reference value. The 

bias must be no more than +/¥10% for the 

alternative test method to be acceptable. 

10.0 What Are the Requirements for 

Precision? 

At a minimum, you must use paired 

sampling systems to establish precision. If 

you are using analyte spiking, including 

isotopic samples, the precision expressed as 

the relative standard deviation (RSD), of the 

alternative test method at the level of the 

applicable emission limitation or standard in 

the subpart of 40 CFR part 63 must be less 

than or equal to 20 percent. If you are 

comparing to a validated test method, the 

alternative test method must be at least as 

precise as the validated method at the level 

of the applicable emission limitation or 

standard in the subpart of 40 CFR part 63 as 

determined by an F test. 

11.0 What Calculations Must I Perform for 

Isotopic Spiking? 

You must analyze the bias, precision, 

relative standard deviation, and data 

acceptance for isotopic spiking tests 

according to the provisions in sections 11.1 

through 11.3. 

11.1 Numerical Bias. Calculate the 

numerical value of the bias using the results 

from the analysis of the isotopically spiked 

field samples and the calculated value of the 

isotopically labeled spike according to 

Equation 301–4.

B S CS = − m Eq. 301-4

Where:

B = Bias at the spike level. 

Sm = Mean of the measured values of the 

isotopically spiked samples. 

CS = Calculated value of the isotopically 

labeled spike.

11.2 Standard Deviation. Calculate the 

standard deviation of the Si values according 

to Equation 301–5.

SD

S S

n

i m = ( ) −

( ) −

∑ 2

1 Eq. 301-5

Where:

Si = Measured value of the isotopically 

labeled analyte in the i-th field sample, 

n = Number of isotopically spiked samples, 

12.

11.3 t Test. Test the bias for statistical 

significance by calculating the t-statistic 

using Equation 301–6. Use the standard 

deviation determined in section 11.2 and the 

numerical bias determined in section 11.1.


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t

B

SD

n

= Eq. 301-6

Compare the calculated t-value with the 

critical value of the two-sided t-distribution 

at the 95 percent confidence level and n¥1 

degrees of freedom. When spiking is 

conducted according to the procedures 

specified in Sections 7.2 and 7.4 as required, 

this critical value is 2.201 for the eleven 

degrees of freedom. If the calculated t-value 

is less than the critical value, the bias is not 

statistically significant and the data are 

acceptable. If the calculated t-value is greater 

than the critical value, the bias is statistically 

significant and you must evaluate the relative 

magnitude of the bias using Equation 301–7.

BR

B

CS

= × 100% Eq. 301-7

Where:

BR = Relative bias.

If the relative bias is less than or equal to 

10 percent, then the data are acceptable. You 

may proceed to evaluate the precision. If not 

the candidate method will not meet the 

requirements of Method 301. 

11.4 Relative Standard Deviation.

Calculate the RSD according to Equation 

301–8

RSD SD

Sm

= 



 



 × 100 Eq. 301-8

where Sm is the measured mean of the 

isotopically labeled spiked samples. The data 

and alternative test method are unacceptable 

if the RSD is greater than 20 percent. 

12.0 What Calculations Must I Perform for 

Comparison With a Validated Method If I Am 

Using Paired Sampling Systems? 

You must analyze the data for comparison 

with a validated method according to Section 

12. Conduct these procedures to determine if 

an alternative test method produces results 

equivalent to a validated method. If the data 

from the alternative test method fail either 

the bias or precision test, the data and the 

alternative test method are unacceptable. 

12.1 Bias Analysis.

12.1.1 Standard Deviation. Determine the 

standard deviation, SDd, of the differences, 

di’s, of the paired samples using Equation 

301–2. 

12.1.2 t Test. Test the bias for statistical 

significance by calculating the t-statistic and 

determine if the mean of the differences 

between the alternative test method and the 

validated method is significant at the 95 

percent confidence level. Calculate the value 

of the t-statistic using Equation 301–3. For 

the spiking procedure for paired sampling 

systems, according to section 7.1 and Table 

1, n equals nine. 

Compare the calculated t-statistic with the 

critical value of the t-statistic. When nine 

runs are conducted, as specified in Section 

7.1 and Table 1, the critical value of the tstatistic is 1.397 for eight degrees of freedom. 

If the calculated t-value is less than the 

critical value, the bias is not statistically 

significant and the data are acceptable. If the 

calculated t-value is greater than the critical 

value, the bias is statistically significant and 

you must evaluate the relative magnitude of 

the bias using Equation 301–9. If the relative 

bias is less than or equal to 10 percent, then 

the data are acceptable. Proceed to evaluate 

precision.

B B

VS R = × 100% Eq. 301-9

Where:

B = Bias = mean of the di’s. 

VS = mean measured by the validated 

method.

12.2. Precision. Compare the variance of 

the alternative test method to that of the 

validated method. If a significant difference 

is determined using the F test, the alternative 

test method and the results are rejected. If the 

F test does not show a significant difference, 

then the alternative test method has 

acceptable precision. This procedure requires 

that you know the standard deviation of the 

validated method, SDv. Use the value 

furnished with the method. If the standard 

deviation of the validated method is not 

available, the paired replicate sampling 

procedure may not be used. 

12.2.1 Variance. Calculate the variance of 

the validated method, Sv

2, using Equation 

301–10.

S SD Eq v v

2 2 = . 301-10

Where:

SDv = Standard deviation provided with the 

validated method.

12.2.2 Pooled Variance. Calculate the 

pooled variance of both methods, S2

pooled, 

according to Equation 301–11.

S

d

n

Eq pooled

i

i

N

2

2

2 1 = −

∑

 301-11

( ) .

Where:

di = The difference between the i-th pair of 

validated and alternative method 

samples. 

n = The number of pairs of samples.

12.2.3 Alternative Test Method Variance.

Calculate the variance of the alternative test 

method, S2

p, from the S2pooled using Equation 

301–12.

SS S p pooled v

22 2 = − Eq. 301-12

(If S2

v > S2pooled, let S2p = S2pooled/2).

12.2.4 The F Test. Determine if the 

variance of the alternative test method is 

significantly different from that of the 

validated method by performing the F test. 

Calculate the experimental F-value using 

Equation 301–13.

F

S

S

p

v

=

2

2 Eq. 301-13

Compare the experimental F value with the 

critical range of F at a 95 percent confidence 

level. When the procedure specified in 

Section 7.1 and Table 1 for paired trains is 

followed as required, the critical range is 

0.291 to 3.44. If the calculated F is outside 

the critical range, the difference in precision 

is significant and the data and alternative test 

method are unacceptable. 

13.0 What Calculations Must I Perform for 

Comparison With a Validated Method If I Am 

Using Quadruplet Replicate Sampling 

Systems? 

If you are using quadruplet replicate 

sampling systems to compare an alternative 

test method to a validated method, then you 

must analyze the data according to the 

provisions in 13.0. If the data from the 

alternative test method fail either the bias or 

precision test, the data and the alternative 

test method are unacceptable. If the 

Administrator determines that the affected 

source has highly variable emission rates, the 

Administrator may require additional 

precision checks. 

13.1 Bias Analysis. Test the bias for 

statistical significance at the 95 percent 

confidence level by calculating the t-statistic. 

13.1.1 Bias. Determine the bias, which is 

defined as the mean of the differences 

between the alternative test method and the 

validated method (dm). Calculate di according 

to Equation 301–14.

d

VV PP

i

i i ii = ( ) + − 1 2 12 ( ) +

2 2 Eq. 301-14

Where:

V1i = First measured value with the validated 

method in the i-th sample. 

V2i = Second measured value with the 

validated method in the i-th sample. 

P1i = First measured value with the 

alternative test method in the i-th 

sample. 

P2i = Second measured value with the 

alternative test method in the i-th 

sample.

13.1.2 Standard Deviation of the 

Differences. Calculate the standard deviation 

of the differences, SDd, using Equation 301–

2. 

13.1.3 T Test. Calculate the t-statistic 

using Equation 301–3, where n is the total 

number of test sample differences (di). For 

the quadruplet sampling system procedure in 

section 7.1 and Table 1, n equals four. 

Compare the calculated t-statistic with the 

critical value of the t-statistic and determine 

if the bias is significant at the 95 percent 

confidence level. When four runs are 

conducted, as specified in section 7.2 and 

Table 1, the critical value of the t-statistic is 

1.638 for three degrees of freedom. If the 

calculated t-value is less than the critical 

value, the bias is not statistically significant 

and the data are acceptable. If the calculated 

t-value is greater than the critical value, the 

bias is statistically significant and you must 

evaluate the relative magnitude of the bias 

using Equation 301–9. If the relative bias is 

less than or equal to 10 percent, then the data 

are acceptable. Proceed to evaluate precision 

of the alternative test method. 

13.2 Precision. Compare the variance of 

the alternative test method to that of the 

validated method. If a significant difference 

is determined using the F test, the alternative 

test method and the results are rejected. If the


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76652 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

F test does not show a significant difference, 

then the alternative test method has 

acceptable precision. This procedure requires 

the standard deviation of the validated 

method, SDv, to be known. Use the value 

furnished with the method. If there are no 

published values, calculate the variance of 

the validated method using Equation 301–15. 

13.2.1 Alternative Test Method Variance.

Calculate the variance of the alternative test 

method, Sp

2, according to Equation 301–15.

S

d

n p

2 1

2

2 = ∑ Eq. 301-15

Where:

di = The difference between the i-th pair of 

samples collected with the alternative 

test method.

13.2.2 The F Test. Determine if the 

variance of the alternative test method is 

greater than that of the validated method by 

calculating the F-value using Equation 301–

13. Compare the experimental F value with 

the critical range of F. The critical range is 

0.264 to 3.79 for the 95 percent confidence 

level when the procedure specified in section 

7.1 and Table 1 for quadruplet trains is 

followed. If the calculated F is outside the 

critical range, the difference in precision is 

significant, and the data and the alternative 

test method are unacceptable. 

14.0 What calculations must I perform for 

analyte spiking?

You must analyze the data for analyte 

spike testing according to section 14. 

14.1 Bias Analysis.

14.1.1 Bias. Calculate the numerical 

value of the bias using the results from the 

analysis of the spiked field samples, the 

unspiked field samples, and the calculated 

value of the spike using Equation 301–16.

B S M CS =− − m m Eq. 301-16

Where:

B = Bias at the spike level. 

Sm = Mean of the spiked samples. 

Mm = Mean of the unspiked samples. 

CS = Calculated value of the spiked level.

14.1.2 T Test. Test the bias for statistical 

significance by calculating the t-statistic 

using Equation 301–17 and comparing it with 

the critical value of the two-sided tdistribution at the 95 percent confidence 

level and n-2 degrees of freedom. This 

critical value is 2.228 for the ten degrees of 

freedom.

t

B

S S u s

=

+2 2

12

Eq. 301-17

Where:

Su

2 = (SDu) 2, SDu is calculated in Equation 

301–19. 

Ss

2 = (SDs) 2, SDs is calculated in Equation 

301–18.

If the calculated t-value is less than the 

critical value, the bias is not statistically 

significant and the data are acceptable. If the 

calculated t-value is greater than the critical 

value, the bias is statistically significant and 

you must evaluate the relative magnitude of 

the bias using Equation 301–7. If the relative 

bias is less than or equal to 10 percent, then 

the data are acceptable. You may proceed to 

evaluate precision. 

14.2 Precision. Calculate the standard 

deviation and the RSD of the alternative test 

method. 

14.2.1 Spiked Samples. Calculate the 

difference, di, between the pairs of the spiked 

alternative test method measurements for 

each replicate sample set. Determine the 

standard deviation (SDs) of the spiked values 

using Equation 301–18.

SD

d

n s is = ∑ 2

2 Eq. 301-18

Where:

dis = Difference between the i-th pair of 

spiked samples. 

n = Number of paired samples.

14.2.2 Unspiked Samples. Calculate the 

standard deviation of the unspiked values 

using Equation 301–19.

SD

d

n u iu = ∑ 2

2 Eq. 301-19

Where:

diu = Difference between the i-th pair of 

unspiked samples. 

n = Number of paired samples.

14.2.3 Pooled Standard Deviation.

Calculate the pooled standard deviation of 

the spiked and unspiked samples if the 

standard deviations are not significantly 

different. Test for this difference using 

Equation 301–20.

F S

S

u

s

=

2

2 Eq. 301-20

Where Su

2 and Ss2 are defined in Equation 

301–17. 

For the case where n = 6 and a 95 percent 

confidence level, the standard deviations 

may be pooled if the calculated F lies 

between 0.139 and 7.146. Calculate the 

pooled standard deviation (SDpooled) using 

Equation 301–21.

SD S S

pooled s u = +2 2

2 Eq. 301-21

If the variances are significantly different 

and cannot be pooled, use the standard 

deviation of the spiked samples for the bias 

analysis in section 14.1.2. 

14.2.4 Relative Standard Deviation.

Calculate the RSD of the alternative test 

method using Equation 301–8 and the pooled 

standard deviation determined from Section 

14.2.3. If the pooled standard deviation or the 

standard deviation from the unspiked 

samples is used, Sm is the mean of the 

unspiked samples. If the standard deviation 

of the spiked samples is used, Sm is the mean 

of the spiked samples. The data and 

alternative test method are unacceptable if 

the RSD is greater than 20 percent. 

15.0 How do I conduct tests at similar 

sources? 

If the Administrator has approved the use 

of an alternative test method to a test method 

required in 40 CFR part 63 for an affected 

source, and the Administrator has approved 

the use of the alternative test method at your 

similar source according to the procedures in 

19.1.1, you must meet the requirements in 

this section. You must have at least three 

replicate samples for each test that you 

conduct at the similar source. You must 

average the results of the samples to 

determine the pollutant concentration. 

Optional Requirements 

16.0 How do I use and conduct ruggedness 

testing? 

If you want to use a validated test method 

at a concentration that is different from the 

concentration in the applicable emission 

limitation in the subpart of 40 CFR part 63 

or for a source category that is different from 

the source category that the test method 

specifies, then you must conduct ruggedness 

testing according to the procedures in 

Citation 10 of Section 18.0 and submit a 

request for a waiver according to 19.1.1. 

Ruggedness testing is a laboratory study to 

determine the sensitivity of a method to 

parameters such as sample collection rate, 

interferant concentration, collecting medium 

temperature, and sample recovery 

temperature. You conduct ruggedness testing 

by changing several variables simultaneously 

instead of changing one variable at a time. 

For example, you can determine the effect of 

seven variables in eight experiments instead 

of one. (W.J. Youden, Statistical Manual of 

the Association of Official Analytical 

Chemists, Association of Official Analytical 

Chemists, Washington, DC, 1975, pp. 33–36). 

17.0 How do I determine the Limit of 

Detection for the alternative method? 

17.1 Limit of Detection. The Limit of 

Detection (LOD) is the lowest level above 

which you may obtain quantitative results 

with an acceptable degree of confidence. For 

this protocol, the LOD is defined as 3 times 

the standard deviation, So, at the blank level. 

This LOD corresponds to an uncertainty of 

±30% at the 99 percent confidence level. 

17.2 Purpose. The LOD will be used to 

establish the lower limit of the test method. 

If the estimated LOD is no more than twice 

the calculated LOD, use Procedure I in Table 

4 to determine So. If the LOD is greater than 

twice the calculated LOD, use Procedure II in 

Table 4 to determine So. 

Other Requirements and Information 

18.0 How do I apply for approval of an 

alternative test method? 

18.1 Submitting Requests. You must 

request to use an alternative test method 

according to the procedures in § 63.7(f). You 

may not use an alternative test method to 

meet any requirement under 40 CFR part 63 

until the Administrator has approved your 

request. The request must include a field 

validation reporting containing the 

information in 18.2. The request must be 

submitted to the Director, Emissions 

Monitoring and Analysis Division, U.S.


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Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 76653

Environmental Protection Agency, C304–02, 

Research Triangle Park, NC 27711. 

18.2 Field Validation Report. The field 

validation report must contain the 

information in 18.2.1 through 18.2.9. 

18.2.1 Regulatory objectives for the 

testing, including a description of the reasons 

for the test, applicable emission limits, and 

a description of the source.

18.2.2 Summary of the results and 

calculations shown in Sections 7.0 through 

17, as applicable.

18.2.3 Analyte certification and value(s).

18.2.4 Laboratory demonstration of the 

quality of the spiking system.

18.2.5 Discussion of laboratory 

evaluations.

18.2.6 Discussion of field sampling.

18.2.7 Discussion of sample preparations 

and analysis.

18.2.8 Storage times of samples (and 

extracts, if applicable).

18.2.9 Reasons for eliminating any 

results.

19.0 How do I request a waiver? 

19.1 Conditions for Waivers. If you meet 

one of the criteria in 19.1.1 through 19.1.3, 

the Administrator may waive the 

requirement to use the procedures in this 

method to validate an alternative test 

method. In addition, if the EPA currently 

recognizes an appropriate test method or 

considers the analyst’s test method to be 

satisfactory for a particular source, the 

Administrator may waive the use of this 

protocol or may specify a less rigorous 

validation procedure. 

19.1.1 Similar Sources. If the alternative 

test method that you want to use has been 

validated at another source and you can 

demonstrate to the Administrator’s 

satisfaction that your affected source is 

similar to that source, then the Administrator 

may waive the requirement for you to 

validate the alternative test method. One 

procedure you may use to demonstrate the 

applicability of the method to your affected 

source is by conducting a ruggedness test as 

described in 16.0.

19.1.2 Documented Methods. If the bias 

and precision of the alternative test method 

that you are proposing have been 

demonstrated through laboratory tests or 

protocols different from this method, and you 

can demonstrate to the Administrator’s 

satisfaction that the bias and precision apply 

to your application, then the Administrator 

may waive the requirement to use this 

method or to use part of this method. 

19.1.3 Conditional Test Methods. If the 

alternative test method has been 

demonstrated to be valid at several sources, 

you may ask the Administrator to designate 

the alternative test method as a conditional 

test method. If the Administrator has 

designated a test method as a conditional test 

method and you are using the conditional 

method within its stated applicability, you 

do not have to validate it according to the 

procedures in this method. You can find a 

list of conditional test methods at http://

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

19.2 Submitting Applications for Waivers.

You must sign and submit each request for 

a waiver from the requirements in this 

method in writing. The request must be 

submitted to the Director, Emissions 

Monitoring and Analysis Division, U.S. 

Environmental Protection Agency, C304–02, 

Research Triangle Park, NC 27711. 

19.3 Information Application for Waiver.

The request for a waiver must contain a 

thorough description of the test method, the 

intended application, and results of any 

validation or other supporting documents. 

The request for a waiver must contain, at a 

minimum, the information in 19.3.1 through 

19.3.4. The Administrator may request 

additional information if necessary to 

determine whether this method can be 

waived for a particular application. 

19.3.1 A Clearly Written Test Method.

The method should be written preferably in 

the format of 40 CFR 60, Appendix A Test 

Methods. It must include an applicability 

statement, concentration range, precision, 

bias (accuracy), and minimum and maximum 

storage time in which samples must be 

analyzed. 

19.3.2 Summaries (see Section 18.3) of 

previous validation tests or other supporting 

documents. If a different procedure from that 

described in this method was used, you must 

submit documents substantiating the bias 

and precision values to the Administrator’s 

satisfaction. 

19.3.3 Ruggedness Testing Results. You 

must submit results of ruggedness testing 

conducted according to Section 16, sample 

stability conducted according to section 8, 

and detection limits conducted according to 

section 17, as applicable. For example, you 

would not need to submit ruggedness testing 

results if you will be using the method at the 

same concentration level as the concentration 

level at which it was validated. 

19.3.4 Applicability Statement and 

Arguments for Waiver Approval. Discussion 

of the applicability statement and arguments 

for approval of the waiver. This discussion 

should address as applicable the following: 

applicable regulation, emission standards, 

effluent characteristics, and process 

operations. 

20.0 What definitions apply to this method? 

Affected source means affected source as 

defined in 40 CFR 63.2 and in the relevant 

subpart under 40 CFR part 63. 

Alternative test method means the 

sampling and analytical methodology 

selected for field validation using the method 

described in this appendix. 

Paired sampling system means a sampling 

system capable of obtaining two replicate 

samples that were collected as closely as 

possible in sampling time and sampling 

location. 

Quadruplet sampling system means a 

sampling system capable of obtaining four 

replicate samples that were collected as 

closely as possible in sampling time and 

sampling location. 

Surrogate compound means a compound 

that serves as a model for the types of 

compounds being analyzed (i.e., similar 

chemical structure, properties, behavior). The 

model can be distinguished by the method 

from the compounds being analyzed. 

21.0 Where can I find additional 

information? 

You can find additional information in the 

references in paragraphs 21.1 through 21.12. 

21.1 Albritton, J.R., G.B. Howe, S.B. 

Tompkins, R.K.M. Jayanty, and C.E. Decker. 

1989. Stability of Parts-Per-Million Organic 

Cylinder Gases and Results of Source Test 

Analysis Audits, Status Report No. 11. 

Environmental Protection Agency Contract 

68–02–4125. Research Triangle Institute, 

Research Triangle Park, NC. September. 

21.2 DeWees, W.G., P.M. Grohse, K.K. 

Luk, and F.E. Butler. 1989. Laboratory and 

Field Evaluation of a Methodology for 

Speciating Nickel Emissions from Stationary 

Sources. EPA Contract 68–02–4442. Prepared 

for Atmospheric Research and Environmental 

Assessment Laboratory, Office of Research 

and Development, U.S. Environmental 

Protection Agency, Research Triangle Park, 

NC 27711. January. 

21.3 Keith, L.H., W. Crummer, J. Deegan 

Jr., R.A. Libby, J.K. Taylor, and G. Wentler. 

1983. Principles of Environmental Analysis. 

American Chemical Society, Washington, 

DC. 

21.4 Maxwell, E.A. 1974. Estimating 

variances from one or two measurements on 

each sample. Amer. Statistician 28:96–97.

21.5 Midgett, M.R. 1977. How EPA 

Validates NSPS Methodology. Environ. Sci. & 

Technol. 11(7):655–659. 

21.6 Mitchell, W.J., and M.R. Midgett. 

1976. Means to evaluate performance of 

stationary source test methods. Environ. Sci. 

& Technol. 10:85–88. 

21.7 Plackett, R.L., and J.P. Burman. 

1946. The design of optimum multifactorial 

experiments. Biometrika, 33:305. 

21.8 Taylor, J.K. 1987. Quality Assurance 

of Chemical Measurements. Lewis 

Publishers, Inc., pp. 79–81. 

21.9 U.S. Environmental Protection 

Agency. 1978. Quality Assurance Handbook 

for Air Pollution Measurement Systems: 

Volume III. Stationary Source Specific 

Methods. Publication No. EPA–600/4–77–

027b. Office of Research and Development 

Publications, 26 West St. Clair St., 

Cincinnati, OH 45268. 

21.10 U.S. Environmental Protection 

Agency. 1981. A Procedure for Establishing 

Traceability of Gas Mixtures to Certain 

National Bureau of Standards Standard 

Reference Materials. Publication No. EPA–

600/7–81–010. Available from the U.S. EPA, 

Quality Assurance Division (MD–77), 

Research Triangle Park, NC 27711. 

21.11 U.S. Environmental Protection 

Agency. 1991. Protocol for The Field 

Validation of Emission Concentrations From 

Stationary Sources. Publication No. 450/4–

90–015. Available from the U.S. EPA, 

Emission Measurement Technical 

Information Center, Technical Support 

Division (MD–14), Research Triangle Park, 

NC 27711. 

21.12 Youden, W.J. Statistical techniques 

for collaborative tests. In: Statistical Manual 

of the Association of Official Analytical 

Chemists, Association of Official Analytical 

Chemists, Washington, DC, 1975, pp. 33–36.

76654 Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 

TABLE 1 OF APPENDIX A.—SAMPLING

PROCEDURES

If you are . . . You must collect . . . 

Comparing 

against a 

validated 

method.

Nine sets of replicate samples using a paired sampling system (a total of 18 

samples) or four sets of 

replicate samples using a 

quadruplet sampling system (a total of 16 samples). In each sample set, 

you must use the validated test method to collect and analyze half of 

the samples. 

TABLE 1 OF APPENDIX A.—SAMPLING

PROCEDURES—Continued

If you are . . . You must collect . . . 

Using isotopic 

spiking (can 

only be used 

for procedures requiring mass 

spectrometry).

A total of 12 replicate samples. You may collect the 

either samples by obtaining six sets of paired samples or three sets of quadruplet samples. 

Using analyte 

spiking.

A total of 24 samples using 

the quadruplet sampling 

system (a total of 6 sets of 

replicate samples). 

TABLE 2 OF APPENDIX A.—CRITICAL

VALUES OF t FOR THE TWO TAILED

95 PERCENT CONFIDENCE LIMIT

Degrees of freedom t95

1 .................................................... 3=078 

2 .................................................... 1=886 

3 .................................................... 1=638 

4 .................................................... 1=533 

5 .................................................... 1=476 

6 .................................................... 1=44 

7 .................................................... 1=415 

8 .................................................... 1=397 

9 .................................................... 1=383 

10 .................................................. 1=372 

TABLE 3 OF APPENDIX A.—STORAGE AND SAMPLING PROCEDURES FOR STACK TEST EMISSIONS

If you are . . . With . . . Then you must . . . 

Using isotopic or analyze spiking procedures ... Sample container (bag or canister) and impinger sampling systems.Analyze six of the samples at the proposed 

minimum storage time and then analyze the 

same six samples at the proposed maximum storage time. 

Sorbent and impinger sampling systems that 

require extraction or digestion.

Extract or digest six of the samples at the proposed minimum storage time and extract or 

digest six other samples at the proposed 

maximum storage time. Analyze an aliquot 

of the first six extracts (digestates) at both 

the proposed minimum and proposed maximum storage times. This will allow analysis 

of extract storage impacts. 

Sorbent sampling systems that require thermal desorption.Analyze six samples at the proposed minimum storage time. Analyze another set of 

six samples at the proposed maximum storage time. 

Comparing an alternative test method against a 

validated test method.

Sampling method that does not include sorbent and impinger sampling systems that 

require extraction or digestion.

Analyze half of the samples (8 or 9) at the 

proposed minimum storage time and half of 

the samples (8 or 9) at the proposed maximum storage time. 

Sorbent and impinger sampling systems that 

require extraction or digestion.

Extract or digest six of the samples at the proposed minimum storage time and extract or 

digest six other samples at the proposed 

maximum storage time. Analyze an aliquot 

of the first six extracts (digestates) at both 

the proposed minimum and proposed maximum storage times. This will allow analysis 

of extract storage impacts. 

TABLE 4 TO APPENDIX A.—PROCEDURES FOR ESTIMATING So

If the estimated LOD is no more than twice the calculated LOD, use 

Procedure I as follows 

If the LOD is greater than twice the calculated LOD, use Procedure II 

as follows. 

Estimate the LOD and prepare a test standard at this level. The test 

standard could consist of a dilution of the analyze described in Section 5.0..

Prepare two additional standards at concentration levels lower than the 

standard used in Procedure I. 

Using the normal sampling and analytical procedures for the method, 

sample and analyze this standard at least seven times in the laboratory.

Sample and analyze each of these standards at least seven times. 

Calculate the standard deviation, So, of the measured values ................ Calculate the standard deviation for each concentration level. 

Calculate the LOD as 3 times So. ............................................................ Plot the standard deviations of the three test standards as a function of 

the standard concentrations. 

Draw a best-fit straight line through the data points and extrapolate to 

zero concentration. The standard deviation at zero concentration is 

So. 

Calculate the LOD as 3 times So. 

Federal Register / Vol. 69, No. 245 / Wednesday, December 22, 2004 / Proposed Rules 76655

* * * * *

[FR Doc. 04–27985 Filed 12–21–04; 8:45 am] 

BILLING CODE 6560–50–P

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 82 

[FRL–7852–1] 

RIN 2060–AM50 

Protection of Stratospheric Ozone: 

Allocation of Essential Use Allowances 

for Calendar Year 2005

AGENCY: Environmental Protection 

Agency (EPA).

ACTION: Proposed rule.

SUMMARY: EPA is proposing to allocate 

essential use allowances for import and 

production of class I stratospheric ozone 

depleting substances (ODSs) for 

calendar year 2005. Essential use 

allowances enable a person to obtain 

controlled class I ODSs as an exemption 

to the regulatory ban of production and 

import of these chemicals, which 

became effective on January 1, 1996. 

EPA allocates essential use allowances 

for exempted production or import of a 

specific quantity of class I ODS solely 

for the designated essential purpose. 

The proposed allocations total 1,524.58 

metric tons of chlorofluorocarbons for 

use in metered dose inhalers.

DATES: Written comments on this 

proposed rule must be received by the 

EPA Docket on or before January 21, 

2005, unless a public hearing is 

requested. Comments must then be 

received on or before 30 days following 

the public hearing. Any party requesting 

a public hearing must notify the contact 

listed below under FOR FURTHER

INFORMATION CONTACT by 5 p.m. eastern 

standard time on January 23, 2005. If a 

hearing is held, EPA will publish a 

document in the Federal Register

announcing the hearing information.

ADDRESSES: Submit your comments, 

identified by Docket ID No. OAR–2004–

0063, by one of the following methods: 

• Federal eRulemaking Portal: http://

www.regulations.gov. Follow the on-line 

instructions for submitting comments. 

• Agency Web site: http://

www.epa.gov/edocket. EDOCKET, EPA’s 

electronic public docket and comment 

system, is EPA’s preferred method for 

receiving comments. Follow the on-line 

instructions for submitting comments. 

• Mail: Air and Radiation Docket, 

Environmental Protection Agency, 

Mailcode 6102T, 1200 Pennsylvania 

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

Attention: Docket ID No. OAR–2004–

0063.

• Hand Delivery: EPA Docket Center, 

(EPA/DC) EPA West, Room B102, 1301 

Constitution Ave., NW., Washington, 

DC, Attention Docket ID No. OAR–

2004–0063. Deliveries are only accepted 

during the Docket’s normal hours of 

operation, and special arrangements 

should be made for deliveries of boxed 

information. 

Instructions: Direct your comments to 

Air Docket ID No. OAR–2004–0063. 

EPA’s policy is that all comments 

received will be included in the public 

docket without change and may be 

made available online at http://

www.epa.gov/edocket, including any 

personal information provided, unless 

the comment includes information 

claimed to be Confidential Business 

Information (CBI) or other information 

whose disclosure is restricted by statute. 

Do not submit information that you 

consider to be CBI or otherwise 

protected through EDOCKET, 

regulations.gov, or e-mail. For 

instructions on how to submit CBI, see 

‘‘How do I submit confidential business 

information to EPA?’’ under 

SUPPLEMENTARY INFORMATION. 

The EPA EDOCKET and the federal 

regulations.gov websites are 

‘‘anonymous access’’ systems, which 

means EPA will not know your identity 

or contact information unless you 

provide it in the body of your comment. 

If you send an e-mail comment directly 

to EPA without going through 

EDOCKET or regulations.gov, your email address will be automatically 

captured and included as part of the 

comment that is placed in the public 

docket and made available on the 

Internet. 

If you submit an electronic comment, 

EPA recommends that you include your 

name and other contact information in 

the body of your comment and with any 

disk or CD–ROM you submit. If EPA 

cannot read your comment due to 

technical difficulties and cannot contact 

you for clarification, EPA may not be 

able to consider your comment. 

Electronic files should avoid the use of 

special characters, any form of 

encryption, and be free of any defects or 

viruses. 

Docket: All documents in the docket 

are listed in the EDOCKET index at 

http://www.epa.gov/edocket. Although 

listed in the index, some information is 

not publicly available, namely CBI or 

other information whose disclosure is 

restricted by statute. Certain other 

material, such as copyrighted material, 

is not placed on the Internet and will be 

publicly available only in hard copy 

form. Publicly available docket 

materials are available either 

electronically in EDOCKET or in hard 

copy at the Air Docket, EPA/DC, EPA 

West, Room B102, 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 Docket ID No. OAR–2004–

0063 is (202) 566–1742.

Materials related to previous EPA 

actions on the essential use program are 

contained in EPA Air Docket No. A–93–

39. Docket A–93–39 may be reviewed at 

the Public Reading Room.

FOR FURTHER INFORMATION CONTACT:

Scott Monroe, Essential Use Program 

Manager, by regular mail: U.S. 

Environmental Protection Agency, 

Stratospheric Protection Division 

(6205J), 1200 Pennsylvania Avenue, 

NW., Washington, DC, 20460; by courier 

service or overnight express: 1301 L 

Street, NW., Washington D.C., 20005, by 

telephone: 202–343–9712; or by e-mail: 

monroe.scott@epa.gov.

SUPPLEMENTARY INFORMATION:

Table of Contents 

I. General Information 

A. How should I submit confidential 

business information to EPA? 

II. Basis for Allocating Essential Use 

Allowances 

A. What are essential use allowances? 

B. Under what authority does EPA allocate 

essential use allowances? 

C. What is the process for allocating 

essential use allowances? 

III. Essential Use Allowances for Medical 

Devices 

IV. Proposed Allocation of Essential Use 

Allowances for Calendar Year 2005

V. 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 

Risks and Safety Risks 

H. Executive Order 13211: Actions that 

Significantly Affect Energy Supply, 

Distribution, or Use 

I. National Technology Transfer and 

Advancement Act

I. General Information 

A. How Should I Submit Confidential 

Business Information to EPA? 

Comments that contain confidential 

business information should be 

submitted in two versions, one clearly 

marked ‘‘Public’’, to be filed in the