28664 Federal Register / Vol. 76, No. 96 / Wednesday, May 18, 2011 / Rules and Regulations 

dates, it is reasonable for the EPA to 

exercise its authority to delay the 

effective dates of the Major Source 

Boiler MACT and the CISWI Rule under 

the APA for a period that exceeds three 

months. 

II. Issuance of a Stay and Delay of 

Effective Date 

Pursuant to section 705 of the APA, 

the EPA hereby postpones the 

effectiveness of the Major Source Boiler 

MACT and the CISWI Rule until the 

proceedings for judicial review of these 

rules are complete or the EPA completes 

its reconsideration of the rules, 

whichever is earlier. By this action, we 

are delaying the effective date of both 

rules, published in the Federal Register 

on March 21, 2011 (76 FR 15608 and 76 

FR 15704). The delay of the effective 

date of the CISWI Rule applies only to 

those provisions issued on March 21, 

2011, and not to any provisions of 40 

CFR part 60, subparts CCCC and DDDD, 

in place prior to that date. This delay of 

effectiveness will remain in place until 

the proceedings for judicial review are 

completed or the EPA completes its 

reconsideration of the rules, whichever 

is earlier, and the Agency publishes a 

notice in the Federal Register 

announcing that the rules are in effect. 

List of Subjects 

40 CFR Part 60 

Environmental protection, 

Administrative practice and procedure, 

Air pollution control, Incorporation by 

reference, Intergovernmental relations, 

Reporting and recordkeeping 

requirements. 

40 CFR Part 63 

Environmental protection, 

Administrative practice and procedure, 

Air pollution control, Hazardous 

substances, Incorporation by reference, 

Intergovernmental relations, Reporting 

and recordkeeping requirements. 

For the reasons set forth above, under 

the authority at 7 U.S.C. 705, the 

effective dates of FRL 9272–8, 76 FR 

15608 (March 21, 2011), and FRL 9273– 

4, 76 FR 15704 (March 21, 2011) are 

delayed until further notice. 

Dated: May 16, 2011. 

Lisa P. Jackson, 

Administrator. 

[FR Doc. 2011–12308 Filed 5–17–11; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 63 

[OAR–2004–0080, FRL–9306–8] 

RIN 2060–AF00 

Method 301—Field Validation of 

Pollutant Measurement Methods From 

Various Waste Media 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: This action amends EPA’s 

Method 301, Field Validation of 

Pollutant Measurement Methods from 

Various Waste Media. We revised the 

procedures in Method 301 based on our 

experience in applying the method and 

to correct errors that were brought to our 

attention. The revised Method 301 is 

more flexible, less expensive, and easier 

to use. This action finalizes 

amendments to Method 301 after 

considering comments received on the 

proposed rule published in the Federal 

Register on December 22, 2004. 

DATES: This final rule is effective on 

May 18, 2011. 

ADDRESSES: EPA has established a 

docket for this action under Docket ID 

No. EPA–HQ–OAR–2004–0080. All 

documents in the docket are listed in 

the http://www.regulations.gov index. 

Although listed in the index, some 

information is not publicly available, 

e.g., confidential business information 

(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 at http:// 

www.regulations.gov or in hard copy at 

the Air Docket, EPA/DC, EPA West, 

Room 3334, 1301 Constitution Avenue, 

NW., Washington, DC. The Docket 

Facility and the Public Reading Room 

are 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. 

FOR FURTHER INFORMATION CONTACT: Ms. 

Lula H. Melton, Office of Air Quality 

Planning and Standards, Air Quality 

Assessment Division, Measurement 

Technology Group (E143–02), U.S. 

Environmental Protection Agency, 

Research Triangle Park, North Carolina 

27711; telephone number: (919) 541– 

2910; fax number: (919) 541–0516; 

e-mail address: melton.lula@epa.gov. 

SUPPLEMENTARY INFORMATION: 

Table of Contents 

I. General Information 

A. Does this action apply to me? 

B. Where can I obtain a copy of this action? 

C. Judicial Review 

II. Background 

III. Summary of the Final Method 

IV. Significant Comments Received on the 

Proposed Amendments to Method 301 

A. Applicability 

B. Reference Material 

C. Validation Testing Over a Broad Range 

of Concentrations and Extended Period 

of Time 

D. Performance Audit 

E. Sample Stability Procedures 

F. Bias and Precision 

G. Limit of Detection 

H. Critical Values of t for the Two-Tailed 

95 Percent Confidence Limit 

I. Paired Sampling Procedure 

J. Standard Deviation 

V. Statutory and Executive Order Reviews 

A. Executive Order 12866—Regulatory 

Planning and Review and Executive 

Order 13563—Improving Regulation and 

Regulatory 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 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution or Use 

I. National Technology Transfer and 

Advancement Act 

J. Executive Order 12898—Federal Actions 

To Address Environmental Justice in 

Minority Populations and Low-Income 

Populations 

K. Congressional Review Act 

I. General Information 

A. Does this action apply to me? 

Method 301 affects/applies to you if 

you want to propose a new or 

alternative test method to meet an EPA 

compliance requirement. 

B. Where can I obtain a copy of this 

action? 

In addition to being available in the 

docket, an electronic copy of this rule 

will also be available on the Worldwide 

Web (www) through the Technology 

Transfer Network (TTN). Following the 

Administrator’s signature, a copy of the 

final rule will be placed on the TTN’s 

policy and guidance page for newly 

proposed or promulgated rules at 

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

provides information and technology 

exchange in various areas of air 

pollution control. A redline strikeout 


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document that compares this final rule 

to the proposed rule has also been 

added to the docket. 

C. Judicial Review 

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

Air Act (CAA), judicial review of this 

final rule is available by filing a petition 

for review in the United States Court of 

Appeals for the District of Columbia 

Circuit by July 18, 2011. Under section 

307(d)(7)(B) of the CAA, only an 

objection to this final rule that was 

raised with reasonable specificity 

during the period for public comment 

can be raised during judicial review. 

Moreover, under section 307(b)(2) of the 

CAA, the requirements established by 

this action may not be challenged 

separately in civil or criminal 

proceedings brought by EPA to enforce 

these requirements. 

II. Background 

This action amends EPA’s Method 

301, Field Validation of Pollutant 

Measurement Methods from Various 

Waste Media. Method 301 was 

originally promulgated in Appendix A 

of 40 CFR part 63 on June 3, 1991. We 

proposed amendments to Method 301 

on December 22, 2004 (69 FR 76642). 

This action responds to comments 

received on that proposal and corrects 

errors found in the method. 

III. Summary of the Final Method 

You would use Method 301 whenever 

you propose to use a test method to 

meet an EPA compliance requirement 

other than a method required under a 40 

CFR part 63 rule. 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. 

IV. Significant Comments Received on 

the Proposed Amendments to Method 

301 

We proposed 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 (LOD), 

(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. 

The following section provides our 

response to significant comments 

received on the proposed technical 

changes and some inadvertant errors 

that occurred with the restructuring of 

and addition of components to the 

method. 

A. Applicability 

Two commenters requested 

clarification that the final rule changes 

made to Method 301 only apply to 

methods submitted to EPA after 

promulgation of the changes and that 

Method 301 can be used whether or not 

a validated method exists. We are 

clarifying in this final rule that 

amendments to Method 301 do not 

apply to methods submitted for 

approval prior to promulgation. Also, 

Method 301 can be used whether or not 

a validated method exists. This action 

clarifies the effective date of the 

amended Method 301, and Section 1.0 

of the final method clarifies that Method 

301 can be used whether or not a 

validated method exists. 

B. Reference Material 

One commenter provided that, as 

written, reference material is analogous 

to analyte. Inadvertantly, in Section 5 of 

Method 301, ‘‘reference materials’’ was 

followed by ‘‘(analytes).’’ This 

paranthetical was modified for 

clarification purposes as noted below. 

A few commenters expressed concern 

that the standard against which 

precision and bias are compared is not 

required to be compared against a true 

value, usually a traceable standard. We 

agree that the reference material should 

be compared to a traceable standard. 

We have amended Section 5 of the 

final method to state the following: 

You must use reference materials (a 

material or substance whose one or more 

properties are sufficiently homogenous to the 

analyte) that are traceable to a national 

standards body (e.g., National Institute of 

Standards and Technology (NIST)) at the 

level of the applicable emission limitation or 

standard that the subpart in 40 CFR part 63 

requires. 

C. Validation Testing Over a Broad 

Range of Concentrations and Extended 

Period of Time 

One commenter requested that 

validation testing over a broad range of 

concentrations and/or over an extended 

period of time be allowed and 

mentioned that they had developed 

technology that could test over a broad 

range of concentrations for an extended 

time-period. The commenter argued that 

if the accuracy and precision 

requirements can be demonstrated with 

sequential sampling procedures, EPA 

should allow it. We agree with the 

commenter. We have approved methods 

demonstrated with sequential sampling 

to determine the precision of a proposed 

alternative method in the past. The final 

method explicitly states that sequential 

sampling procedures are allowed. 

D. Performance Audit 

One commenter stated that they do 

not agree that the performance audit 

requirements in Section 6 of the 

proposed rule should be included in 

Method 301. The commenter supported 

their position by stating that the audit 

material may not correspond to the 

matrix for which the alternate test 

method was designed, and it is similar 

to having to ask EPA permission to use 

a method that has passed Method 301 

validation criteria. In addition, the 

commenter stated that the 30-day lead 

time for requesting the performance 

audit material reduces an affected 

party’s flexibility in meeting 

performance testing timing 

requirements. 

The function of an audit sample is to 

allow a tester to demonstrate that their 

measurement system, using a wellestablished measurement method, is 

operating within established quality 

assurance limits. If the alternative 

method is being compared to a validated 

test method as part of the Method 301 

validation and an audit sample for the 

validated method exists, then an audit 

should be used for the validated 

method. Since the amendments to 

Method 301 were proposed on 

December 22, 2004, EPA promulgated a 

rule on September 13, 2010 (75 FR 

55636), that moves all discussion of 

audits from the individual rules to the 

General Provisions of Part 63. Therefore, 

we have removed the proposed Section 

6 which discussed performance audits. 

E. Sample Stability Procedures 

We proposed procedures for sample 

stability. Method 301 previously lacked 

specific procedures for ensuring that 

samples collected under proposed 

alternative methods were analyzed 


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within an appropriate time. We revised 

Section 7.4 to include 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 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 

Method 301. 

Several commenters provided 

comments on the minimum and 

maximum storage holding time limits 

specified in Section 7.0 of Method 301. 

Commenters recommended that either 

the minimum and maximum holding 

times be removed and that holding 

times should be defined by the data or 

that they be liberalized (e.g., increase 

the minimum hold time from 24 hours 

to 48 to 72 hours). We agree with the 

commenters and are revising the 

minimum hold time to be seven days. 

The method will also require that the 

samples be analyzed again at the 

proposed maximum storage time or two 

weeks after the initial analysis. 

F. Bias and Precision 

We proposed to change the 

acceptance criteria for the bias in a 

proposed alternative method from ± 30 

percent to ± 10 percent and 

concurrently to eliminate the 

requirement for correcting all data 

collected with the method. We provided 

that we believe that 12 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. 

One commenter stated that they did 

not believe that bias acceptance criteria 

should be changed unless uncertainties 

in the reference value are included in 

determining the significance of 

differences. 

One commenter provided that the 

proposed reduction of bias from ± 30 

percent to ± 10 percent is too stringent. 

One commenter suggested allowing a 

bias of ± 15 percent with no correction 

factors while continuing to allow a bias 

of ± 30 percent with the use of 

correction factors for bias values 

between 15 percent and 30 percent. The 

commenter provided a summary of EPA 

Method 301 validations of several 

methods to support their position. 

We agree that reducing the acceptable 

bias to ± 10 percent may be too stringent 

because there may be testing situations 

that are so difficult that there are no 

methods readily available that could 

meet this requirement. We believe that 

a reasonable solution is to allow 

methods that have a bias greater than 

10 percent if the results from these 

methods are corrected to account for 

that bias. However, we believe that we 

should not approve the use of methods 

with greater than 30 percent bias even 

if the user was willing to correct the 

results. We have changed the final 

method to allow a bias of ± 10 percent 

with no correction factors and allow a 

bias of ± 30 percent with the use of 

correction factors for bias values 

between 10 percent and 30 percent. 

We proposed to change the 

acceptance criteria for method precision 

when using analyte spiking from ± 50 

percent to ± 20 percent. In addition, we 

proposed to eliminate the requirement 

for different numbers of replicate 

samples depending on the method’s 

relative precision. We also proposed to 

tighten the acceptance criteria for the 

precision of candidate alternative test 

methods. 

One commenter stated that the 

proposed reduction of precision criteria 

from ± 50 percent to ± 20 percent is too 

stringent. The commenter suggested 

allowing a precision of ± 30 percent 

with no use of replicate runs and the 

continued allowance of a precision of 

± 50 percent with the use of additional 

sample runs for precision values 

between 30 percent and 50 percent. The 

commenter provided a summary of EPA 

Method 301 validations of several 

methods to support their position. 

Based on our evaluation of the 

summary provided by the commenter 

and their suggestion, we have changed 

the final method. The method will 

continue to require a precision of ± 20 

percent when only the required three 

runs per test are performed. However, 

we have added an option to allow test 

methods with a precision greater than 

± 20 percent, but less than ± 50 percent, 

provided that the user collect nine 

sample runs per test during any 

compliance testing where the method is 

used. 

G. Limit of Detection 

We proposed to replace the 

determination of the PLQ with a 

procedure to determine the 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. We provided that for most 

environmental measurements, it appears 

that 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, we stated that the PLQ 

has no meaning. Several commenters 

disagreed that the PLQ is a meaningless 

concept and that there are instances that 

substituting the LOD for the PLQ is not 

always appropriate. Some of these 

commenters stated that the Office of 

Water formed a Federal Advisory 

Committee Act (FACA) Committee to 

consider alternative approaches to 

similar procedures they proposed (40 

CFR part 136 Appendix B) and that 

Method 301 should be deferred until 

after those discussions have concluded 

and that consistent application be 

applied across the Agency based on 

those discussions. 

The PLQ is a limit determined by the 

standard deviation of an estimate of a 

concentration; if the standard deviation 

of the estimate exceeds a threshold, then 

that estimate is unacceptable. The LOD 

is a limit determined by the estimate of 

the concentration itself. If this estimate 

possesses a value that cannot be 

distinguished from an estimate resulting 

from a blank sample with a stated level 

of confidence, then this estimate is 

unacceptable. The LOD is clearly a 

threshold that should be used in 

Method 301 since an estimate that 

cannot be distinguished from one 

resulting from a blank sample is 

unlikely to provide meaningful results. 

The PLQ does not appear to have any 

relevance for Method 301. There does 

not appear to be a good reason for a 

method that produces a standard 

deviation that exceeds an established 

threshold to not go through the full rigor 

of the bias and precision tests 

prescribed in Method 301. For these 

reasons, Method 301 retains the use of 

the LOD in lieu of the PLQ. 

One commenter provided that the 

proposed LOD determination does not 

appear appropriate for radiochemical 

methods and suggested that the content 

of the Multi-Agency Radiological 

Laboratory Analytical Protocols Manual 

(MARLAP) be used. We agree with the 

commenter and have amended Method 

301 to allow for the use of the MARLAP 

for radiochemical methods. 

A few commenters requested that the 

calculation of the LOD be better defined 

and clarified in Table 4 of the method. 

One commenter expressed that the 

description of the procedures used for 

estimating the standard deviation at 

zero concentration (S0) in Table 4 needs 

to be clarified. 

The LOD is defined as the lowest 

quantity of a substance that can be 

distinguished from the absence of that 

substance (i.e., blank value) with a 


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stated level of confidence. For example, 

suppose blank samples are normally 

distributed, and S0 represents the 

standard deviation of the blank samples 

(i.e., the standard deviation of pure 

‘‘noise’’). Then a sample value larger 

than 3S0 will have a probability of not 

being a blank of at least 99 percent if S0

is estimated with at least 14 degrees of 

freedom (or at least 7 degrees of freedom 

if a 1-sided alternative hypothesis is 

assumed). If S0 is ‘‘known’’, then the 

probability will be 99.74 percent, but 

this is often truncated to 99 percent. 

The method for obtaining S0 has been 

clarified to proceed as follows: 

(1) Pick a concentration level that you 

think should approximate the LOD and 

call this level LOD1. Prepare seven 

samples of a standard set at a 

concentration of LOD1. Estimate the 

standard deviation of these seven 

samples, and call it S1. 

(2) Define LOD0 = 3S1. 

(3) If LOD1 ≤ 2LOD0, then define S0 = 

S1. 

(4) If LOD1 > 2LOD0, then proceed as 

follows: 

a. Prepare two additional standards at 

concentrations lower than LOD1, and 

call these LOD2 and LOD3. Prepare 

seven samples of each of these two 

standards and estimate their standard 

deviations and call them S2 and S3, 

respectively. 

b. Plot S1, S2, and S3 as a function of 

concentration, draw a best-fit straight 

line through them, and extrapolate to 

zero concentration. 

c. Define S0 as the extrapolation of the 

standard deviation at zero 

concentration. 

H. Critical Values of t for the TwoTailed 95 Percent Confidence Limit 

Two commenters provided that the 

values of t for the two-tailed 95 percent 

confidence limit are wrong since they 

reflected an 80 percent confidence limit 

and there are some apparent typesetting 

errors. We corrected these values to 

reflect the 95 percent confidence limit 

and eliminated the typesetting errors in 

the final method. 

I. Paired Sampling Procedure 

Two commenters pointed out several 

errors and expressed concerns with the 

methods to ascertain and test precision 

in Section 12. 

Upon evaluation, we have decided to 

revise Section 12.2 in Method 301. We 

are deleting the comparison of the 

precision of the alternative method to 

that of the validated method. This 

decision was made because the paired 

sampling method described in it does 

not allow for the estimation of the 

within-sample standard deviation for 

either the alternative or validated 

methods. 

J. Standard Deviation 

One commenter expressed that the 

precision is a function of concentration; 

in other words, as the concentration 

level increases, so does the standard 

deviation of the estimate of that 

concentration. This could render the 

relative standard deviation (Eq. 301–8 in 

Section 10.4) meaningless. 

A second commenter also expressed 

that the standard deviation is a function 

of concentration. This commenter noted 

that pollutant concentrations from an 

emission source are variable, resulting 

in a range of possible concentration 

values being measured. The commenter 

suggested that the appropriate 

procedure to compare two methods 

under these circumstances is to compare 

the regression lines of the two methods 

across a range of concentrations. 

We agree that this could be a 

potentially serious concern if there is 

little control over the concentrations 

being measured. However, if there is an 

appropriate level of control, then the 

procedures given in Method 301 are 

sufficient. In most situations, we believe 

that an appropriate level of control 

exists. For example, consider the case 

where an alternative method is 

compared against a validated method 

using quadruple samples. We believe 

that an appropriate level of control 

exists if the following four conditions 

are met: (1) There is positive correlation 

between the estimates within both 

alternative and validated pairs in the 

quadruple samples, and the respective 

correlation coefficients are reasonably 

constant as a function of concentration; 

(2) there is positive correlation between 

the alternative and validated estimates 

in the quadruple samples, and the 

correlation coefficient is reasonably 

constant as a function of concentration; 

(3) the within-quadruple sample 

concentrations are reasonably similar; 

and (4) if the between-quadruple sample 

concentrations vary greatly, then the 

functional relationship between the 

standard deviation and concentration is 

reasonably similar for both the 

alternative and validated methods. We 

believe that these four conditions hold, 

for most cases, and an appropriate level 

of control exists. If one or more of these 

conditions is violated, then the user 

may request that they be allowed to 

compare the regression lines resulting 

from the alternative and validated 

estimates as a function of concentration 

as an alternative to the requirements in 

Method 301. 

V. Statutory and Executive Order 

Reviews 

A. Executive Order 12866—Regulatory 

Planning and Review and Executive 

Order 13563—Improving Regulation 

and Regulatory Review 

This action is not a ‘‘significant 

regulatory action’’ under the terms of 

Executive Order 12866 (58 FR 51735, 

October 4, 1993) and is therefore not 

subject to review under Executive 

Orders 12866 and 13563 (76 FR 3821, 

January 21, 2011). 

B. Paperwork Reduction Act 

This action does not impose an 

information collection burden under the 

provisions of the Paperwork Reduction 

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

defined at 5 CFR 1320.3(b). We are not 

promulgating any new paperwork 

requirements (e.g., monitoring, 

reporting, recordkeeping) as part of this 

final action. This final rule amends 

Method 301 which may be used to 

validate test data or a new test method. 

C. Regulatory Flexibility Analysis 

The Regulatory Flexibility Act (RFA) 

generally requires an agency to prepare 

a regulatory flexibility analysis of any 

rule subject to notice and comment 

rulemaking requirements under the 

Administrative Procedure Act or any 

other statute unless the agency certifies 

that the rule will not have a significant 

economic impact on a substantial 

number of small entities. Small entities 

include small businesses, small 

organizations, and small governmental 

jurisdictions. 

For purposes of assessing the impacts 

of this action on small entities, a small 

entity is defined as: (1) A small business 

as defined by the Small Business 

Administration’s (SBA) regulations at 13 

CFR 121.201; (2) a small governmental 

jurisdiction that is a government of a 

city, county, town, school district or 

special district with a population of less 

than 50,000; and (3) a small 

organization that is any not-for-profit 

enterprise that is independently owned 

and operated and is not dominant in its 

field. 

After considering the economic 

impacts of this final rule on small 

entities, I certify that this action will not 

have a significant economic impact on 

a substantial number of small entities. 

This final rule will not impose any 

requirements on small entities. Small 

entities may chose to use this regulatory 

option of validating their own new or 

alternative compliance test method, but 

they are not required to choose this 

option. Any small entity choosing to use 

Method 301 to validate a new or 


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alternative test method would likely do 

so because this option is less 

burdensome than the original method in 

the regulations. 

D. Unfunded Mandates Reform Act 

This action contains no Federal 

mandates under the provisions of Title 

II of the Unfunded Mandates Reform 

Act of 1995 (UMRA), 2 U.S.C. 1531– 

1538 for State, local, or Tribal 

governments or the private sector. This 

action imposes no enforceable duty on 

any State, local or Tribal governments or 

the private sector. Therefore, this action 

is not subject to the requirements of 

sections 202 or 205 of the UMRA. This 

action is also not subject to the 

requirements of section 203 of UMRA 

because it contains no regulatory 

requirements that might significantly or 

uniquely affect small governments. Any 

small entity that chooses to use Method 

301 would likely do so because this 

option is less burdensome. 

E. Executive Order 13132—Federalism 

This action does not have federalism 

implications. It will not have substantial 

direct effects on the States, on the 

relationship between the national 

government and the States, or on the 

distribution of power and 

responsibilities among the various 

levels of government, as specified in 

Executive Order 13132. This final rule 

simply amends Method 301 which may 

be used to validate test data or a new 

test method. 

F. Executive Order 13175—Consultation 

and Coordination With Indian Tribal 

Governments 

This action does not have Tribal 

implications, as specified in Executive 

Order 13175 (65 FR 67429, November 9, 

2000). This final rule amends Method 

301 which can be used to validate a new 

or alternative compliance test method. It 

does not add any new requirements and 

does not affect pollutant emissions or 

air quality. Thus, Executive Order 13175 

does not apply to this action. 

Although EO 13175 does not apply to 

this final rule, EPA specifically solicited 

comment on the proposed rule from 

Tribal officials. No comments were 

received. 

G. Executive Order 13045—Protection of 

Children From Environmental Health 

Risks and Safety Risks 

EPA interprets EO 13045 (62 FR 

19885, April 23, 1997) as applying only 

to those regulatory actions that concern 

health or safety risks, such that the 

analysis required under section 5–501 of 

the EO has the potential to influence the 

regulation. This action is not subject to 

EO 13045 because it does not establish 

an environmental standard intended to 

mitigate health or safety risks. 

H. Executive Order 13211—Actions 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution, or Use 

This action is not subject to Executive 

Order 13211, (66 FR 28355 (May 22, 

2001)) because it is not a significant 

regulatory action under Executive Order 

12866. 

I. National Technology Transfer and 

Advancement Act 

Section 12(d) of the National 

Technology Transfer and Advancement 

Act of 1995 (NTTAA), Public Law 104– 

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

EPA to use voluntary consensus 

standards in its regulatory activities 

unless to do so would be inconsistent 

with applicable law or otherwise 

impractical. Voluntary consensus 

standards are technical standards (for 

example, materials specifications, test 

methods, sampling procedures, and 

business practices) that are developed or 

adopted by voluntary consensus 

standards bodies. The NTTAA directs 

EPA to provide Congress, through OMB, 

explanations when the Agency decides 

not to use available and applicable 

voluntary consensus standards. 

This action involves technical 

standards. While EPA has identified 

ASTM D4855–97 as being potentially 

applicable, we have decided not to use 

it in this rulemaking. The use of this 

voluntary consensus standard would 

have been impractical as the ASTM 

standard is less prescriptive than 

Method 301 for many procedures. For 

example, the ASTM standard does not 

require the use of a t-test explicitly to 

test the precision of an alternative 

method, but instead states that a t-test 

or F-test should be used as appropriate. 

The primary difference between the 

ASTM standard and EPA Method 301 is 

that the ASTM standard addresses the 

testing of ‘‘materials’’ rather than 

environmental samples. Therefore, we 

believe the ASTM is impractical as an 

alternative to Method 301. 

J. Executive Order 12898—Federal 

Actions To Address Environmental 

Justice in Minority Populations and 

Low-Income Populations 

Executive Order (EO) 12898 (59 FR 

7629 (Feb. 16, 1994)) establishes Federal 

executive policy on environmental 

justice. Its main provision directs 

Federal agencies, to the greatest extent 

practicable and permitted by law, to 

make environmental justice part of their 

mission by identifying and addressing, 

as appropriate, disproportionately high 

and adverse human health or 

environmental effects of their programs, 

policies, and activities on minority 

populations and low-income 

populations in the United States. 

EPA has determined that this final 

rule will not have disproportionately 

high and adverse human health or 

environmental effects on minority or 

low-income populations because it does 

not affect the level of protection 

provided to human health or the 

environment. This action amends a 

method for validating new or alternative 

compliance test methods. It does not 

change any existing rules that limit air 

pollution emission limits. 

K. Congressional Review Act 

The Congressional Review Act, 5 

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

Business Regulatory Enforcement 

Fairness Act of 1996, generally provides 

that before a rule may take effect, the 

agency promulgating the rule must 

submit a rule report, which includes a 

copy of the rule, to each House of the 

Congress and to the Comptroller General 

of the United States. EPA will submit a 

report containing this rule and other 

required information to the U.S. Senate, 

the U.S. House of Representatives, and 

the Comptroller General of the United 

States prior to publication of the rule in 

the Federal Register. A major rule 

cannot take effect until 60 days after it 

is published in the Federal Register. 

This action is not a ‘‘major rule’’ as 

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

will be effective May 18, 2011. 

List of Subjects in 40 CFR Part 63 

Environmental protection, Alternative 

test method, Air pollution control, Field 

validation, Hazardous air pollutants, 

Method 301. 

Dated: May 10, 2011. 

Lisa P. Jackson, 

Administrator. 

For the reasons stated in the 

preamble, title 40, chapter I of the Code 

of the Federal Regulations is 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: 

Appendix A to Part 63—Test Methods 

Method 301—Field Validation of Pollutant 

Measurement Methods From Various Waste 

Media 

Sec. 


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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 

5.0 What reference materials must I use? 

Sampling Procedures 

6.0 What sampling procedures must I use? 

7.0 How do I ensure sample stability? 

Bias and Precision 

8.0 What are the requirements for bias? 

9.0 What are the requirements for 

precision? 

10.0 What calculations must I perform for 

isotopic spiking? 

11.0 What calculations must I perform for 

comparison with a validated method if I 

am using quadruplet replicate sampling 

systems? 

12.0 What calculations must I perform for 

analyte spiking? 

13.0 How do I conduct tests at similar 

sources? 

Optional Requirements 

14.0 How do I use and conduct ruggedness 

testing? 

15.0 How do I determine the Limit of 

Detection (LOD) for the alternative 

method? 

Other Requirements and Information 

16.0 How do I apply for approval to use an 

alternative test method? 

17.0 How do I request a waiver? 

18.0 Where can I find additional 

information? 

Using Method 301 

1.0 What is the purpose of Method 301? 

The purpose of Method 301 is to provide 

a set of procedures that you, the owner or 

operator of an affected source subject to 

requirements under 40 CFR part 63 can use 

to validate an alternative test method to a test 

method required in 40 CFR part 63 or to 

validate a stand-alone alternative test method 

based on established precision and bias 

criteria. If you use Method 301 to validate 

your proposed alternative method, you must 

use the procedures described in this method. 

This method describes the minimum 

procedures that you must use to validate an 

alternative test method to meet 40 CFR part 

63 compliance requirements. If you choose to 

propose a validation method other than 

Method 301, you must submit and obtain the 

Administrator’s approval for the alternative 

validation method. 

2.0 When must I use Method 301? 

If you want to use an alternative test 

method to meet requirements in a subpart of 

40 CFR part 63, you can use Method 301 to 

validate the alternative test method. You 

must request approval to use this alternative 

test method according to the procedures in 

Sections 16 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 for 

alternative test methods. Section 17 describes 

the requirements for obtaining a waiver. 

3.0 What does Method 301 include? 

3.1 Procedures. 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. 

3.2 Definitions. 

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. 

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. 

Alternatively, though it is not required, we 

allow validation testing over a broad range of 

concentrations over an extended time period 

to determine precision of a proposed 

alternative method. Sections 5.0 through 17.0 

describe the procedures in detail. 

Reference Materials 

5.0 What reference materials must I use? 

You must use reference materials (a 

material or substance whose one or more 

properties are sufficiently homogenous to the 

analyte) that are traceable to a national 

standards body (e.g., National Institute of 

Standards and Technology (NIST)) 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. You must 

obtain information about your analyte 

according to the procedures in Sections 5.1 

through 5.4. 

5.1 Exhaust Gas Tests Concentration. 

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 

certification for the analyte concentration 

and stability. 

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. 

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. 

Sampling Procedures 

6.0 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 (or the equivalent). Isotopic sampling 

can only be used for procedures requiring 

mass spectrometry or radiological 

procedures. You must collect samples 

according to the requirements in Table 1. 

You must perform the sampling according to 

the procedures in Sections 6.1 through 6.4. 

6.1 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 

Sections 6.3.1 through 6.3.2 for the 

applicable waste medium. 

6.2 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 6.3. 

6.3 Spiking Procedure. 

6.3.1 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 


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introduced as close to the tip of the sampling 

train as possible. 

6.3.2 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 would be approximately equal 

to the analyte concentration in the stack plus 

the applicable emission standard (corrected 

for spike volume). The volume amount of 

analyte must be less than 10 percent of the 

sample volume. 

6.3.3 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. 

6.3.4 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). 

6.4 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 this 

subsection. You must place the probes in the 

same horizontal plane. 

6.4.1 Paired Sampling Probes. For paired 

sampling probes, the 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 (where 

required) are used. 

6.4.2 Quadruplet Sampling Probes. For 

quadruplet sampling probes, the tips should 

be in a 6.0 cm x 6.0 cm square area measured 

from the center line of the opening of the 

probe tip with a single pitot tube (where 

required) in the center or two pitot tubes 

(where required) with their location on either 

side of the probe tip configuration. You must 

propose an alternative arrangement whenever 

the cross-sectional area of the probe tip 

configuration is approximately five percent 

or more of the stack or duct cross-sectional 

area. 

7.0 How do I ensure sample stability? 

7.1 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 7.2 or 7.3. 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 7.2 or 7.3. The 

minimum storage time should be as soon as 

possible, but no longer than 72 hours after 

collection of the sample. The maximum 

storage time should be no longer than two 

weeks. 

7.2 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. 

7.3 Storage and Sampling Procedures for 

Testing Other Waste Media (e.g., Soil/ 

Sediment, Solid Waste, Water/Liquid). You 

must analyze half of the replicate samples at 

the proposed minimum storage time and the 

other half at the proposed maximum storage 

time or within two weeks of the initial 

analysis to identify the effect of storage times 

on analyte samples. The minimum storage 

time should be as soon as possible, but no 

longer than seven days after collection of the 

sample. 

7.4 Sample Stability. After you have 

conducted sampling and analysis according 

to Section 7.2 or 7.3, compare the results at 

the minimum and maximum storage times. 

Calculate the difference in the results using 

Equation 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. 

7.4.1 Standard Deviation. Determine 

the standard deviation (SDd) of the 

differences (di’s) of the paired samples 

using Equation 301–2. 

Where: 

di = The difference between the results of the 

ith sample, Rmini ¥ Rmaxi. 

dm = The mean of the paired sample 

differences. 

n = Total number of paired samples. 

7.4.2 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 and n ¥ 1 degrees of freedom. 

Calculate the value of the t-statistic 

using Equation 301–3. 

Where: 

n = 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 Section 7.2 or 

7.3 with new samples using shorter 

proposed maximum storage times. 

Bias and Precision 

8.0 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 percent without the use 

of correction factors, and no more than 

± 30 percent with the use of correction 

factors for bias values between 10 and 

30 percent for the alternative test 

method to be acceptable. 

9.0 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. For samples with a precision 

greater than 20 percent but less than 50 


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percent, a minimum of nine sample 

runs will be required. 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 (Section 11.2.2). 

10.0 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 

10.1 through 10.3. 

10.1 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. 

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. 

10.2 Standard Deviation. Calculate 

the standard deviation of the Si values 

according to Equation 301–5. 

Where: 

Si = Measured value of the isotopically 

labeled analyte in the i-th field sample, 

n = Number of isotopically spiked samples, 

12. 

10.3 t Test. Test the bias for 

statistical significance by calculating the 

t-statistic using Equation 301–6. Use the 

standard deviation determined in 

Section 10.2 and the numerical bias 

determined in Section 10.1. 

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 6.2 and 6.4 as required, this 

critical value is 2.201 for the 11 degrees 

of freedom. If the calculated t-value is 

less than the critical value, the bias is 

not statistically significant, and the bias 

of the candidate test method is 

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. 

Where: 

BR = Relative bias. 

If the relative bias is less than or equal 

to ten percent, the bias of the candidate 

test method is acceptable and no 

correction factors are required. If the 

relative bias is greater than 10 percent 

but less than 30 percent, and if you 

correct all future data collected with the 

method for the magnitude of the bias, 

the bias of the candidate test method is 

acceptable. If either of the preceding 

two cases applies, you may continue to 

evaluate the method by calculating its 

precision. If not, the candidate method 

will not meet the requirements of 

Method 301. 

10.4 Relative Standard Deviation. 

Calculate the RSD according to Equation 

301–8. 

Where: 

Sm = 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. 

11.0 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 this 

section. 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. 

11.1 Bias Analysis. Test the bias for 

statistical significance at the 95 percent 

confidence level by calculating the 

t-statistic. 

11.1.1 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 

301–9. 

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. 

2i = Second measured value with the 

alternative test method in the i-th 

sample. 

11.1.2 Standard Deviation of the 

Differences. Calculate the standard 

deviation of the differences, SDd, using 

Equation 301–2. 

11.1.3 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 6.1 and Table 1, n 

equals four. Compare the calculated tstatistic with the critical value of the tVerDate Mar<15>2010 14:51 May 17, 2011 Jkt 223001 PO 00000 Frm 00047 Fmt 4700 Sfmt 4700 E:\FR\FM\18MYR1.SGM 18MYR1

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28672 Federal Register / Vol. 76, No. 96 / Wednesday, May 18, 2011 / Rules and Regulations 

statistic, and determine if the bias is 

significant at the 95 percent confidence 

level. When four runs are conducted, as 

specified in Section 6.2 and Table 1, the 

critical value of the t-statistic is 3.182 

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 301–10. 

Where: 

B = Bias ¥ mean of the di’s. 

VS = Mean measured by the validated 

method. 

If the relative bias is less than or equal 

to 10 percent, the bias of the candidate 

test method is acceptable and no 

correction factors are required. If the 

relative bias is greater than 10 percent 

but less than 30 percent, and if you 

correct all future data collected with the 

method for the magnitude of the bias, 

the bias of the candidate test method is 

acceptable. If either of the preceding 

two cases applies, you may continue to 

evaluate the method by calculating its 

precision. If not, the candidate method 

will not meet the requirements of 

Method 301. 

11.2 Precision. Compare the 

estimated variance (or standard 

deviation) 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. Use 

the value furnished with the method. 

Calculate the estimated variance of the 

validated method using Equation 301– 

11. 

11.2.1 Alternative Test Method 

Variance. Calculate the estimated 

variance of the alternative test method, 

Sp

2, according to Equation 301–11. 

Where: 

di = The difference between the i-th pair of 

samples collected with the alternative 

test method. 

n = Number of samples and the degrees of 

freedom. 

11.2.2 F Test. Determine if the 

estimated variance of the alternative test 

method is greater than that of the 

validated method by calculating the Fvalue using Equation 301–12. 

Where: 

Sp

2 = The estimated variance of the 

alternative method. 

Sv

2 = The estimated variance of the validated 

method. 

Compare the experimental F value 

with the one-sided confidence level for 

F. The one-sided confidence level of 95 

percent for F is 6.388 when the 

procedure specified in Section 6.1 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 candidate test method are 

unacceptable. 

12.0 What calculations must I perform 

for analyte spiking? 

You must analyze the data for analyte 

spike testing according to this section. 

12.1 Bias Analysis. Test the bias for 

statistical significance at the 95 percent 

confidence level by calculating the tstatistic. 

12.1.1 Bias. Determine 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 301–13. 

Where: 

S1i = First measured value of the ith spiked 

sample. 

S2i = Second measured value of the ith 

spiked sample. 

M1i = First measured value of the ith 

unspiked sample. 

M2i = Second measured value of the ith 

unspiked sample. 

CS = Calculted value of the spiked level. 

12.1.2 Standard Deviation of the 

Differences. Calculate the standard 

deviation of the differences, SDd, using 

Equation 301–2. 

12.1.3 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 Table 1, n equals six. 

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 six 

runs are conducted, as specified in 

Table 1, the two-sided confidence level 

critical value is 2.571 for the five 

degrees of freedom. If the relative bias 

is less than or equal to 10 percent with 

no correction factors, or the bias is 

greater than 10 percent but less than 30 

percent with the use of correction 

factors, then the data are acceptable. 

Proceed to evaluate precision of the 

candidate test method. 

Where: 

B = Bias ¥ mean of the di’s. 

VS = Mean measured by the validated 

method. 

12.2 Precision. Calculate the standard 

deviation and the relative standard deviation 

of the candidate test method. The relative 

standard deviation of the candidate test 

method can be calculated using Equation 

301–8. 

13.0 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 

Section 17.1.1, 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 

14.0 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 18.16 of Section 18.0 and submit a 

request for a waiver according to Section 

17.1.1. 

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 


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Federal Register / Vol. 76, No. 96 / Wednesday, May 18, 2011 / Rules and Regulations 28673 

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). 

15.0 How do I determine the Limit of 

Detection for the alternative method? 

15.1 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 three 

times the standard deviation, So, at the blank 

level. 

15.2 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. For radiochemical 

methods, use the Multi-Agency Radiological 

Laboratory Analytical Protocols (MARLAP) 

Manual (i.e., use the minimum detectable 

concentration (MDC) and not the LOD) 

available at http://www.epa.gov/radiation/ 

docs/marlap/402-b-04-001c-20_final.pdf. 

Other Requirements and Information 

16.0 How do I apply for approval to use an 

alternative test method? 

16.1 Submitting Requests. You must 

request to use an alternative test method 

according to the procedures in Section 

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 report containing 

the information in Section 16.2. The request 

must be submitted to the Director, Air 

Quality Assessment Division, U.S. 

Environmental Protection Agency, C304–02, 

Research Triangle Park, NC 27711. 

16.2 Field Validation Report. The field 

validation report must contain the 

information in Sections 16.2.1 through 

16.2.8. 

16.2.1 Regulatory objectives for the 

testing, including a description of the reasons 

for the test, applicable emission limits, and 

a description of the source. 

16.2.2 Summary of the results and 

calculations shown in Sections 6.0 through 

16, as applicable. 

16.2.3 Analyte certification and value(s). 

16.2.4 Discussion of laboratory 

evaluations. 

16.2.5 Discussion of field sampling. 

16.2.6 Discussion of sample preparations 

and analysis. 

16.2.7 Storage times of samples (and 

extracts, if applicable). 

16.2.8 Reasons for eliminating any 

results. 

17.0 How do I request a waiver? 

17.1 Conditions for Waivers. If you meet 

one of the criteria in Sections 17.1.1 through 

17.1.2, the Administrator may waive the 

requirement to use the procedures in this 

method to validate an alternative test 

method. In addition, if 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. 

17.1.1 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 Section 14.0. 

17.1.2 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. 

17.2 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, Air Quality 

Assessment Division, U.S. Environmental 

Protection Agency, C304–02, Research 

Triangle Park, NC 27711. 

17.3 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 Sections 17.3.1 

through 17.3.4. The Administrator may 

request additional information if necessary to 

determine whether this method can be 

waived for a particular application. 

17.3.1 A Clearly Written Test Method. 

The method should be written preferably in 

the format of 40 CFR part 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. 

17.3.2 Summaries 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. 

17.3.3 Ruggedness Testing Results. You 

must submit results of ruggedness testing 

conducted according to Section 14.0, sample 

stability conducted according to Section 7.0, 

and detection limits conducted according to 

Section 15.0, 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. 

17.3.4 Applicability Statement and Basis 

for Waiver Approval. Your discussion of the 

applicability statement and basis for approval 

of the waiver should address the following as 

applicable: Applicable regulation, emission 

standards, effluent characteristics, and 

process operations. 

18.0 Where can I find additional 

information? 

You can find additional information in the 

references in Sections 18.1 through 18.16. 

18.1 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. 

18.2 ASTM Standard E 1169–89 (current 

version), ‘‘Standard Guide for Conducting 

Ruggedness Tests,’’ available from ASTM, 

100 Barr Harbor Drive, West Conshohoken, 

PA 19428. 

18.3 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. 

18.4 International Conference on 

Harmonization of Technical Requirements 

for the Registration of Pharmaceuticals for 

Human Use, ICH–Q2A, ‘‘Text on Validation 

of Analytical Procedures,’’ 60 FR 11260 

(March 1995). 

18.5 International Conference on 

Harmonization of Technical Requirements 

for the Registration of Pharmaceuticals for 

Human Use, ICH–Q2b, ‘‘Validation of 

Analytical Procedures: Methodology,’’ 62 FR 

27464 (May 1997). 

18.6 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. 

18.7 Maxwell, E.A. 1974. Estimating 

variances from one or two measurements on 

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

18.8 Midgett, M.R. 1977. How EPA 

Validates NSPS Methodology. Environ. Sci. & 

Technol. 11(7):655–659. 

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

1976. Means to evaluate performance of 

stationary source test methods. Environ. Sci. 

& Technol. 10:85–88. 

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

1946. The design of optimum multifactorial 

experiments. Biometrika, 33:305. 

18.11 Taylor, J.K. 1987. Quality 

Assurance of Chemical Measurements. Lewis 

Publishers, Inc., pp. 79–81. 

18.12 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. 

18.13 U.S. Environmental Protection 

Agency. 1981. A Procedure for Establishing 

Traceability of Gas Mixtures to Certain 


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28674 Federal Register / Vol. 76, No. 96 / Wednesday, May 18, 2011 / Rules and Regulations 

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. 

18.14 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. 

18.15 Wernimont, G.T., ‘‘Use of Statistics 

to Develop and Evaluate Analytical 

Methods,’’ AOAC, 1111 North 19th Street, 

Suite 210, Arlington, VA 22209. USA, 78–82 

(1987). 

18.16 Youden, W.J. Statistical techniques 

for collaborative tests. Statistical Manual of 

the Association of Official Analytical 

Chemists, Association of Official Analytical 

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

TABLE 1 OF APPENDIX A—SAMPLING PROCEDURES

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

comparing against a validated method .............. 9 sets of replicate samples using a paired sampling system (a total of 18 samples) or 4 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. 

using isotopic spiking (can only be used for procedures requiring mass spectrometry).a total of 12 replicate samples. You may collect the samples either by obtaining 6 sets of 

paired samples or 3 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 ............................................ 12.706 

2 ............................................ 4.303 

3 ............................................ 3.182 

4 ............................................ 2.776 

5 ............................................ 2.571 

TABLE 2 OF APPENDIX A—CRITICAL

VALUES OF t FOR THE TWO TAILED

95 PERCENT CONFIDENCE LIMIT— 

Continued 

Degrees of freedom t95

6 ............................................ 2.447 

7 ............................................ 2.365 

8 ............................................ 2.306 

TABLE 2 OF APPENDIX A—CRITICAL

VALUES OF t FOR THE TWO TAILED

95 PERCENT CONFIDENCE LIMIT— 

Continued 

Degrees of freedom t95

9 ............................................ 2.262 

10 .......................................... 2.228 

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

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

using isotopic or analyte spiking procedures ..... sample container (bag or canister) and impinger sampling systems.analyze 6 of the samples within 7 days and 

then analyze the same 6 samples at the 

proposed maximum storage time or 2 

weeks after the initial analysis. 

sorbent and impinger sampling systems that 

require extraction or digestion.

extract or digest 6 of the samples within 7 

days and extract or digest 6 other samples 

at the proposed maximum storage time or 2 

weeks after the first extraction or digestion. 

Analyze an aliquot of the first 6 extracts 

(digestates) within 7 days and proposed 

maximum storage times or 2 weeks after 

the initial analysis. This will allow analysis 

of extract storage impacts. 

sorbent sampling systems that require thermal 

desorption.

analyze 6 samples within 7 days. Analyze another set of 6 samples at the proposed 

maximum storage time or within 2 weeks of 

the initial analysis. 

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) within 7 

days and half of the samples (8 or 9) at the 

proposed maximum storage time or within 2 

weeks of the initial analysis. 

sorbent and impinger sampling systems that 

require extraction or digestion.

extract or digest 6 of the samples within 7 

days and extract or digest 6 other samples 

at the proposed maximum storage time or 

within 2 weeks of the first extraction or digestion. Analyze an aliquot of the first 6 extracts (digestates) within 7 days and at the 

proposed maximum storage times or within 

2 weeks of the initial analysis. This will 

allow analysis of extract storage impacts. 


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Federal Register / Vol. 76, No. 96 / Wednesday, May 18, 2011 / Rules and Regulations 28675 

TABLE 4 OF APPENDIX A—PROCEDURES FOR ESTIMATING So

If the estimated LOD (LOD1, expected approximate LOD concentration 

level) is no more than twice the calculated LOD, use Procedure I as 

follows. Estimate the LOD (LOD1) and prepare a test standard at this 

level. The test standard could consist of a dilution of the analyte described in Section 5.0.

If the estimated LOD (LOD1, expected approximate LOD concentration 

level) is greater than twice the calculated LOD, use Procedure II as 

follows. Prepare two additional standards (LOD2 and LOD3) at concentration levels lower than the standard used in Procedure I 

(LOD1). 

Using the normal sampling and analytical procedures for the method, 

sample and analyze this standard at least 7 times in the laboratory.

Sample and analyze each of these standards (LOD2 and LOD3) at 

least 7 times. 

Calculate the standard deviation, S1, of the measured values ................ Calculate the standard deviation (S2 and S3) for each concentration 

level. 

Calculate the LOD0 (referred to as the calculated LOD) as 3 times S1, 

where S0 = S1.

Plot the standard deviations of the three test standards (S1, S2 and S3) 

as a function of concentration. 

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 LOD0 (referred to as the calculated LOD) as 3 times So. 

* * * * * 

[FR Doc. 2011–12058 Filed 5–17–11; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 180 

[EPA–HQ–OPP–2009–0263; FRL–8865–8] 

Spirotetramat; Pesticide Tolerances 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: This regulation establishes 

tolerances for residues of spirotetramat, 

including its metabolites and 

degradates, in or on multiple 

commodities which are identified and 

discussed later in this document. Bayer 

CropScience requested these tolerances 

under the Federal Food, Drug, and 

Cosmetic Act (FFDCA). 

DATES: This regulation is effective May 

18, 2011. Objections and requests for 

hearings must be received on or before 

July 18, 2011, and must be filed in 

accordance with the instructions 

provided in 40 CFR part 178 (see also 

Unit I.C. of the SUPPLEMENTARY

INFORMATION). 

ADDRESSES: EPA has established a 

docket for this action under docket 

identification (ID) number EPA–HQ– 

OPP–2009–0263. All documents in the 

docket are listed in the docket index 

available at http://www.regulations.gov. 

Although listed in the index, some 

information is not publicly available, 

e.g., Confidential Business Information 

(CBI) or other information whose 

disclosure is restricted by statute. 

Certain other material, such as 

copyrighted material, is not placed on 

the Internet and will be publicly 

available only in hard copy form. 

Publicly available docket materials are 

available in the electronic docket at 

http://www.regulations.gov, or, if only 

available in hard copy, at the OPP 

Regulatory Public Docket in Rm. S– 

4400, One Potomac Yard (South Bldg.), 

2777 S. Crystal Dr., Arlington, VA. The 

Docket Facility is open from 8:30 a.m. 

to 4 p.m., Monday through Friday, 

excluding legal holidays. The Docket 

Facility telephone number is (703) 305– 

5805. 

FOR FURTHER INFORMATION CONTACT: Rita 

Kumar, Registration Division (7505P), 

Office of Pesticide Programs, 

Environmental Protection Agency, 1200 

Pennsylvania Ave., NW., Washington, 

DC 20460–0001; telephone number: 

(703) 308–8291; e-mail address: 

kumar.rita@epa.gov. 

SUPPLEMENTARY INFORMATION: 

I. General Information 

A. Does this action apply to me? 

You may be potentially affected by 

this action if you are an agricultural 

producer, food manufacturer, or 

pesticide manufacturer. Potentially 

affected entities may include, but are 

not limited to those engaged in the 

following activities: 

• Crop production (NAICS code 111). 

• Animal production (NAICS code 

112). 

• Food manufacturing (NAICS code 

311). 

• Pesticide manufacturing (NAICS 

code 32532). 

This listing is not intended to be 

exhaustive, but rather to provide a guide 

for readers regarding entities likely to be 

affected by this action. Other types of 

entities not listed in this unit could also 

be affected. The North American 

Industrial Classification System 

(NAICS) codes have been provided to 

assist you and others in determining 

whether this action might apply to 

certain entities. If you have any 

questions regarding the applicability of 

this action to a particular entity, consult 

the person listed under FOR FURTHER

INFORMATION CONTACT. 

B. How can I get electronic access to 

other related information? 

You may access a frequently updated 

electronic version of EPA’s tolerance 

regulations at 40 CFR part 180 through 

the Government Printing Office’s e-CFR 

site at http://www.gpoaccess.gov/ecfr. 

To access the harmonized test 

guidelines referenced in this document 

electronically, please go to http:// 

www.epa.gov/ocspp and select ‘‘Test 

Methods & Guidelines.’’ 

C. How can I file an objection or hearing 

request? 

Under FFDCA section 408(g), 21 

U.S.C. 346a, any person may file an 

objection to any aspect of this regulation 

and may also request a hearing on those 

objections. You must file your objection 

or request a hearing on this regulation 

in accordance with the instructions 

provided in 40 CFR part 178. To ensure 

proper receipt by EPA, you must 

identify docket ID number EPA–HQ– 

OPP–2009–0263 in the subject line on 

the first page of your submission. All 

objections and requests for a hearing 

must be in writing, and must be 

received by the Hearing Clerk on or 

before July 18, 2011. Addresses for mail 

and hand delivery of objections and 

hearing requests are provided in 40 CFR 

178.25(b). 

In addition to filing an objection or 

hearing request with the Hearing Clerk 

as described in 40 CFR part 178, please 

submit a copy of the filing that does not 

contain any CBI for inclusion in the 

public docket. Information not marked 

confidential pursuant to 40 CFR part 2 

may be disclosed publicly by EPA 

without prior notice. Submit a copy of 

your non-CBI objection or hearing 

request, identified by docket ID number 

EPA–HQ–OPP–2009–0263, by one of 

the following methods: 


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