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dates, it is reasonable for the EPA toexercise its authority to delay theeffective dates of the Major SourceBoiler MACT and the CISWI Rule underthe APA for a period that exceeds threemonths.

II. Issuance of a Stay and Delay ofEffective Date

Pursuant to section 705 of the APA,the EPA hereby postpones theeffectiveness of the Major Source BoilerMACT and the CISWI Rule until theproceedings for judicial review of theserules are complete or the EPA completesits reconsideration of the rules,whichever is earlier. By this action, weare delaying the effective date of bothrules, published in the Federal Registeron March 21, 2011 (76 FR 15608 and 76FR 15704). The delay of the effectivedate of the CISWI Rule applies only tothose provisions issued on March 21,

2011, and not to any provisions of 40CFR part 60, subparts CCCC and DDDD,in place prior to that date. This delay ofeffectiveness will remain in place untilthe proceedings for judicial review arecompleted or the EPA completes itsreconsideration of the rules, whicheveris earlier, and the Agency publishes anotice in the Federal Registerannouncing that the rules are in effect.

List of Subjects

40 CFR Part 60

Environmental protection,

Administrative practice and procedure,Air pollution control, Incorporation byreference, Intergovernmental relations,Reporting and recordkeepingrequirements.

40 CFR Part 63

Environmental protection,Administrative practice and procedure,Air pollution control, Hazardoussubstances, Incorporation by reference,Intergovernmental relations, Reportingand recordkeeping requirements.

For the reasons set forth above, under

the authority at 7 U.S.C. 705, theeffective dates of FRL 92728, 76 FR15608 (March 21, 2011), and FRL 92734, 76 FR 15704 (March 21, 2011) aredelayed until further notice.

Dated: May 16, 2011.

Lisa P. Jackson,

Administrator.

[FR Doc. 201112308 Filed 51711; 8:45 am]

BILLING CODE 656050P

ENVIRONMENTAL PROTECTIONAGENCY

40 CFR Part 63

[OAR20040080, FRL93068]

RIN 2060AF00

Method 301Field Validation of

Pollutant Measurement Methods FromVarious Waste Media

AGENCY: Environmental ProtectionAgency (EPA).ACTION: Final rule.

SUMMARY: This action amends EPAsMethod 301, Field Validation ofPollutant Measurement Methods fromVarious Waste Media. We revised theprocedures in Method 301 based on ourexperience in applying the method andto correct errors that were brought to ourattention. The revised Method 301 ismore flexible, less expensive, and easier

to use. This action finalizesamendments to Method 301 afterconsidering comments received on theproposed rule published in the FederalRegister on December 22, 2004.DATES: This final rule is effective onMay 18, 2011.ADDRESSES: EPA has established adocket for this action under Docket IDNo. EPAHQOAR20040080. Alldocuments in the docket are listed inthe http://www.regulations.govindex.Although listed in the index, someinformation is not publicly available,e.g., confidential business information

(CBI) or other information whosedisclosure is restricted by statute.Certain other material, such ascopyrighted material, is not placed onthe Internet and will be publiclyavailable only in hard copy form.Publicly available docket materials areavailable either electronically at http://www.regulations.govor in hard copy atthe Air Docket, EPA/DC, EPA West,Room 3334, 1301 Constitution Avenue,NW., Washington, DC. The DocketFacility and the Public Reading Roomare open from 8:30 a.m. to 4:30 p.m.,Monday through Friday, excluding legalholidays. The telephone number for thePublic Reading Room is (202) 5661744,and the telephone number for the AirDocket is (202) 5661742.FOR FURTHER INFORMATION CONTACT: Ms.Lula H. Melton, Office of Air QualityPlanning and Standards, Air QualityAssessment Division, MeasurementTechnology Group (E14302), U.S.Environmental Protection Agency,Research Triangle Park, North Carolina27711; telephone number: (919) 5412910; fax number: (919) 5410516;e-mail address: [email protected].

SUPPLEMENTARY INFORMATION:

Table of Contents

I. General InformationA. Does this action apply to me?B. Where can I obtain a copy of this action?C. Judicial Review

II. BackgroundIII. Summary of the Final MethodIV. Significant Comments Received on the

Proposed Amendments to Method 301A. ApplicabilityB. Reference MaterialC. Validation Testing Over a Broad Range

of Concentrations and Extended Periodof Time

D. Performance AuditE. Sample Stability ProceduresF. Bias and PrecisionG. Limit of DetectionH. Critical Values of t for the Two-Tailed

95 Percent Confidence LimitI. Paired Sampling Procedure

J. Standard DeviationV. Statutory and Executive Order Reviews

A. Executive Order 12866RegulatoryPlanning and Review and Executive

Order 13563Improving Regulation andRegulatory Review

B. Paperwork Reduction ActC. Regulatory Flexibility ActD. Unfunded Mandates Reform ActE. Executive Order 13132FederalismF. Executive Order 13175Consultation

and Coordination With Indian TribalGovernments

G. Executive Order 13045Protection ofChildren From Environmental HealthRisks and Safety Risks

H. Executive Order 13211ActionsConcerning Regulations ThatSignificantly Affect Energy Supply,Distribution or Use

I. National Technology Transfer and

Advancement ActJ. Executive Order 12898Federal Actions

To Address Environmental Justice inMinority Populations and Low-IncomePopulations

K. Congressional Review Act

I. General Information

A. Does this action apply to me?

Method 301 affects/applies to you ifyou want to propose a new oralternative test method to meet an EPAcompliance requirement.

B. Where can I obtain a copy of thisaction?

In addition to being available in thedocket, an electronic copy of this rulewill also be available on the WorldwideWeb (www) through the TechnologyTransfer Network (TTN). Following theAdministrators signature, a copy of thefinal rule will be placed on the TTNspolicy and guidance page for newlyproposed or promulgated rules athttp://www.epa.gov/ttn/oarpg.The TTNprovides information and technologyexchange in various areas of airpollution control. A redline strikeout

VerDate Mar2010 14:51 May 17, 2011 Jkt 223001 PO 00000 Frm 00040 Fmt 4700 Sfmt 4700 E:\FR\FM\18MYR1.SGM 18MYR1
http://www.regulations.gov/http://www.regulations.gov/http://www.regulations.gov/mailto:[email protected]://www.epa.gov/ttn/oarpgmailto:[email protected]://www.regulations.gov/http://www.regulations.gov/http://www.regulations.gov/http://www.epa.gov/ttn/oarpg

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document that compares this final ruleto the proposed rule has also beenadded to the docket.

C. Judicial Review

Under section 307(b)(1) of the CleanAir Act (CAA), judicial review of thisfinal rule is available by filing a petitionfor review in the United States Court of

Appeals for the District of ColumbiaCircuit by July 18, 2011. Under section307(d)(7)(B) of the CAA, only anobjection to this final rule that wasraised with reasonable specificityduring the period for public commentcan be raised during judicial review.Moreover, under section 307(b)(2) of theCAA, the requirements established bythis action may not be challengedseparately in civil or criminalproceedings brought by EPA to enforcethese requirements.

II. Background

This action amends EPAs Method301, Field Validation of PollutantMeasurement Methods from VariousWaste Media. Method 301 wasoriginally promulgated in Appendix Aof 40 CFR part 63 on June 3, 1991. Weproposed amendments to Method 301on December 22, 2004 (69 FR 76642).This action responds to commentsreceived on that proposal and correctserrors found in the method.

III. Summary of the Final Method

You would use Method 301 wheneveryou propose to use a test method tomeet an EPA compliance requirement

other than a method required under a 40CFR part 63 rule. The method specifiesprocedures for determining anddocumenting the precision and bias ofmeasured concentrations from variousmedia (e.g., sludge, exhaust gas,wastewater) at the level of an applicablestandard for a source. Bias (or systemicerror) is established by comparing yourproposed method against a referencevalue.

A correction factor is employed toeliminate/minimize bias. Thiscorrection factor is established fromdata obtained during your validation

test. Methods that have bias correctionfactors outside a specified range areconsidered unacceptable. Methodprecision (or random error) at the levelof the standard must be demonstrated to

be as precise as the validated method foracceptance.

IV. Significant Comments Received onthe Proposed Amendments to Method301

We proposed five major technicalchanges to Method 301. These technicalchanges include the following:

(1) Replacing the Practical Limit ofQuantitation (PLQ) with a procedure todetermine the Limit of Detection (LOD),

(2) Revising the bias acceptancecriteria and eliminating correctionfactors,

(3) Revising precision acceptancecriteria when using analyte spiking,

(4) Allowing analyte spiking evenwhen there is an existing test method,and

(5) Establishing new procedures forensuring sample stability.

The following section provides ourresponse to significant commentsreceived on the proposed technicalchanges and some inadvertant errorsthat occurred with the restructuring ofand addition of components to themethod.

A. Applicability

Two commenters requested

clarification that the final rule changesmade to Method 301 only apply tomethods submitted to EPA afterpromulgation of the changes and thatMethod 301 can be used whether or nota validated method exists. We areclarifying in this final rule thatamendments to Method 301 do notapply to methods submitted forapproval prior to promulgation. Also,Method 301 can be used whether or nota validated method exists. This actionclarifies the effective date of theamended Method 301, and Section 1.0of the final method clarifies that Method

301 can be used whether or not avalidated method exists.

B. Reference Material

One commenter provided that, aswritten, reference material is analogousto analyte. Inadvertantly, in Section 5 ofMethod 301, reference materials wasfollowed by (analytes). Thisparanthetical was modified forclarification purposes as noted below.

A few commenters expressed concernthat the standard against whichprecision and bias are compared is notrequired to be compared against a true

value, usually a traceable standard. Weagree that the reference material shouldbe compared to a traceable standard.

We have amended Section 5 of thefinal method to state the following:

You must use reference materials (amaterial or substance whose one or moreproperties are sufficiently homogenous to theanalyte) that are traceable to a nationalstandards body (e.g., National Institute ofStandards and Technology (NIST)) at thelevel of the applicable emission limitation orstandard that the subpart in 40 CFR part 63requires.

C. Validation Testing Over a BroadRange of Concentrations and ExtendedPeriod of Time

One commenter requested thatvalidation testing over a broad range ofconcentrations and/or over an extendedperiod of time be allowed andmentioned that they had developed

technology that could test over a broadrange of concentrations for an extendedtime-period. The commenter argued thatif the accuracy and precisionrequirements can be demonstrated withsequential sampling procedures, EPAshould allow it. We agree with thecommenter. We have approved methodsdemonstrated with sequential samplingto determine the precision of a proposedalternative method in the past. The finalmethod explicitly states that sequentialsampling procedures are allowed.

D. Performance Audit

One commenter stated that they do

not agree that the performance auditrequirements in Section 6 of theproposed rule should be included inMethod 301. The commenter supportedtheir position by stating that the auditmaterial may not correspond to thematrix for which the alternate testmethod was designed, and it is similarto having to ask EPA permission to usea method that has passed Method 301validation criteria. In addition, thecommenter stated that the 30-day leadtime for requesting the performanceaudit material reduces an affectedpartys flexibility in meeting

performance testing timingrequirements.

The function of an audit sample is toallow a tester to demonstrate that theirmeasurement system, using a well-established measurement method, isoperating within established qualityassurance limits. If the alternativemethod is being compared to a validatedtest method as part of the Method 301validation and an audit sample for thevalidated method exists, then an auditshould be used for the validatedmethod. Since the amendments toMethod 301 were proposed on

December 22, 2004, EPA promulgated arule on September 13, 2010 (75 FR55636), that moves all discussion ofaudits from the individual rules to theGeneral Provisions of Part 63. Therefore,we have removed the proposed Section6 which discussed performance audits.

E. Sample Stability Procedures

We proposed procedures for samplestability. Method 301 previously lackedspecific procedures for ensuring thatsamples collected under proposedalternative methods were analyzed


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stated level of confidence. For example,suppose blank samples are normallydistributed, and S0 represents thestandard deviation of the blank samples(i.e., the standard deviation of purenoise). Then a sample value largerthan 3S0 will have a probability of not

being a blank of at least 99 percent if S0is estimated with at least 14 degrees of

freedom (or at least 7 degrees of freedomif a 1-sided alternative hypothesis isassumed). If S0 is known, then theprobability will be 99.74 percent, butthis is often truncated to 99 percent.

The method for obtaining S0 has beenclarified to proceed as follows:

(1) Pick a concentration level that youthink should approximate the LOD andcall this level LOD1. Prepare sevensamples of a standard set at aconcentration of LOD1. Estimate thestandard deviation of these sevensamples, 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, andcall these LOD2 and LOD3. Prepareseven samples of each of these twostandards and estimate their standarddeviations and call them S2 and S3,respectively.

b. Plot S1, S2, and S3 as a function ofconcentration, draw a best-fit straightline through them, and extrapolate tozero concentration.

c. Define S0 as the extrapolation of the

standard deviation at zeroconcentration.

H. Critical Values of t for the Two-Tailed 95 Percent Confidence Limit

Two commenters provided that thevalues of t for the two-tailed 95 percentconfidence limit are wrong since theyreflected an 80 percent confidence limitand there are some apparent typesettingerrors. We corrected these values toreflect the 95 percent confidence limitand eliminated the typesetting errors inthe final method.

I. Paired Sampling Procedure

Two commenters pointed out severalerrors and expressed concerns with themethods to ascertain and test precisionin Section 12.

Upon evaluation, we have decided torevise Section 12.2 in Method 301. Weare deleting the comparison of theprecision of the alternative method tothat of the validated method. Thisdecision was made because the pairedsampling method described in it doesnot allow for the estimation of thewithin-sample standard deviation for

either the alternative or validatedmethods.

J. Standard Deviation

One commenter expressed that theprecision is a function of concentration;in other words, as the concentrationlevel increases, so does the standarddeviation of the estimate of thatconcentration. This could render therelative standard deviation (Eq. 3018 inSection 10.4) meaningless.

A second commenter also expressedthat the standard deviation is a functionof concentration. This commenter notedthat pollutant concentrations from anemission source are variable, resultingin a range of possible concentrationvalues being measured. The commentersuggested that the appropriateprocedure to compare two methodsunder these circumstances is to comparethe regression lines of the two methods

across a range of concentrations.We agree that this could be a

potentially serious concern if there islittle control over the concentrations

being measured. However, if there is anappropriate level of control, then theprocedures given in Method 301 aresufficient. In most situations, we believethat an appropriate level of controlexists. For example, consider the casewhere an alternative method iscompared against a validated methodusing quadruple samples. We believethat an appropriate level of controlexists if the following four conditions

are met: (1) There is positive correlationbetween the estimates within bothalternative and validated pairs in thequadruple samples, and the respectivecorrelation coefficients are reasonablyconstant as a function of concentration;(2) there is positive correlation betweenthe alternative and validated estimatesin the quadruple samples, and thecorrelation coefficient is reasonablyconstant as a function of concentration;(3) the within-quadruple sampleconcentrations are reasonably similar;and (4) if the between-quadruple sampleconcentrations vary greatly, then thefunctional relationship between thestandard deviation and concentration isreasonably similar for both thealternative and validated methods. We

believe that these four conditions hold,for most cases, and an appropriate levelof control exists. If one or more of theseconditions is violated, then the usermay request that they be allowed tocompare the regression lines resultingfrom the alternative and validatedestimates as a function of concentrationas an alternative to the requirements inMethod 301.

V. Statutory and Executive OrderReviews

A. Executive Order 12866RegulatoryPlanning and Review and ExecutiveOrder 13563Improving Regulationand Regulatory Review

This action is not a significantregulatory action under the terms of

Executive Order 12866 (58 FR 51735,October 4, 1993) and is therefore notsubject to review under ExecutiveOrders 12866 and 13563 (76 FR 3821,

January 21, 2011).

B. Paperwork Reduction Act

This action does not impose aninformation collection burden under theprovisions of the Paperwork ReductionAct, 44 U.S.C. 3501 et seq. Burden isdefined at 5 CFR 1320.3(b). We are notpromulgating any new paperworkrequirements (e.g., monitoring,reporting, recordkeeping) as part of thisfinal action. This final rule amendsMethod 301 which may be used tovalidate test data or a new test method.

C. Regulatory Flexibility Analysis

The Regulatory Flexibility Act (RFA)generally requires an agency to preparea regulatory flexibility analysis of anyrule subject to notice and commentrulemaking requirements under theAdministrative Procedure Act or anyother statute unless the agency certifiesthat the rule will not have a significanteconomic impact on a substantialnumber of small entities. Small entitiesinclude small businesses, small

organizations, and small governmentaljurisdictions.

For purposes of assessing the impactsof this action on small entities, a smallentity is defined as: (1) A small businessas defined by the Small BusinessAdministrations (SBA) regulations at 13CFR 121.201; (2) a small governmentaljurisdiction that is a government of acity, county, town, school district orspecial district with a population of lessthan 50,000; and (3) a smallorganization that is any not-for-profitenterprise that is independently ownedand operated and is not dominant in its

field.After considering the economicimpacts of this final rule on smallentities, I certify that this action will nothave a significant economic impact ona substantial number of small entities.This final rule will not impose anyrequirements on small entities. Smallentities may chose to use this regulatoryoption of validating their own new oralternative compliance test method, butthey are not required to choose thisoption. Any small entity choosing to useMethod 301 to validate a new or


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alternative test method would likely doso because this option is less

burdensome than the original method inthe regulations.

D. Unfunded Mandates Reform Act

This action contains no Federalmandates under the provisions of TitleII of the Unfunded Mandates Reform

Act of 1995 (UMRA), 2 U.S.C. 15311538 for State, local, or Tribalgovernments or the private sector. Thisaction imposes no enforceable duty onany State, local or Tribal governments orthe private sector. Therefore, this actionis not subject to the requirements ofsections 202 or 205 of the UMRA. Thisaction is also not subject to therequirements of section 203 of UMRA

because it contains no regulatoryrequirements that might significantly oruniquely affect small governments. Anysmall entity that chooses to use Method301 would likely do so because this

option is less burdensome.E. Executive Order 13132Federalism

This action does not have federalismimplications. It will not have substantialdirect effects on the States, on therelationship between the nationalgovernment and the States, or on thedistribution of power andresponsibilities among the variouslevels of government, as specified inExecutive Order 13132. This final rulesimply amends Method 301 which may

be used to validate test data or a newtest method.

F. Executive Order 13175Consultationand Coordination With Indian TribalGovernments

This action does not have Tribalimplications, as specified in ExecutiveOrder 13175 (65 FR 67429, November 9,2000). This final rule amends Method301 which can be used to validate a newor alternative compliance test method. Itdoes not add any new requirements anddoes not affect pollutant emissions orair quality. Thus, Executive Order 13175does not apply to this action.

Although EO 13175 does not apply tothis final rule, EPA specifically solicited

comment on the proposed rule fromTribal officials. No comments werereceived.

G. Executive Order 13045Protection ofChildren From Environmental HealthRisks and Safety Risks

EPA interprets EO 13045 (62 FR19885, April 23, 1997) as applying onlyto those regulatory actions that concernhealth or safety risks, such that theanalysis required under section 5501 ofthe EO has the potential to influence theregulation. This action is not subject to

EO 13045 because it does not establishan environmental standard intended tomitigate health or safety risks.

H. Executive Order 13211ActionsConcerning Regulations ThatSignificantly 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 significantregulatory action under Executive Order12866.

I. National Technology Transfer andAdvancement Act

Section 12(d) of the NationalTechnology Transfer and AdvancementAct of 1995 (NTTAA), Public Law 104113, 12(d) (15 U.S.C. 272 note) directsEPA to use voluntary consensusstandards in its regulatory activitiesunless to do so would be inconsistentwith applicable law or otherwiseimpractical. Voluntary consensusstandards are technical standards (forexample, materials specifications, testmethods, sampling procedures, and

business practices) that are developed oradopted by voluntary consensusstandards bodies. The NTTAA directsEPA to provide Congress, through OMB,explanations when the Agency decidesnot to use available and applicablevoluntary consensus standards.

This action involves technicalstandards. While EPA has identifiedASTM D485597 as being potentiallyapplicable, we have decided not to useit in this rulemaking. The use of this

voluntary consensus standard wouldhave been impractical as the ASTMstandard is less prescriptive thanMethod 301 for many procedures. Forexample, the ASTM standard does notrequire the use of a t-test explicitly totest the precision of an alternativemethod, but instead states that a t-testor F-test should be used as appropriate.The primary difference between theASTM standard and EPA Method 301 isthat the ASTM standard addresses thetesting ofmaterials rather thanenvironmental samples. Therefore, we

believe the ASTM is impractical as an

alternative to Method 301.J. Executive Order 12898FederalActions To Address Environmental

Justice in Minority Populations andLow-Income Populations

Executive Order (EO) 12898 (59 FR7629 (Feb. 16, 1994)) establishes Federalexecutive policy on environmentaljustice. Its main provision directsFederal agencies, to the greatest extentpracticable and permitted by law, tomake environmental justice part of theirmission by identifying and addressing,

as appropriate, disproportionately highand adverse human health orenvironmental effects of their programs,policies, and activities on minoritypopulations and low-incomepopulations in the United States.

EPA has determined that this finalrule will not have disproportionatelyhigh and adverse human health or

environmental effects on minority orlow-income populations because it doesnot affect the level of protectionprovided to human health or theenvironment. This action amends amethod for validating new or alternativecompliance test methods. It does notchange any existing rules that limit airpollution emission limits.

K. Congressional Review Act

The Congressional Review Act, 5U.S.C. 801 et seq., as added by the SmallBusiness Regulatory EnforcementFairness Act of 1996, generally provides

that before a rule may take effect, theagency promulgating the rule mustsubmit a rule report, which includes acopy of the rule, to each House of theCongress and to the Comptroller Generalof the United States. EPA will submit areport containing this rule and otherrequired information to the U.S. Senate,the U.S. House of Representatives, andthe Comptroller General of the UnitedStates prior to publication of the rule inthe Federal Register. A major rulecannot take effect until 60 days after itis published in the Federal Register.This action is not a major rule asdefined by 5 U.S.C. 804(2). This rulewill be effective May 18, 2011.

List of Subjects in 40 CFR Part 63

Environmental protection, Alternativetest method, Air pollution control, Fieldvalidation, Hazardous air pollutants,Method 301.

Dated: May 10, 2011.

Lisa P. Jackson,

Administrator.

For the reasons stated in thepreamble, title 40, chapter I of the Codeof the Federal Regulations is amendedas follows:

PART 63[AMENDED]

1. The authority citation for part 63continues to read as follows:

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

2. Appendix A is amended by revisingMethod 301 to read as follows:

Appendix A to Part 63Test Methods

Method 301Field Validation of PollutantMeasurement Methods From Various WasteMedia

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 Iam using quadruplet replicate samplingsystems?

12.0 What calculations must I perform foranalyte spiking?

13.0 How do I conduct tests at similarsources?

Optional Requirements

14.0 How do I use and conduct ruggednesstesting?

15.0 How do I determine the Limit ofDetection (LOD) for the alternativemethod?

Other Requirements and Information

16.0 How do I apply for approval to use analternative 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 providea set of procedures that you, the owner oroperator of an affected source subject torequirements under 40 CFR part 63 can useto validate an alternative test method to a testmethod required in 40 CFR part 63 or tovalidate a stand-alone alternative test method

based on established precision and biascriteria. If you use Method 301 to validateyour proposed alternative method, you mustuse the procedures described in this method.This method describes the minimumprocedures that you must use to validate analternative test method to meet 40 CFR part63 compliance requirements. If you choose topropose a validation method other thanMethod 301, you must submit and obtain the

Administrators approval for the alternativevalidation method.

2.0 When must I use Method 301?

If you want to use an alternative testmethod to meet requirements in a subpart of40 CFR part 63, you can use Method 301 tovalidate the alternative test method. Youmust request approval to use this alternativetest method according to the procedures inSections 16 and 63.7(f). You must receive theAdministrators written approval to use thealternative test method before you use thealternative test method to meet requirementsunder 40 CFR part 63. In some cases, the

Administrator may decide to waive therequirement to use Method 301 foralternative test methods. Section 17 describesthe requirements for obtaining a waiver.

3.0 What does Method 301 include?

3.1 Procedures. This method includesminimum procedures to determine anddocument systematic error (bias) and randomerror (precision) of measured concentrations

from exhaust gases, wastewater, sludge, andother media. It contains procedures forensuring sample stability if such proceduresare not included in the test method. Thismethod also includes optional procedures forruggedness and detection limits.

3.2 Definitions.Affected source means affected source as

defined in 40 CFR 63.2 and in the relevantsubpart under 40 CFR part 63.

Alternative test methodmeans thesampling and analytical methodologyselected for field validation using the methoddescribed in this appendix.

Paired sampling system means a samplingsystem capable of obtaining two replicatesamples that were collected as closely as

possible in sampling time and samplinglocation.Quadruplet sampling system means a

sampling system capable of obtaining fourreplicate samples that were collected asclosely as possible in sampling time andsampling location.

Surrogate compoundmeans a compoundthat serves as a model for the types ofcompounds being analyzed (i.e., similarchemical structure, properties, behavior). Themodel can be distinguished by the methodfrom the compounds being analyzed.

4.0 How do I perform Method 301?

First, you introduce a known concentrationof an analyte or compare the alternative testmethod against a validated test method todetermine the alternative test methods bias.Then, you collect multiple, collocatedsimultaneous samples to determine thealternative test methods precision.Alternatively, though it is not required, weallow validation testing over a broad range ofconcentrations over an extended time periodto determine precision of a proposedalternative method. Sections 5.0 through 17.0describe the procedures in detail.

Reference Materials

5.0 What reference materials must I use?

You must use reference materials (amaterial or substance whose one or moreproperties are sufficiently homogenous to the

analyte) that are traceable to a nationalstandards body (e.g., National Institute ofStandards and Technology (NIST)) at thelevel of the applicable emission limitation orstandard that the subpart in 40 CFR part 63requires. If you want to expand theapplicable range of the method, you mustconduct additional runs with higher andlower analyte concentrations. You mustobtain information about your analyteaccording to the procedures in Sections 5.1through 5.4.

5.1 Exhaust Gas Tests Concentration.You must get a known concentration of eachanalyte from an independent source such as

a speciality gas manufacturer, specialtychemical company, or chemical laboratory.You must also get the manufacturerscertification for the analyte concentrationand stability.

5.2 Tests for Other Waste Media. Youmust get the pure liquid components of eachanalyte from an independent manufacturer.The manufacturer must certify the purity andshelf life of the pure liquid components. You

must dilute the pure liquid components inthe same type medium as the waste from theaffected source.

5.3 Surrogate Analytes. If youdemonstrate to the Administratorssatisfaction that a surrogate compound

behaves as the analyte does, then you mayuse surrogate compounds for highly toxic orreactive compounds. A surrogate may be anisotope or one that contains a unique element(for example, chlorine) that is not present inthe source or a derivation of the toxic orreactive compound if the derivativeformation is part of the methods procedure.You may use laboratory experiments orliterature data to show behavioralacceptability.

5.4 Isotopically Labeled Materials.Isotope mixtures may contain the isotope andthe natural analyte. The isotope labeledanalyte concentration must be more than fivetimes the natural concentration of theanalyte.

Sampling Procedures

6.0 What sampling procedures must I use?

You may determine bias and precision bycomparing against a validated test method,using isotopic sampling, or using analytespiking (or the equivalent). Isotopic samplingcan only be used for procedures requiringmass spectrometry or radiologicalprocedures. You must collect samplesaccording to the requirements in Table 1.

You must perform the sampling according tothe procedures in Sections 6.1 through 6.4.

6.1 Isotopic Spiking. Spike all 12 sampleswith the analyte at the concentration in theapplicable emission limitation or standard inthe subpart of 40 CFR part 63. If there is noapplicable emission limitation or standard,spike at the expected level of the samples.Follow the appropriate spiking procedures inSections 6.3.1 through 6.3.2 for theapplicable waste medium.

6.2 Analyte Spiking. In each quadrupletset, spike half of the samples (two out of thefour) with the analyte according to theapplicable procedure in Section 6.3.

6.3 Spiking Procedure.6.3.1 Gaseous Analyte with Sorbent or

Impinger Sampling Trains. Sample theanalyte (in the laboratory or in the field) ata concentration that is close to theconcentration in the applicable emissionlimitation or standard in the subpart of 40CFR Part 63 (or the expected sampleconcentration where there is no standard) forthe time required by the method, and thensample the gas stream for an equal amountof time. The time for sampling both theanalyte and gas stream should be equal;however, the time should be adjusted toavoid sorbent breakthrough. The stack gasand the gaseous analyte may be sampled atthe same time. The analyte must be


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introduced as close to the tip of the samplingtrain as possible.

6.3.2 Gaseous Analyte with SampleContainer (Bag or Canister). Spike the samplecontainers after completion of each test runwith an amount equal to the concentration inthe applicable emission limitation orstandard in the subpart of 40 CFR part 63 (orthe expected sample concentration wherethere is no standard). The final concentration

of the analyte would be approximately equalto the analyte concentration in the stack plusthe applicable emission standard (correctedfor spike volume). The volume amount ofanalyte must be less than 10 percent of thesample volume.

6.3.3 Liquid and Solid Analyte withSorbent or Impinger Trains. Spike the trainswith an amount equal to the concentration inthe applicable emission limitation orstandard in the subpart of 40 CFR part 63 (orthe expected sample concentration wherethere is no standard) before sampling thestack gas. If possible, do the spiking in thefield. If it is not possible to do the spikingin the field, you can do it in the laboratory.

6.3.4 Liquid and Solid Analyte with

Sample Container (Bag or Canister). Spikethe containers at the completion of each testrun with an amount equal to theconcentration in the applicable emissionlimitation or standard in the subpart of 40CFR part 63 (or the expected sampleconcentration where there is no standard).

6.4 Probe Placement and Arrangementfor Stationary Source Stack or DuctSampling. To sample a stationary source asdefined in 40 CFR 63.2, you must place theprobe according to the procedures in thissubsection. You must place the probes in thesame horizontal plane.

6.4.1 Paired Sampling Probes. For pairedsampling probes, the probe tip should be 2.5cm from the outside edge of the other sampleprobe, with a pitot tube on the outside ofeach probe. The Administrator may approvea validation request where other pairedarrangements for the pitot tube (whererequired) are used.

6.4.2 Quadruplet Sampling Probes. Forquadruplet sampling probes, the tips should

be in a 6.0 cm x 6.0 cm square area measuredfrom the center line of the opening of theprobe tip with a single pitot tube (whererequired) in the center or two pitot tubes(where required) with their location on eitherside of the probe tip configuration. You mustpropose an alternative arrangement wheneverthe cross-sectional area of the probe tipconfiguration is approximately five percentor more of the stack or duct cross-sectionalarea.

7.0 How do I ensure sample stability?

7.1 Developing Storage and AnalysisProcedures. If the alternative test methodincludes well-established proceduressupported by experimental data for samplestorage and the time within which thecollected samples must be analyzed, youmust store the samples according to theprocedures in the alternative test method.You are not required to conduct theprocedures in Section 7.2 or 7.3. If thealternative test method does not include suchprocedures, you must propose procedures forstoring and analyzing samples to ensuresample stability. At a minimum, yourproposed procedures must meet therequirements in Section 7.2 or 7.3. Theminimum storage time should be as soon aspossible, but no longer than 72 hours aftercollection of the sample. The maximum

storage time should be no longer than twoweeks.

7.2 Storage and Sampling Procedures forStack Test Emissions. You must store andanalyze samples of stack test emissionsaccording to Table 3. If you are using analytespiking procedures, you must include equalnumbers of spiked and unspiked samples.

7.3 Storage and Sampling Procedures forTesting Other Waste Media (e.g., Soil/

Sediment, Solid Waste, Water/Liquid). Youmust analyze half of the replicate samples atthe proposed minimum storage time and theother half at the proposed maximum storagetime or within two weeks of the initialanalysis to identify the effect of storage timeson analyte samples. The minimum storagetime should be as soon as possible, but nolonger than seven days after collection of thesample.

7.4 Sample Stability. After you haveconducted sampling and analysis accordingto Section 7.2 or 7.3, compare the results atthe minimum and maximum storage times.Calculate the difference in the results usingEquation 3011.

Where:

di = difference between the results of the ithsample.

Rmini = results from the ith sample at theminimum storage time.

Rmaxi = results from the ith sample at themaximum storage time.

7.4.1 Standard Deviation. Determinethe standard deviation (SDd) of thedifferences (dis) of the paired samplesusing Equation 3012.

Where:

di = The difference between the results of theith sample, Rmini Rmaxi.

dm = The mean of the paired sampledifferences.

n = Total number of paired samples.

7.4.2 t Test. Test the difference inthe results for statistical significance bycalculating the t-statistic and

determining if the mean of thedifferences between the initial resultsand the results after storage issignificant at the 95 percent confidencelevel and n 1 degrees of freedom.Calculate the value of the t-statisticusing Equation 3013.

Where:

n = The total number of paired samples.

Compare the calculated t-statisticwith the critical value of the t-statisticfrom Table 2. If the calculated t-value isless than the critical value, thedifference is not statistically significant;thus, the sampling and analysisprocedure ensures stability, and youmay submit a request for validation of

the proposed alternative test method. Ifthe calculated t-value is greater than thecritical value, the difference isstatistically significant, and you mustrepeat the procedures in Section 7.2 or7.3 with new samples using shorterproposed maximum storage times.

Bias and Precision

8.0 What are the requirements forbias?

You must establish bias by comparingthe results of the sampling using the

alternative test method against areference value. The bias must be nomore than 10 percent without the useof correction factors, and no more than 30 percent with the use of correctionfactors for bias values between 10 and30 percent for the alternative testmethod 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, theprecision expressed as the relativestandard deviation (RSD) of thealternative test method at the level ofthe applicable emission limitation orstandard in the subpart of 40 CFR part63 must be less than or equal to 20percent. For samples with a precisiongreater than 20 percent but less than 50


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percent, a minimum of nine sampleruns will be required. If you arecomparing to a validated test method,the alternative test method must be atleast as precise as the validated methodat the level of the applicable emissionlimitation or standard in the subpart of40 CFR part 63 as determined by an Ftest (Section 11.2.2).

10.0 What calculations must I performfor isotopic spiking?

You must analyze the bias, precision,relative standard deviation, and dataacceptance for isotopic spiking testsaccording to the provisions in Sections10.1 through 10.3.

10.1 Numerical Bias. Calculate the

numerical value of the bias using theresults from the analysis of theisotopically spiked field samples andthe calculated value of the isotopically

labeled spike according to Equation3014.

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 valuesaccording to Equation 3015.

Where:

Si = Measured value of the isotopicallylabeled analyte in the i-th field sample,

n = Number of isotopically spiked samples,12.

10.3 t Test. Test the bias forstatistical significance by calculating thet-statistic using Equation 3016. Use thestandard deviation determined inSection 10.2 and the numerical biasdetermined in Section 10.1.

Compare the calculated t-value withthe critical value of the two-sidedt-distribution at the 95 percentconfidence level and n-1 degrees offreedom. When spiking is conductedaccording to the procedures specified inSections 6.2 and 6.4 as required, thiscritical value is 2.201 for the 11 degreesof freedom. If the calculated t-value isless than the critical value, the bias isnot statistically significant, and the biasof the candidate test method isacceptable. If the calculated t-value isgreater than the critical value, the biasis statistically significant, and you must

evaluate the relative magnitude of thebias using Equation 3017.

Where:

BR = Relative bias.

If the relative bias is less than or equalto ten percent, the bias of the candidatetest method is acceptable and nocorrection factors are required. If therelative bias is greater than 10 percent

but less than 30 percent, and if youcorrect all future data collected with themethod for the magnitude of the bias,the bias of the candidate test method isacceptable. If either of the preceding

two cases applies, you may continue toevaluate the method by calculating itsprecision. If not, the candidate methodwill not meet the requirements ofMethod 301.

10.4 Relative Standard Deviation.Calculate the RSD according to Equation3018.

Where:

Sm = The measured mean of the isotopicallylabeled spiked samples.

The data and alternative test methodare unacceptable if the RSD is greaterthan 20 percent.

11.0 What calculations must I performfor comparison with a validated methodif I am using quadruplet replicatesampling systems?

If you are using quadruplet replicatesampling systems to compare analternative test method to a validatedmethod, then you must analyze the dataaccording to the provisions in thissection. If the data from the alternativetest method fail either the bias orprecision test, the data and thealternative test method areunacceptable. If the Administratordetermines that the affected source hashighly variable emission rates, theAdministrator may require additionalprecision checks.

11.1 Bias Analysis. Test the bias forstatistical significance at the 95 percentconfidence level by calculating thet-statistic.

11.1.1 Bias. Determine the bias,which is defined as the mean of thedifferences between the alternative testmethod and the validated method (dm).Calculate di according to Equation3019.

Where:

V1i = First measured value with the validatedmethod in the i-th sample.

V2i = Second measured value with thevalidated method in the i-th sample.

P1i = First measured value with thealternative test method in the i-thsample.

2i = Second measured value with thealternative test method in the i-thsample.

11.1.2 Standard Deviation of theDifferences. Calculate the standarddeviation of the differences, SDd, usingEquation 3012.

11.1.3 t Test. Calculate the t-statisticusing Equation 3013, where n is thetotal number of test sample differences(di). For the quadruplet sampling systemprocedure in Section 6.1 and Table 1, nequals four. Compare the calculated t-statistic with the critical value of the t-


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statistic, and determine if the bias issignificant at the 95 percent confidencelevel. When four runs are conducted, asspecified in Section 6.2 and Table 1, thecritical value of the t-statistic is 3.182for three degrees of freedom. If thecalculated t-value is less than thecritical value, the bias is not statisticallysignificant and the data are acceptable.

If the calculated t-value is greater thanthe critical value, the bias is statisticallysignificant, and you must evaluate therelative magnitude of the bias usingEquation 30110.

Where:

B = Biasmean of the dis.VS = Mean measured by the validated

method.

If the relative bias is less than or equalto 10 percent, the bias of the candidatetest method is acceptable and nocorrection factors are required. If therelative bias is greater than 10 percent

but less than 30 percent, and if youcorrect all future data collected with themethod for the magnitude of the bias,the bias of the candidate test method isacceptable. If either of the precedingtwo cases applies, you may continue toevaluate the method by calculating itsprecision. If not, the candidate method

will not meet the requirements ofMethod 301.

11.2 Precision. Compare theestimated variance (or standarddeviation) of the alternative test methodto that of the validated method. If asignificant difference is determinedusing the F test, the alternative testmethod and the results are rejected. If

the F test does not show a significantdifference, then the alternative testmethod has acceptable precision. Usethe value furnished with the method.Calculate the estimated variance of thevalidated method using Equation 30111.

11.2.1 Alternative Test MethodVariance. Calculate the estimatedvariance of the alternative test method,Sp2, according to Equation 30111.

Where:

di = The difference between the i-th pair ofsamples collected with the alternativetest method.

n = Number of samples and the degrees offreedom.

11.2.2 F Test. Determine if theestimated variance of the alternative testmethod is greater than that of thevalidated method by calculating the F-value using Equation 30112.

Where:

Sp2 = The estimated variance of thealternative method.

Sv2 = The estimated variance of the validatedmethod.

Compare the experimental F valuewith the one-sided confidence level forF. The one-sided confidence level of 95percent for F is 6.388 when theprocedure specified in Section 6.1 andTable 1 for quadruplet trains isfollowed. If the calculated F is outsidethe critical range, the difference inprecision is significant, and the data andthe candidate test method areunacceptable.

12.0 What calculations must I performfor analyte spiking?

You must analyze the data for analytespike testing according to this section.

12.1 Bias Analysis. Test the bias forstatistical significance at the 95 percentconfidence level by calculating the t-statistic.

12.1.1 Bias. Determine the bias usingthe results from the analysis of thespiked field samples, the unspiked fieldsamples, and the calculated value of thespike using Equation 30113.

Where:

S1i = First measured value of the ith spikedsample.

S2i = Second measured value of the ithspiked sample.

M1i = First measured value of the ithunspiked sample.

M2i = Second measured value of the ithunspiked sample.

CS = Calculted value of the spiked level.

12.1.2 Standard Deviation of theDifferences. Calculate the standarddeviation of the differences, SDd, using

Equation 3012.12.1.3 t Test. Calculate the t-statisticusing Equation 3013, where n is thetotal number of test sample differences(di). For the quadruplet sampling systemprocedure in Table 1, n equals six.Compare the calculated t-statistic withthe critical value of the t-statistic, anddetermine if the bias is significant at the95 percent confidence level. When sixruns are conducted, as specified inTable 1, the two-sided confidence levelcritical value is 2.571 for the fivedegrees of freedom. If the relative bias

is less than or equal to 10 percent withno correction factors, or the bias isgreater than 10 percent but less than 30percent with the use of correctionfactors, then the data are acceptable.Proceed to evaluate precision of thecandidate test method.

Where:

B = Biasmean of the dis.

VS = Mean measured by the validatedmethod.

12.2 Precision. Calculate the standarddeviation and the relative standard deviationof the candidate test method. The relativestandard deviation of the candidate testmethod can be calculated using Equation3018.

13.0 How do I conduct tests at similarsources?

If the Administrator has approved the useof an alternative test method to a test methodrequired in 40 CFR part 63 for an affectedsource, and the Administrator has approved

the use of the alternative test method at yoursimilar source according to the procedures inSection 17.1.1, you must meet therequirements in this section. You must haveat least three replicate samples for each testthat you conduct at the similar source. Youmust average the results of the samples todetermine the pollutant concentration.

Optional Requirements

14.0 How do I use and conduct ruggednesstesting?

If you want to use a validated test methodat a concentration that is different from the

concentration in the applicable emissionlimitation in the subpart of 40 CFR part 63or for a source category that is different fromthe source category that the test methodspecifies, then you must conduct ruggednesstesting according to the procedures inCitation 18.16 of Section 18.0 and submit arequest for a waiver according to Section17.1.1.

Ruggedness testing is a laboratory study todetermine the sensitivity of a method toparameters such as sample collection rate,interferant concentration, collecting mediumtemperature, and sample recoverytemperature. You conduct ruggedness testing


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by changing several variables simultaneouslyinstead of changing one variable at a time.For example, you can determine the effect ofseven variables in eight experiments insteadof one. (W.J. Youden, Statistical Manual ofthe Association of Official AnalyticalChemists, Association of Official AnalyticalChemists, Washington, DC, 1975, pp. 3336).

15.0 How do I determine the Limit of

Detection for the alternative method?15.1 Limit of Detection. The Limit ofDetection (LOD) is the lowest level abovewhich you may obtain quantitative resultswith an acceptable degree of confidence. Forthis protocol, the LOD is defined as threetimes the standard deviation, So, at the blanklevel.

15.2 Purpose. The LOD will be used toestablish the lower limit of the test method.If the estimated LOD is no more than twicethe calculated LOD, use Procedure I in Table4 to determine So. If the LOD is greater thantwice the calculated LOD, use Procedure II inTable 4 to determine So. For radiochemicalmethods, use the Multi-Agency RadiologicalLaboratory Analytical Protocols (MARLAP)

Manual (i.e., use the minimum detectableconcentration (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 analternative test method?

16.1 Submitting Requests. You mustrequest to use an alternative test methodaccording to the procedures in Section63.7(f). You may not use an alternative testmethod to meet any requirement under 40CFR part 63 until the Administrator hasapproved your request. The request mustinclude a field validation report containingthe information in Section 16.2. The request

must be submitted to the Director, AirQuality Assessment Division, U.S.Environmental Protection Agency, C30402,Research Triangle Park, NC 27711.

16.2 Field Validation Report. The fieldvalidation report must contain theinformation in Sections 16.2.1 through16.2.8.

16.2.1 Regulatory objectives for thetesting, including a description of the reasons

for the test, applicable emission limits, anda description of the source.

16.2.2 Summary of the results andcalculations shown in Sections 6.0 through16, 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 meetone of the criteria in Sections 17.1.1 through17.1.2, the Administrator may waive therequirement to use the procedures in thismethod to validate an alternative test

method. In addition, if EPA currentlyrecognizes an appropriate test method orconsiders the analysts test method to besatisfactory for a particular source, theAdministrator may waive the use of thisprotocol or may specify a less rigorousvalidation procedure.

17.1.1 Similar Sources. If the alternativetest method that you want to use has beenvalidated at another source and you can

demonstrate to the Administratorssatisfaction that your affected source issimilar to that source, then the Administratormay waive the requirement for you tovalidate the alternative test method. Oneprocedure you may use to demonstrate theapplicability of the method to your affectedsource is by conducting a ruggedness test asdescribed in Section 14.0.

17.1.2 Documented Methods. If the biasand precision of the alternative test methodthat you are proposing have beendemonstrated through laboratory tests orprotocols different from this method, and youcan demonstrate to the Administratorssatisfaction that the bias and precision applyto your application, then the Administrator

may waive the requirement to use thismethod or to use part of this method.17.2 Submitting Applications for Waivers.

You must sign and submit each request fora waiver from the requirements in thismethod in writing. The request must besubmitted to the Director, Air QualityAssessment Division, U.S. EnvironmentalProtection Agency, C30402, ResearchTriangle Park, NC 27711.

17.3 Information Application for Waiver.The request for a waiver must contain athorough description of the test method, theintended application, and results of anyvalidation or other supporting documents.The request for a waiver must contain, at aminimum, the information in Sections 17.3.1

through 17.3.4. The Administrator mayrequest additional information if necessary todetermine whether this method can bewaived for a particular application.

17.3.1 A Clearly Written Test Method.The method should be written preferably inthe format of 40 CFR part 60, Appendix ATest Methods. It must include anapplicability statement, concentration range,precision, bias (accuracy), and minimum andmaximum storage time in which samplesmust be analyzed.

17.3.2 Summaries of previous validationtests or other supporting documents. If adifferent procedure from that described inthis method was used, you must submitdocuments substantiating the bias and

precision values to the Administratorssatisfaction.

17.3.3 Ruggedness Testing Results. Youmust submit results of ruggedness testingconducted according to Section 14.0, samplestability conducted according to Section 7.0,and detection limits conducted according toSection 15.0, as applicable. For example, youwould not need to submit ruggedness testingresults if you will be using the method at thesame concentration level as the concentrationlevel at which it was validated.

17.3.4 Applicability Statement and Basisfor Waiver Approval. Your discussion of theapplicability statement and basis for approval

of the waiver should address the following asapplicable: Applicable regulation, emissionstandards, effluent characteristics, andprocess operations.

18.0 Where can I find additionalinformation?

You can find additional information in thereferences 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 OrganicCylinder Gases and Results of Source TestAnalysis Audits, Status Report No. 11.Environmental Protection Agency Contract68024125. Research Triangle Institute,Research Triangle Park, NC. September.

18.2 ASTM Standard E 116989 (currentversion), Standard Guide for ConductingRuggedness 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 andField Evaluation of a Methodology forSpeciating Nickel Emissions from StationarySources. EPA Contract 68024442. Prepared

for Atmospheric Research and EnvironmentalAssessment Laboratory, Office of Researchand Development, U.S. EnvironmentalProtection Agency, Research Triangle Park,NC 27711. January.

18.4 International Conference onHarmonization of Technical Requirementsfor the Registration of Pharmaceuticals forHuman Use, ICHQ2A, Text on Validationof Analytical Procedures, 60 FR 11260(March 1995).

18.5 International Conference onHarmonization of Technical Requirementsfor the Registration of Pharmaceuticals forHuman Use, ICHQ2b, Validation ofAnalytical Procedures: Methodology, 62 FR27464 (May 1997).

18.6 Keith, L.H., W. Crummer, J. DeeganJr., 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. Estimatingvariances from one or two measurements oneach sample. Amer. Statistician 28:9697.

18.8 Midgett, M.R. 1977. How EPAValidates NSPS Methodology. Environ. Sci. &Technol. 11(7):655659.

18.9 Mitchell, W.J., and M.R. Midgett.1976. Means to evaluate performance ofstationary source test methods. Environ. Sci.& Technol. 10:8588.

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. LewisPublishers, Inc., pp. 7981.

18.12 U.S. Environmental ProtectionAgency. 1978. Quality Assurance Handbookfor Air Pollution Measurement Systems:Volume III. Stationary Source SpecificMethods. Publication No. EPA600/477027b. Office of Research and DevelopmentPublications, 26 West St. Clair St.,Cincinnati, OH 45268.

18.13 U.S. Environmental ProtectionAgency. 1981. A Procedure for EstablishingTraceability of Gas Mixtures to Certain

http://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdfhttp://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdfhttp://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdfhttp://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdfhttp://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdfhttp://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdf

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National Bureau of Standards StandardReference Materials. Publication No. EPA600/781010. Available from the U.S. EPA,Quality Assurance Division (MD77),Research Triangle Park, NC 27711.

18.14 U.S. Environmental ProtectionAgency. 1991. Protocol for The FieldValidation of Emission Concentrations From

Stationary Sources. Publication No. 450/490015. Available from the U.S. EPA,Emission Measurement TechnicalInformation Center, Technical SupportDivision (MD14), Research Triangle Park,NC 27711.

18.15 Wernimont, G.T., Use of Statisticsto Develop and Evaluate Analytical

Methods, AOAC, 1111 North 19th Street,Suite 210, Arlington, VA 22209. USA, 7882(1987).

18.16 Youden, W.J. Statistical techniquesfor collaborative tests. Statistical Manual ofthe Association of Official AnalyticalChemists, Association of Official AnalyticalChemists, Washington, DC, 1975, pp. 3336.

TABLE 1 OF APPENDIX ASAMPLING 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 ofreplicate samples using a quadruplet sampling system (a total of 16 samples). In each sam-ple set, you must use the validated test method to collect and analyze half of the samples.

using isotopic spiking (can only be used for pro-cedures requiring mass spectrometry).

a total of 12 replicate samples. You may collect the samples either by obtaining 6 sets ofpaired 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 sam-ples).

TABLE 2 OF APPENDIX ACRITICALVALUES OF t FOR THE TWO TAILED95 PERCENT CONFIDENCE LIMIT

Degrees of freedom t951 ..... .. ... ... .. ... .. ... .. ... ... .. ... .. ... .. . 12.7062 ............................................ 4.3033 ............................................ 3.1824 ............................................ 2.7765 ............................................ 2.571

TABLE 2 OF APPENDIX ACRITICALVALUES OF t FOR THE TWO TAILED95 PERCENT CONFIDENCE LIMITContinued

Degrees of freedom t956 ............................................ 2.447

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

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

TABLE 2 OF APPENDIX ACRITICALVALUES OF t FOR THE TWO TAILED95 PERCENT CONFIDENCE LIMITContinued

Degrees of freedom t959 ............................................ 2.262

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

TABLE 3 OF APPENDIX ASTORAGE 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 im-pinger sampling systems.

analyze 6 of the samples within 7 days andthen analyze the same 6 samples at theproposed maximum storage time or 2weeks after the initial analysis.

sorbent and impinger sampling systems thatrequire extraction or digestion.

extract or digest 6 of the samples within 7days and extract or digest 6 other samplesat the proposed maximum storage time or 2weeks after the first extraction or digestion.Analyze an aliquot of the first 6 extracts(digestates) within 7 days and proposedmaximum storage times or 2 weeks afterthe initial analysis. This will allow analysisof extract storage impacts.

sorbent sampling systems that require thermaldesorption.

analyze 6 samples within 7 days. Analyze an-other set of 6 samples at the proposedmaximum storage time or within 2 weeks ofthe initial analysis.

comparing an alternative test method against avalidated test method.

sampling method that does not include sor-bent and impinger sampling systems thatrequire extraction or digestion.

analyze half of the samples (8 or 9) within 7days and half of the samples (8 or 9) at theproposed maximum storage time or within 2weeks 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 samplesat the proposed maximum storage time orwithin 2 weeks of the first extraction or di-gestion. Analyze an aliquot of the first 6 ex-tracts (digestates) within 7 days and at theproposed maximum storage times or within2 weeks of the initial analysis. This willallow analysis of extract storage impacts.


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TABLE 4 OF APPENDIX APROCEDURES FOR ESTIMATING SoIf the estimated LOD (LOD1, expected approximate LOD concentration

level) is no more than twice the calculated LOD, use Procedure I asfollows. Estimate the LOD (LOD1) and prepare a test standard at thislevel. The test standard could consist of a dilution of the analyte de-scribed in Section 5.0.

If the estimated LOD (LOD1, expected approximate LOD concentrationlevel) is greater than twice the calculated LOD, use Procedure II asfollows. Prepare two additional standards (LOD2 and LOD3) at con-centration 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) atleast 7 times.

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

Calculate the LOD0 (referred to as the calculated LOD) as 3 times S 1,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 tozero concentration. The standard deviation at zero concentration isSo.

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

* * * * *

[FR Doc. 201112058 Filed 51711; 8:45 am]

BILLING CODE 656050P

ENVIRONMENTAL PROTECTION

AGENCY

40 CFR Part 180

[EPAHQOPP20090263; FRL88658]

Spirotetramat; Pesticide Tolerances

AGENCY: Environmental ProtectionAgency (EPA).

ACTION: Final rule.

SUMMARY: This regulation establishestolerances for residues of spirotetramat,including its metabolites anddegradates, in or on multiplecommodities which are identified and

discussed later in this document. BayerCropScience requested these tolerancesunder the Federal Food, Drug, andCosmetic Act (FFDCA).

DATES: This regulation is effective May18, 2011. Objections and requests forhearings must be received on or before

July 18, 2011, and must be filed inaccordance with the instructionsprovided in 40 CFR part 178 (see alsoUnit I.C. of the SUPPLEMENTARYINFORMATION).

ADDRESSES: EPA has established adocket for this action under docket

identification (ID) number EPAHQOPP20090263. All documents in thedocket are listed in the docket indexavailable at http://www.regulations.gov.Although listed in the index, someinformation is not publicly available,e.g., Confidential Business Information(CBI) or other information whosedisclosure is restricted by statute.Certain other material, such ascopyrighted material, is not placed onthe Internet and will be publiclyavailable only in hard copy form.Publicly available docket materials are

available in the electronic docket athttp://www.regulations.gov,or, if onlyavailable in hard copy, at the OPPRegulatory Public Docket in Rm. S4400, 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 DocketFacility telephone number is (703) 3055805.FOR FURTHER INFORMATION CONTACT: RitaKumar, Registration Division (7505P),Office of Pesticide Programs,Environmental Protection Agency, 1200Pennsylvania Ave., NW., Washington,DC 204600001; telephone number:(703) 3088291; e-mail address:[email protected].

SUPPLEMENTARY INFORMATION:

I. General Information

A. Does this action apply to me?

You may be potentially affected bythis action if you are an agriculturalproducer, food manufacturer, orpesticide manufacturer. Potentiallyaffected entities may include, but arenot limited to those engaged in thefollowing 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 beexhaustive, but rather to provide a guidefor readers regarding entities likely to beaffected by this action. Other types ofentities not listed in this unit could also

be affected. The North AmericanIndustrial Classification System(NAICS) codes have been provided toassist you and others in determiningwhether this action might apply tocertain entities. If you have anyquestions regarding the applicability ofthis action to a particular entity, consult

the person listed under FOR FURTHERINFORMATION CONTACT.

B. How can I get electronic access toother related information?

You may access a frequently updated

electronic version of EPAs toleranceregulations at 40 CFR part 180 throughthe Government Printing Offices e-CFRsite at http://www.gpoaccess.gov/ecfr.To access the harmonized testguidelines referenced in this documentelectronically, please go to http://www.epa.gov/ocsppand select TestMethods & Guidelines.

C. How can I file an objection or hearingrequest?

Under FFDCA section 408(g), 21U.S.C. 346a, any person may file anobjection to any aspect of this regulation

and may also request a hearing on thoseobjections. You must file your objectionor request a hearing on this regulationin accordance with the instructionsprovided in 40 CFR part 178. To ensureproper receipt by EPA, you mustidentify docket ID number EPAHQOPP20090263 in the subject line onthe first page of your submission. Allobjections and requests for a hearingmust be in writing, and must bereceived by the Hearing Clerk on or

before July 18, 2011. Addresses for mailand hand delivery of objections andhearing requests are provided in 40 CFR178.25(b).

In addition to filing an objection orhearing request with the Hearing Clerkas described in 40 CFR part 178, pleasesubmit a copy of the filing that does notcontain any CBI for inclusion in thepublic docket. Information not markedconfidential pursuant to 40 CFR part 2may be disclosed publicly by EPAwithout prior notice. Submit a copy ofyour non-CBI objection or hearingrequest, identified by docket ID numberEPAHQOPP20090263, by one ofthe following methods:
http://www.regulations.gov/http://www.regulations.gov/mailto:[email protected]://www.gpoaccess.gov/ecfrhttp://www.epa.gov/ocspphttp://www.epa.gov/ocsppmailto:[email protected]://www.epa.gov/ocspphttp://www.epa.gov/ocspphttp://www.regulations.gov/http://www.regulations.gov/http://www.gpoaccess.gov/ecfr

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