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Federal Register / Vol. 55, No. 27 / Thursday, February 8, 1990 / Proposed Rules

ENVIRONMENTAL PROTECTIONAGENCY40 CFR Parts 260,261, 262, 264, 265,

268 and 270

[FRL-3721-7]

Hazardous Waste ManagementSystem; Testing and MonitoringActivities

AGENCY* Environmental ProtectionAgency.ACTION: Notice of reopening of commentperiod; notice of data availability.

SUMMARY: On January 23, 1989, theAgency proposed to amend itshazardous waste testing and monitoringregulations under Subtitle C of RCRAby: (1) Incorporating the Third Edition of"Test Methods for Evaluating SolidWaste, Physical/Chemical Methods,"(SW-846) into the RCRA regulations; (2)updating SW--846 with additionalmethods and information; and (3)mandating minimum Quality Control(QC) procedures for all RCRA testing.(See 54 FR 3212-3229, January 23, 1989.)In.response to comments, EPA isconsidering, in addition to the option ofpromulgating the rulemaking asproposed, a number of technicalmodifications and/or clarifications tothe Third Edition of SW-846 and theinclusion of specific QC procedures inSW-846 which are described in the"Report on Minimumn Criteria to AssureData Quality," which would beincorporated as Chapter One of SW-846.The Agency is also considering deletingappendices III and X to 40 CFR part 261.Therefore, the Agency is reopening thecomment period on the proposal for thepurpose of receiving comments, withsupporting documentation, on these newoptions and the deletion of appendicesIII and X.DATES: EPA will accept publiccomments on this Notice until March 12,1990.ADDRESSES: The public should submitan original and two copies of theircomments on this Notice to thefollowing address: EPA RCRA DocketClerk (OS-305), U.S. EnvironmentalProtection Agency, 401 M Street, SW.,Washington, DC 20460. Comments mustbe marked "Docket Number F-90-WTRX-FFFFF."

The administrative record for thisrulemaking is located at the EPA RCRADocket, room M-Z427 at the aboveaddress, and is available for viewingfrom 9 a.m. to 4 p.m., Monday through

Friday, excluding Federal holidays. Call(202) 475-9327 for appointments. Thepublic may copy a maximum of 100pages of material from any oneregulatory docket at no cost; additionalcopies cost $0.15 per page.

Copies of the "Report on MinimumCriteria to Assure Data Quality" areavailable from the RCRA Hotline at(800) 424-9346 (toll free) or (202) 382-3000. The document number is EPA/530-SW-90-021 and there is no cost for thisreport. This report is also included in theadministrative record (RCRA Docket).

Copies of the Third Edition of SW-846and of the proposed Update 1 to theThird Edition are available from theGovernment Printing Office,Superintendent of Documents,Washington, DC 20402 (202) 783-3238.The document number is 955-001-00000-1 and the cost is $110.00 for the four-volume set plus updates. Updatepackageswill be automatically mailedto all subscribers.

Copies of the Second Edition of SW-846 are available from the NationalTechnical Information Service (NTIS),5285 Port Royal Road, Springfield, VA22161, (703] 487-4600. The documentnumber is PB87-120-291 and the cost is$48.95 for paper copies and $13.50 formicrofiche.

FOR FURTHER INFORMATION CONTACT1For general information contact theRCRA Hotline at (800) 424--9346 (tollfree) or (202) 382-3000. For technicalinformation contact Charles Sellers,Office of Solid Waste, OS-331, U.S.Environmental Protection Agency, 401 MStreet SW., Washington, DC 20460, (202)382-4761.

SUPPLEMENTARY INFORMATION:

Preamble Outline

I. AuthorityII. Background SummaryII. Discussion of Technical Modifications

and ClarificationsA. General IntroductionB. Specific Issues

1. Quality Control2. Required versus Optional Use of SW-

846 Testing Methods3. Trace Analysis vs. Macroanalysis4. Equipment Standards and Reagent

Preparation5. Holding Times6. Representative Sampling7. Analysis of Nonaqueous Liquids for

Elemental Species8. Matrix Spikes and Method of Stand-

ard Additions

9. Spike Recovery Correction10. Reagent Grade Water11. Appendices Ill and X to 40 CFR part

261IV. Request for Comments

I. Authority

The rulemaking to which this Notice isaddressed is being proposed under theauthority of sections 2002, 3001, 3004,3005, and 3006 of the Solid WasteDisposal Act, as amended (commonlyknown as the Resource Conservationand Recovery Act, or RCRA), 42 U.S.C.6912, 6921, 6924, 6925, and 6926.

II. Background Summary

Subtitle C of the ResourceConservation- and Recovery Act of 1976(RCRA) creates a comprehensivenational program for the safemanagement of hazardous waste.Associated with characterizing wastes,determining their proper management,and monitoring the performance ofwaste management units is a diversegroup of testing methods that addressthe sampling and analytical proceduresto be used. These methods are intendedto promote accuracy, sensitivity,specificity, precision and comparabilityof analyses and test results.

EPA Publication SW-846,.'TestMethods for Evaluating Solid Waste,Physical/Chemical Methods", containsthe testing methods that EPA hasevaluated and found to be among thoseaccqptable for RCRA testing and whichare required for specific regulations asdiscussed below. In situations where theregulations require the use ofappropriate SW-846 methods, theregulations specify use of the SecondEdition of EPA's SW-846 manual (1982)as amended by Updates I (April 1984)and II (April 1985). In January, 1989, EPAproposed to amend the regulations tospecify the use of the Third Editioninstead of the Second Edition. For a fulldescription and background of theproposal addressed by this Noitice, referto 54 FR 3212-3229 (anuary 23, 1989).

I1. Discussion of TechnicalModifications and Clarifications

This Notice announces severaltechnical clarifications andmodifications to the SW-846 proposal ofJanuary 23, 1989. (See 54 FR 3212-3229.)Included in these modifications is a newdocument, entitled "Report on MinimumCriteria to Assure Data Quality,"(Report) that defines good field andlaboratory practices. This document isbeing considered as a replacement forthe previously proposed Chapter One ofthe Third Edition of SW-846. The

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Agency is also considering making all ofChapter One (not just sections-1.2 and1.3 of Chapter One, as proposed in theJanuary 1989 Notice) mandatory for allRCRA testing, with the exclusion ofcertain reasonable and legitimateexceptions noted in Section I1. B. To,obtain this document, refer to thesection under "ADDRESSES' of thisnotice.

In addition, the Agency is alsoconsidering deleting appendices III andX to 40 CFR part 261. Appendix III isunnecessary and potentially misleading,and appendix X will become obsolete.upon incorporation of the Third Editionof SW-846.

The public is invited to submitcomments only on the Report, and itsreplacement of the proposed ChapterOne of SW-846, the technicalclarifications and modifications to theThird Edition, and the deletion ofappendices III and X to CFR 40 part 261as addressed by this Notice. This Noticedoes not reopen the comment period onany other aspect of the January 23, 1989rulemaking proposal. All timelycomments submitted on the newinformation contained in today's noticetogether with all the timely commentspreviously submitted in response to theJanuary notice, will be considered inpreparation of a final rulemaking.

A. General Introduction

The nature of SW-846 is such thatprocedures are written to determineanalytes at low concentrations, e.g.,parts per million (ppm) or parts perbillion (ppb). Testing under RCRA,however, requires the afialysis of a ,broad range of matrices (e.g., water, soil,clay, nonaqueous liquids, process "residues, ash) and a broad range ofconcentrations (e.g., ppb to percentlevels). No one set of testing proceduresis, therefore, uniformly applicable. Thisproblem often may be overcome byproviding a selection of samplepreparation (including dilution,concentration, sample size adjustment,etc.), cleanup, and determinativeprocedures from which the analyst canselect the proper analytical procedure tobe used in an individual situation. Forexample, when analyzing a relativelyclean ground water sample for a semi-volatile organic compound, it may besufficient to employ a sample-preparation procedure, Method 3510,coupled with determinative procedure,Method 8270. On the other hand, if onemust analyze a wastewater containingcompounds that interfere with thedetermination of the compounds ofinterest, the analyst will have to employone of the cleanup methods prior tousing the determinative procedure in

Method 8270. The various preparation,cleanup, and determinative proceduresare listed in the appropriate sections ofSW-846. Except for those situations

-where the RCRA regulations specify useof a particular method, it is appropriatefor the chemist to use judgment,tempered by experience, in selecting anappropriate set of methods from SW-846or the scientific literature for preparingand analyzing a given sample.

B. Specific Issues

1. Quality Control

In the January 1989 Notice ofProposed Rulemaking (NPRM), theAgency proposed to make certainQuality Control (QC) proceduresmandatory for all testing and analysisconducted to comply with the hazardouswaste regulations under subtitle C ofRCRA. The January proposal representsone part of EPA's program to establishand require minimum QC procedures forall RCRA-related testing and analysis.The goal of this effort is to ensureconsistent and correct application ofappropriate methods and to producedata of known and documented quality.

The proposed QC procedures to befollowed are found in the revisedChapter One of the Third Edition ofSW-846, Update I (specifically sections1.2 and 1.3, and procedures referencedtherein). Because of the wide reachingnature of these procedures and theirimportance to the RCRA program, theAgency received many comments onthis QC procedures chapter. In addition,the Agency received the assistance ofthe American addition, the Agency.received the assistance of the AmericanSociety for Testing and Materials(ASTM) in clarifying the QCrequirements and definitions.. Based on the comments received andother new information, the Agency hasrevised Chapter One of the ThirdEdition of SW-846. These revisions arecontained in a document entitled"Report on Minimum Criteria to AssureData Quality." The Agency is alsoconsidering making all of Chapter One(not just sections 1.2 and 1.3 of ChapterOne, as proposed in the-January 1989notice) mandatory for all RCRA testing,with the exclusion of certain reasonableand legitimate exceptions noted below.The Agency is considering adoptingthese revisions as Chapter One of theThird Edition of SW-846 in the finalrule. These techical revisions providedefinitions and procedures necessary forgenerating data of known anddocumented quality when performingRCRA-related sampling and analysisactivities. The Agency believes that thisrevised Chapter One will better meet the

needs of the regulated community aswell as the regulatory agencies and,therefore, solicits comments on theproposed revisions.

2. Required Versus Optional Use of SW-846 Testing Methods

Certain hazardous-waste regulationsunder Subtitle C of RCRA require thatspecific testing methods described in theidentified edition of SW-846 beemployed for certain applications. Theserequired methods and regulatorycitations (40 CFR parts 260-270) are theones specified for determining whether:(1) Wastes exhibit the characteristics ofcorrosivity or toxicity, § § 261.22(a) and261.24(a); (2) for determining if wastescontain free liquids, § § 264.314(a) and265.314(d); (3) for any testing done insupport of a petition for delisting of awaste, § 260.22(d)(1)(i); and (4) fortesting during a trial burn in support ofan application for a hazardous wasteincineration permit § 270.62(b)(2)(i)(C).For other RCRA testing and monitoringneeds, any reliable analytical methodsmay be used to meet the regulatoryrequirements. This notice, or 'thesubsequent final rule, should -not beconstrued to require the use of SW-846,Third Edition methods except wherespecifically prescribed by regulation. Inaddition, unless specifically required inSW-846 or this rule, regulatoy agencies(and others) need not be required to usethe full Chapter One quality controlprocedures when they are faced withsituations (such as those describedbelow) where the specific .application ofthe quality control procedures may notbe appropriate.

The testing methods and approachesdescribed in SW-846 are designedprimarily for use by persons todemonstrate that a regulatory thresholdhas not been exceeded. Because of thisfocus, the Agency has receivedquestions regarding the applicability ofSW-846 to other types of activities. Forexample, in the majority of cases theregulated community uses SW-846methods to prove that a waste-does notcontain a given analyte at a specificconcentration or does not exhibit ahazardous waste characteristic.(Demonstrating that a waste is not ahazardous waste is hereinafter referredto as proving the negative).

The sampling strategy for thesesituations (proving the negative) shouldbe thorough enough to insure that onedoes not conclude a waste is non-hazardous when, in fact, it is hazardous.For example, one needs to take enoughsamples so that one does not miss areasof high concentration in an otherwiseclean material. Samples must be

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handled so that properties do notchange and contaminants are not lost.The analytical methods must bequantitative, and regulatory detectionlimits must be met and documented.

While the regulated community isconcerned with proviing the negative, orabsence of any hazardous constituentsor characteristics, regulatory agenciesare often concerned with demonstratingthe opposite-that the wasteconcentration of a specific analyte in awaste, exceeds a regulatory level, orthat the waste exhibits a hazardouswaste characteristic. (Hereinafterreferred to as proving the positive).

Sampling strategies for thesesituations (proving the positive) often donot require a precise determination ofthe actual magnitude of the property. Ifa sample possesses the property ofinterest, or contains the constituent at ahigh enough level relative to theregulatory threshold, then thepopulation from which the sample wasdrawn must also possess the property ofinterest or contain that constituent.Depending on the degree to which theproperty of interest is exceeded, testingof samples which represent all aspectsof the waste or other material may notbe necessary to prove that the waste issubject to regulation.

Likewise, a sample need not alwaysbe handled to prevent losses because ifthe sample contains the constituentabove a regulatory level even withlosses, then clearly the level has beenexceeded. Therefore, use of methods toshow that a level has been exceededneed not always be quantitative, butcould simply be qualitative or semi-quantitative. The results for qualitativeor semi-quantitative determinations areoften expressed by stating that thesample contains a minimum amount ofanalyte. Well defined detection limits,adequate analyte recoveries, and highdegrees of precision are not alwaysnecessary attributes of methods used tomake such determinations. Simplyproving a compound present (selectivity)in the waste and that its concentrationis greater than a regulatory limit are theimportant attributes.

While quality control requirementsaddress both positive showings andnegative showings equally, someprocedures or steps in a method, whichare quality control related, may only beimportant in those sampling andanalytical determinations performed toensure that the trace concentrations ofhazardous constituents are accuratelymeasured. For example, holding timesare considered a quality control issue.However, there are cases (explainedbelow) where adherence to a specificholding time has little or no impact on

the adequacy of a regulatorydetermination. While SW-846 samplingand laboratory practices and QCprocedures are generally appropriatewhen testing to show either a positive ornegative situation, the full panoply ofChapter One QC procedures may notalways be needed. An example of a QCprocedure, such as a matrix spike, thatdoes not apply is where one is todetermine whether a waste exhibits thecharacteristic of corrosivity or whetherit contains free liquids. In these casesspiking does not apply because spikingwould change the sample's behavior andthe results would be meaningless.Another example is when characterizinga high concentration liquid waste forignitability. Here a field blank is notapplicable since ignitability testing is a"yes/no" type test (i.e., the liquid isignitable or its not). Thus, a field blankhas no relevance in this cqse.

Furthermore, some of the chemicalanalysis test methods set forth inappendix III to 40 part 261 would not beappropriate for demonstrating that asample contains a constituent becausethe working concentration range of themethod is much lower than theconcentration of the sample. This pointis covered in more detail in the nextsection; however, it is noted thatsections of SW-846 (beyond ChapterOne) require some revision to betterclarify the applicability of certain tests.

Therefore, the Agency intends torevise the discussion of the applicabilityof some quality control procedures usedin SW-846, beyond the changes made toChapter One, using language similar tothat provided above, to make thesetypes of distinctions.

3. Trace Analysis vs Macroanalysis

Implicit in the proceding argument isthe fact that SW--846 was designedlargely for use in showing that a wastedoes not contain certain hazardousconstituents or characteristics. In thatregard, many SW--846 samplepreparation methods are designedaround trace analysis rather than thepercent level determinations oftenrequired for concentrated wastes. Thesemethods, however, might be suitable forpercent level determination analysiswhen appropriately modified by theanalyst.

For example, it is permissible toadjust the sample preparation methodsprior to determination when theconcentrations of the target analytes inthe samples are known or believed tofall outside of the linear operating rangeof the analytical instrument used formeasurement. The Agency has alwaysbelieved that when very concentratedsamples are analyzed, dilution or

reduction in size of the sample aliquottested may be needed to assure that theanalytical values obtained are withinthe linear operating range of theinstrument. Furthermore, the Agencyunderstands that the analyst may electto use smaller samples and/or dilutionwhen concentrations exceed thecapacities of reagents or columns statedfor use in the methods. In addition, itmay be necessary to use the alternativetechniques described in existingmethods for the introduction of a sampleinto an instrument when highconcentrations of target analytes areknown or believed to exist. An exampleof this would be the use of the directinjection method for sample introductionrather than the purge and trap techniquewhen the sample contains highconcentrations of volatile organiccompounds. However, the analyst mustmake particular note of any deviationsfrom the published methodology whenreporting the results of the analysis.

The Agency anticipates makingchanges in the final promulgation toSW-846 that will allow the analystneeded latitude regarding sample size,sample dilution, sample concentration,and choice of analytical methodologywhen macroahalysis is performed6These changes would consist of addinga discussion similar to the one above toappropriate chapters and methodscontained in SW-846. The Agencyrequests comment on these anticipatedchanges.

4. Equipment Standards and ReagentPreparation

In each analytical method in SW-646,detailed specifications are given relativeto the type and size of individualglassware and other apparatus, and tothe preparation of reagents such asstock standard solutions. Thisspecificity derives, in part, from thedesire to give as much assistance aspossible to the analyst and to ensureuniform testing protocols.

Since many types and sizes ofglassware and supplies arecommercially available, and since it ispossible to prepare reagents andstandards in many different ways, someof those given in the methods may bereplaced by any similar types as long assubstitution does not affect the overallquality of the analyses.

For example, vials are frequentlyspecified as glass "with a Teflon-linedscrew-cap." An acceptable alternativecould be Teflon-lined crimped top vials.Similarly, reagents can be prepared inany quantity appropriate to achieveoptimum efficiency of laboratoryoperations, provided that concentrations

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Federal Register I Vol. 55, No. 27 / Thursday, February 8, 1990 / Proposed Rules

specified in the methods remainunchanged. For example, the 1ON NaOHspecified in Method 3510 can be madeup in any volume provided that theproportion of 40g NaOH per 100 ml ofsolution remains constant.

The Agency considers that thesubstitution of equivalent glassware andequipment would meet the overallrequirements for quality control, andbelieves that this flexibility is importantfor the analytical chemist to be able tomeet a variety of needs. However, theAgency is concerned that the public notinterpret this flexibility in ways thatwould substantially affect the analyses.One principle to keep in mind is that thisflexibility applies, in general, to volumecapacity (size] and make or brand nameof glassware and equipment, but not tothe funciton or type of equipmentspecified. Similarly, when mixingbatches of standard reagents, the size ofa batch is not important except thatthere be enough for its intended use.What is important in the preparation ofstandards and reagents is thedesignated concentration and purity ofthe final product.

The Agency anticipates makingchanges in the final promulgation toSW-846 that will explicitly permit theanalyst latitude regarding choice ofglassware and equipment based on thediscussion above. These changes willconsist of adding a discussion similar tothe one above to SW-846. The Agencyrequests comment on these anticipatedchanges.

5. Holding Times

Use within the Agency of holdingtimes and preservation techniquesoriginated with the National PollutantDischarge Elimination System (NPDES),authorized under the Clean Water Act(CWA), which was concerned with theloss of trace level contaminants fromwastewater samples collected andanalyzed under a self-monitoringprogram. This practice is continuedunder the Contract Laboratory Program(CLP) and authorized under theComprehensive EnvironmentalResponse, Compenstation, and LiabilityAct (CERCLA), which implementsessentially the same holding times andpreservatives for all water samplescontaining low contaminant levels.

Holding times and preservationtechniques are currently understudy bythe Agency. As yet, no study has beenpublished to indicate that highlycontaminated materials require suchmeasures to preserve their integrity.

Like the other Agency programs, SW-846 has adopted many of theserecommended holding times. TheAgency recognizes that these holding

times were designed for aqueoussamples containing trace levels ofcontaminants. These samples must beextracted and/or analyzed within thespecified holding time for the results tobe considered reflective of total values.Results of samples not analyzed withinthe specified holding time will beconsidered minimum values. That is, theactual concentration will be assumed forregulatory purposes to be equal to orgreater than the concentrationdetermined after the holding time hasexpired. The Agency anticipates makingchanges in the final promulgation toSW-846 that will permit the analystlatitude regarding implementation ofholding times based on the discussionabove. These changes will consist ofadding a discussion similar to the oneabove to SW-846. The Agency requestscomment on these anticipated changes.

6. Representative Sampling

Comments received on the January1989 proposal revealed a great deal ofconfusion over what constitutesrepresentative sampling in relation tothe sampling approach used in a specificcase. Current regulations require thatrepresentative sampling be performedwhen assessing wastes for hazardouscharacteristics. The issue becomes"what is the sample meant torepresent". The Agency offers thefollowing four examples to clarify itsinterpretation of representativesampling.

(1] Materials comprised of particles ofextremes in density or size are, at times,difficult to representatively sample. Anexample is a large pile of smelter slagwhere particles range in size from dustparticles to 1300 lb casts. In such cases,non-random sampling based on theexperience and judgment of the personperforming the sampling may beemployed (e.g., collecting particles lessthan Y2 inch in diameter). This non-random sample provides a reasonableapproximation to a random samplesince large particles are expected tohave similar composition to smallerones because they resulted from thesame process. Furthermore, this non-random sample is expected to be"representative" of the pile since thecomposition of small and large particlesare similar. Care must be taken toensure that the purpose of the samplingis considered when conducting non-random sampling. For the aboveexample, the chemical composition ofthe waste may be independent ofparticle size; however, properties of thewaste such as its leaching potential maystill be dependent on particle size.

(2) Obtaining a representative sampleof high volume wastes presents a major

sampling challenge. Mining residues, forexample, may occupy hundreds of acres,making representative sampling of theentire waste very difficult. In such cases,replicate composites composed ofrandom grab samples of the readilyavailable material (e.g., residues within12 inches of the surface) may he taken.Conclusions regarding the level ofhazard of the waste can be drawn byexamining the variability of the valuesobtained on replicate composites. Thesampling, compositing and dataevaluation process is then repeated untilthe confidence in the representativenessof the mean reaches the desired level(e.g., less than 10% probability that thetrue mean is above an appropriateregulatory threshold). The concept isthat while each individual sample oreven composite may not berepresentative of the residue, the sumtotal of samples taken will represent theaverage property of the waste eventhough the entire waste stream was notsampled.

(3) In some very limited situations,because the bulk of the waste materialis unavailable and decisions need to bemade on a limited amount of theremaining material, and where it isunclear whether a sample isrepresentative of a waste, the Agencywill assume that the available materialis representative of the waste unlessproven otherwise. For example, it is notalways possible to obtain arepresentative sample of a hazardouswaste that has been illegally disposed,when all that is left for testing is a drumcontainingly only residues of the waste.In such an instance, a representativesample of that residue is assumed torepresent the waste that was in thedrum, and conclusions regarding thehazardousness of the waste can bedrawn.

(4) One aspect of the representativesampling issue that warrantsclarification is the situation in which abody of waste to be characterized maybe composed of a number of differentwastes. For example, a disposal site isfound that contains components ofqualitatively different properties le.g.,color, composition, physical state andthe question to be answered is whetherhazardous waste was disposed of at thesite. In this case, one is faced with thesituation, not of sampling allcomponents at the site, but rather ofsampling one or more individualcomponents of the body of waste at thesite. Each of the qualitatively differentcomponents (materials could be adiscrete waste, and the 6oncept ofrepresentative sampling would refer tosampling of each discrete waste rather



than sampling all of the waste at the siteas a whole. Therefore, when faced withsuch a situation, the sampler wouldidentify the components of the wastesite to be characterized and wouldobtain data representative of theproperties of each component ofinterest. The decision as to whether ornot the site contains hazardous wastewould, therefore, hinge on whether anyof the individual components disposedwere hazardous, and not on whether theaverage of all of the components at thesite exhibit the properties of hazardouswaste.

The Agency anticipates adding adiscussion similar to the one above toSW-846. The Agency requests commenton this addition.7. Analysis of Nonaqueous Liquids forElemental Species

Sample preparation methods are notcurrently available in SW-846 to rendernonaqueous liquids in a form that can beanalyzed by the atomic absorption orinductively coupled plasma atomicemissions (ICP) type analytical methodsfor six important elements. Theseelements are: mercury, arsenic,selenium, lead, barium, and silver. Lackof appropriate SW-846 methods mayhinder compliance with various RCRAregulations.

To correct this deficiency, EPA iscurrently developing a microwavedigestion method. In addition, theAgency is considering the approval of amethod currently available as "TestMethod C-Bomb, Acid DigestionMethod" as found in ASTM MethodE926-88: "Methods of Preparing Refuse-Derived Fuel [RDF) Samples forAnalyses of Metals". Method E926-88 isavailable from the American Society forTesting and Materials (ASTM), 1916Race Street, Philadelphia, PA 19103,telephone number (215) 299-5585.Together, these two methods(microwave digestion and bomb, aciddigestion) will provide procedures toprepare nonaqueous liquids forelemental analysis.

Pending final action on incorporationof these methods into SW-846 fornonaqueous samples, the Agencybelieves that the results from TestMethod C of ASTM Method E926-88 arevalid as long as the recommendedquality assurance and quality controlprocedures specified in the proposedReport and this method (Test Method Cof ASTM Method E926-88) are followed.

8. Matrix Spikes and Method ofStandard Additions

The Agencyhas received manyquestions about the use of a matrixspike (sometimes referred to as the

method of known addition) and themethod of standard additions (MSA).Specifically, many chemists performingmetals analyses believe that MSA,particularly where internal standardsare used, is not necessary and is anunwarranted burden and have asked forclarification regarding the use of bothmatrix spikes and MSA.

The Agency has always recommendedthe use of matrix spikes and standardadditions to assure accuracy as part ofthe RCRA program. The Agency requiresthe method of standard additions whenanalyzing EP Toxicity leachates insupport of delisting petitions, and whenanalyzing new matrices (to determinewhether there are suppressiveinterferences). The Agency considersthat these methods (MSA and matrixspikes) are always appropriate althoughMSA may not always be required.Furthermore, when comparing theresults from different analyses of thesame sample for the same analyte, thedetermination made using the method ofstandard addition is preferable over onethat does not.

9. Spike Recovery CorrectionMatrix spike recoveries are used to

determine whether the analyticalprocedure is effective and to permitnormalization of results to 100%. (Note:the recoveries of the analytes in thematrix spike mixture must berepresentative of all target analytes orthe individual target analytes must bespiked into the matrix to determinepercent recovery.) For purposes ofRCRA testing, the Agency believes it isappropriate to correct a measuredconcentration for recovery. Therefore, inresponse to questions, the Agency isproposing to add the following languageto Chapter One of SW-846, ThirdEdition:

The bias determined from the matrix spikeinformation shall be used to correct themeasured values. Details on the calculationsare provided in the glossary under thedefinition of bias.

Insert in glossary:Bias (B)

The deviation of the measured value(Xt) from an accepted reference value(T) or a known spiked amount (K). Biascan be assessed by comparing ameasured value to an acceptedreference value in a sample of knownconcentration or by determining therecovery of a known amount ofcontaminant spiked into a sample. Thus,the bias is calculated as:B=Xt-T

orB=(X.-X,)-Kwhere

Xt= measured value for reference value,X,=measured value for spiked sample,X.= measured value for unspiked sample,.

andK=known value of the spike in the sample.

Using the following equations yieldsthe percent recovery (%R). The value of%R is then used to correct the measuredvalues for that batch of data. Thus,%R=100(Xt/T)

or%R=100 (X.-X,)/Kand

X,=1oo(XJ/%R)where X,=corrected value.

10. Reagent Grade Water

Finally, the Agency has had manyrequests for clarification regarding thelevel of purity needed for the reagentgrade water used when conducting tests.The Agency defines reagent water (forRCRA purposes) as water which isgenerated by any method which wouldachieve the performance specificationsfor ASTM Type II water.

For volatile analyses, it isrecommended that reagent water befurther treated by one of the followingmethods:

(1) Pass the water through a carbonfilter bed containing approximately 500grams of activated carbon (Calgon Corp.Filtrasorb-300 or equivalent);

(2) Pass the water through apurification system (Millipore Super-Qor equivalent); or

(3) Boil water for 15 minutes and then,while maintaining the watertemperature at 85 *C to 95 °C, bubble acontaminant free inert gas (e.g.,nitrogen) through the water for 1 hour.While still hot, transfer the water to anarrow mouth screw-cap bottle underzero-headspace and seal with a Teflon-lined septum and cap.

The Agency further recommends thatreagent water should be monitoredperiodically for impurities as part of thelaboratory's QA program.

For a method blank to be acceptablefor use with the accompanying samples,the concentration in the blank of anyanalyte of concern must be no higherthan the highest of either:

(1) The detection limit, or(2) Five percent of the regulatory limit

for that analyte, or(3) Five percent of the measured

concentration in the sample.In addition, the method blank must

contain no other impurities at aconcentration which will affect theperformance of the method.

These technical points are beingconsidered for inclusion in.the ThirdEdition of SW-846 at this time, andcomment is requested.

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11. Appendices III and X to 41o CFR Part261

The Agency is considering removingappendices III and X of part 261 from theregulations. Appendix III summarizesinformation found in SW-846 for theconvenience of the regulatedcommunity. It does not contain anyadditional or independent requirements.In addition, as currently framed,appendix III implies that use of SW-846is mandatory in all instances. This is notthe case. SW--846 is required for use inonly certain well defined instances (see54 FR 3212-3229, January 23, 1989). Toremove any ambiguity, the Agency isconsidering removal of appendix Ill inits entirety.

Appendix X was established to meetthe needs for the chemical analysis ofcertain wastes containing particularchlorinated dioxins, dibenzofurans, andphenols in order to establish thosewastes as acutely hazardous (see 50 FR1978-2006, January 14,1985). AppendixX contains Method 8280: Method ofAnalysis for Chlorinated Dibenzo-P-Dioxins and Dibenzofurans. Thismethod is superseded by the methodcontained in the Third Edition of SW-846, which is retitled Method 8280: TheAnalysis of Polychlorinated Dibenzo-P-Dioxins and PolychlorinatedDibenzofurans. To avoid any ambiguity,the Agency is considering removal ofappendix X in its entirety. Therefore, theAgency is requesting comments onremoval of appendices III and X fromthe Code of Federal Regulations.

The Agency's regulations contain noreferences to appendix X. The Agencyproposed to delete references toappendix III in its regulations as follows:

-Delete "Appendix i1" in 40 CFR260.22(d)(1){i) and insert in its place"'Test Methods for Evaluating SolidWaste, Physical/Chemical Methods,'EPA Publication SW--84, incorporatedby reference, see § 260.11(a)";

-Delete "referenced in 40 CFR part261, appendix II" in 40 CFR270.19(c)f1)(iii) and insert in its place"§ 260.11(a)"4

-Insert "'Test Methods forEvaluating Solid Waste, Physical/Chemical Methods,' EPA publicationSW-846, incorporated by reference, see§ 260.11(a), or * * " in 40,CFR260.1(b)(5) after the words "thoseprescribed in," in 40 CFR 260.20(a) afterthe words "Iesirg or analytical methodto," in40 CFR 260.21(a) after the words"testing or analytical method to" andafter the words "method." prescribedin," and in 40 CFR 260.21(b)(3) after thewords "methods prescribed in."

IV. Request for Comments

The Agency requests comments on: (1)The specific clarifications and/orchanges in procedures for use andinterpretation of guidance from theRCRA test methods manual, SW-846discussed above; (2) The "Report onMinimum Criteria to Assure DataQuality" and its replacement of theproposed Chapter One to SW-B46 asdiscussed in the January 1989 Notice;and (3) on the deletion of appendices Mand X to 40 CFR part 261. It should benoted that the Agency is only reopeningthe comment period on these specificpoints presented in this Notice.

Comments on this Notice must berecieved by EPA on or before March 12,1990, to ensure consideration. Commentsare to be addressed, in triplicate, toDocket Number F-90-WTRX-FFFFF.

Dated: January 29,1990.Mary A. Ceade,Acting AssistantAdministrator for SolidWaste and Emergenty Response.[FR Doc. 90-2972 Filed 2-7-90; 8:45 am]BILLING CODE 5560-50-M

DEPARTMENT OF TRANSPORTATION

Research and Special ProgramsAdministration

49 CFR Parts 171, 172, 173,174, 175,176,177, and 178

[Docket No. ,HM-169A; Notice No. 90-1]

Transportation Regulations;Compatibility With Regulations ofInternational Atomic Energy Agency,Extension of Comment Period

AGENCY: Research and Special ProgramsAdministration (RSPA], Department ofTransportation fDOI).ACTION: Extension of time -to filecomments.

SUMMARY: On November 14, 1989, RSPApublished a notice of proposedrulemaking (NPRM) in the FederalRegister (54 FR 47454]; Docket No. HM-169A, Notice No. 89-8 which proposedto align DOT's Hazardous MaterialRegulations PiMR; 49 CFR parts 171-180) with the 1985 Edition of theInternational Atomic Energy AgencyRegulations for the Safe Transport ofRadioactive Materials, Safety Series No.6. Because of the broad scope, detail andcomplexity of the proposals -containedwithin the NPRM, TheRadiopharmaceutical Shippers ardCarriers Conference, and -others,requested a 90 day extension of thecomment period. RSPA concurs with

these requests and this notice extendsthat comment period.DATES: The date for filing the commentsis extended from February 9, 1990, toMay 11, 1990.ADDRESSES: Address comments toDockets Unit (DHM-30), Office ofHazardous Materials Transportation,RSPA, U.S. Department -ofTransportation, Washington, DC 20590.Comments should identify the docketand notice number and be submitted,when possible, in five copies. Personswishing to receive confirmation ofreceipt of their comments should includea self-addressed stamped postcard. TheDockets Unit is located in Room 8419 ofthe Nassif Building, 400 Seventh Street,SW., Washington, DC 20590. Officehours are fr.30 a.m. to 5:00 p.m. Mondaythrough Friday, except federal holidays.FOR FURTHER INFORMATION CONTACT:Michael E. Wangler, Chief, RadioactiveMaterials Branch, Technical Division,Office of Hazardous MaterialsTransportation, 400 Seventh Street SW.,Washington, DC, 20590, (202) 366-4545.

Issued in Washirngton, DC on February 2,1990, under authority delegated in 49VFRpart 106, Appendix A.Alan 1. Roberts,Director, Office of Hazardous MaterialsTransportation.[FR Doc. 90-2850 Filed 2-7-90; 8:45 am]BILLING CODE 4910-60-M

National Highway Traffic Safety

Administration

49CFR Part 571

[Docket No. 90-02; Notice 11

RIN 2127-AD22

Federal Motor Vehicle SafetyStandards; New Pneumatic Tires

AGENCY: National Highway TrafficSafety Administration jNHTSAJ, DOT.ACTION: Notice of proposed rulemaking.

SUMMARY: This notice proposes -toimplement the petition by the EuropeanTyre and Rim Technical Organisation(E.T.R.T.O.) requesting that NHTSAamend its labeling requirements inStandard No. 109, New PneumaticTires-PassengerCar sto require amanufacturer to place the requiredmarkings between the bead and a pointone-half the distance from the bead tothe shoulder of the tire, if the tire'smaximum -section width is close to thebead. This amendment would add -toStandard No. 109 a provision previouslyadded by the agency to another tirestandard, the one related to tires on
