53988 federal register /vol. 60, no. 201/wednesday ... federal register/vol. 60, no. 201/wednesday,...

53988 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules

ENVIRONMENTAL PROTECTIONAGENCY

40 CFR Part 136

[FRL–5308–4]

Guidelines Establishing TestProcedures for the Analysis ofPollutants: New Methods

AGENCY: Environmental ProtectionAgency (EPA).ACTION: Proposed rule and request forcomment.

SUMMARY: Under the Clean Water Act,Section 304(h), EPA proposes to amendits list of approved analytical techniquesby adding new or revised testprocedures for certain metal andinorganic chemical pollutants, byadding method citations to Table IB andby amending the incorporation byreference section of the regulationaccordingly.

EPA is also proposing to substitutereagents that are more environmentallyfriendly for certain hazardous and toxicchemical reagents currently used incertain approved methods.

In addition, EPA is proposing towithdraw approval of certain outdatedor little used analytical methods, as wellas, certain methods that require the useof hazardous or toxic reagents. For eachmethod that is proposed for withdrawal,one or more commonly used methodshave been previously approved.

Comments are requested on thisproposed rulemaking. After consideringcomments received in response to thisproposal, EPA will promulgate a finalrule.

This action amends guidelinesestablishing test procedures for theanalysis of pollutants by addingclarifying notes to lists of approved testprocedures, by adding and updatingcertain method citations in Tables IBand IC, and by amending theincorporation by reference section of theregulation accordingly.DATES: Comments on the proposedamendments will be accepted untilDecember 18, 1995.ADDRESSES: Send written comments tothe 304(h) Docket Clerk (Ben Honaker),Water Docket (MC–4101), U.S.Environmental Protection Agency, 401M Street, SW., Washington, DC 20460.Please submit any references cited inyour comments. EPA would appreciatean original and three copies of yourcomments and enclosures (includingreferences). Commenters who want EPAto acknowledge receipt of theircomments should enclose a self-addressed, stamped envelope. No

facsimiles (faxes) will be acceptedbecause EPA cannot assure that theywill be submitted to the Water Docket.

The supporting materials are availablefor review at the Water Docket at theaddress above. For access to DocketMaterials, call (202) 260–3027 between9 am and 3:30 pm for an appointment.FOR FURTHER INFORMATION CONTACT: Mr.James E. Longbottom, Aquatic ResearchDivision, National Exposure ResearchLaboratory, Office of Research andDevelopment, U.S. EnvironmentalProtection Agency, Cincinnati, Ohio45268. Telephone number: (513) 569–7308.SUPPLEMENTARY INFORMATION:

Materials in the public docketinclude:

• ‘‘Methods for the Determination ofMetals in Environmental Samples’’Supplement I, EPA–600/R–94/111, May1994.

• ‘‘Methods for the Determination ofInorganic Substances in EnvironmentalSamples’’, EPA–600/R–93/100, August1993.

• ‘‘Determination of Trace Elementsin Water by Inductively CoupledPlasma-Mass Spectrometry:Collaborative Study’’, Journal of AOAC-International, 77, pp. 1004–1023, 1994.

• ‘‘Determination of Inorganic Anionsin Water by Ion Chromatography:Collaborative Study’’, Journal of AOAC-International, 77, pp. 1253–1263, 1994.

• ‘‘Ion Chromatographic Method forDissolved Hexavalent Chromium inDrinking Water, Ground Water, andIndustrial Wastewater Effluents:Collaborative Study’’, Journal of AOAC-International, 77, pp. 994–1004, 1994.

• ‘‘Low-level Chlorine Analysis byAmperometric Titration’’, Journal of theWater Pollution Control Federation, 51,pp. 2636–2640, 1979.

A copy of the first two items can alsobe obtained from EPA through afacsimile request to the ChemistryResearch Branch, Aquatic ResearchDivision, Cincinnati, Ohio, on (513)569–7757.

I. Authority

This regulation is proposed underauthority of sections 301, 304(h) and501(a) of the Clean Water Act, 33 U.S.C.1251 et seq. (the Federal WaterPollution Control Act Amendments of1972 as amended) (the ‘‘Act’’). Section301 prohibits the discharge of anypollutant into navigable waters unlessthe discharge complies with a NPDESpermit, issued under Section 402 of theAct. Section 304(h) of the Act requiresthe Administrator of the EPA to‘‘promulgate guidelines establishing testprocedures for the analysis of pollutants

that shall include the factors whichmust be provided in any certificationpursuant to section 401 of this Act orpermit application pursuant to section402 of this Act’’. Section 501(a) of theAct authorizes the Administrator to‘‘prescribe such regulations as arenecessary to carry out his functionsunder this Act’’.

The use of approved test proceduresor approved alternate procedures isrequired whenever the wasteconstituent specified is required to bemeasured for: an NPDES permitapplication; discharge monitoringreports; state certification; and otherrequests from the permitting authorityfor quantitative or qualitative effluentdata. Use of approved test procedures isalso required for the expression ofpollutant amounts, characteristics, orproperties in effluent limitationsguidelines and standards ofperformance and pretreatmentstandards, unless otherwise specificallynoted or defined.

II. Regulatory BackgroundThe CWA establishes two principal

bases for effluent limitations. First,existing discharges are required to meettechnology-based effluent limitations.New source discharges must meet newsource performance standards based onthe best demonstrated technology-basedcontrols. Second, where necessary,additional requirements are imposed toassure attainment and maintenance ofwater quality standards established bythe States under Section 303 of theCWA. In establishing or reviewingNPDES permit limits, EPA must ensurethat permitted discharges will not causeor contribute to a violation of waterquality standards, including designatedwater uses.

For use in permit applications,discharge monitoring reports, and statecertification and to ensure compliancewith effluent limitations, standards ofperformance, and pretreatmentstandards, EPA has promulgatedregulations providing nationally-approved testing procedures at 40 CFRPart 136. Test procedures havepreviously been approved for 262different parameters. Those proceduresapply to the analysis of inorganic(metal, non-metal, mineral) and organicchemical (including pesticides),radiological, biological, nutrient,demand, residue, and physicalparameters.

Additionally, some particularindustries may discharge pollutants forwhich test procedures have not beenproposed and approved under 40 CFRPart 136. Under 40 CFR 122.41 permitwriters may impose monitoring

53989Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules

requirements and establish test methodsfor pollutants for which no approvedPart 136 method exists. 40 CFR 122.41(j)(4). EPA may also approve additionaltest procedures when establishingindustry-wide technology-based effluentlimitations guidelines and standards asdescribed at 40 CFR 401.13.

The procedures for approval ofalternate test procedures (ATPs) aredescribed at 40 CFR 136.4 and 136.5.Under these procedures theAdministrator may approve alternatetest procedures for nationwide usewhich are developed and proposed byany person. 40 CFR 136.4 (a). Personswishing to use such alternateprocedures, must apply to the State orRegional EPA permitting office [forlimited approval under 136.4 (b)], andto the Director of the EnvironmentalMonitoring Systems Laboratory inCincinnati [for nationwide approvalunder 136.4 (d)]. As specified below,today’s proposed rule would approveadditional nationwide test proceduresfor certain metals, anions, Cr(VI) andVOCs in wastewater and relatedsamples.

III. Summary of Proposed MethodsThe proposed methods have been

reviewed by appropriate members ofand written in the EPA EnvironmentalMonitoring Management CouncilFormat.

The methods proposed for additioninclude new methods for: preparation ofsamples for metals analysis, inductivelycoupled plasma/mass spectrometry(ICP/MS), a stabilized temperaturegraphite furnace atomic absorption(STGFAA) method for metals, and ionchromatography (IC) methods for anionsand for hexavalent chromium [Cr(VI)]. Arevised EPA inductively coupledplasma atomic emission spectrometry(ICP–AES) method for metals to replacethe currently approved method, and alow-level extension of the approvedmethod for the determination of lowlevel total residual chlorine are alsobeing proposed.

Methods 200.7, 200.8, and 200.9 wereapproved for use in EPA’s drinkingwater programs at 40 CFR Part141.23(k)(1) on December 5, 1994 (59 FR62466). When the methods proposedtoday are promulgated at 40 CFR Part136 for use in EPA’s wastewaterprograms, these three methods will beconformed for the two programs.

Although not part of today’s proposal,the Agency’s Environmental MonitoringManagement Council (EMMC) will soonpropose integrated methods for citationin several regulations, including those atPart 136. The methods include agraphite furnace atomic absorption

spectrometry method for certain metalsand an inductively coupled plasmaatomic emissions spectrometry methodfor metals. These methods may beincluded in the final rule for today’sproposal.

In the interest of pollution prevention,EPA is proposing to replace mercuricsulfate with copper sulfate in the totalKjeldahl nitrogen methods and topermit the substitution of the AMCO–AEPA–1 Standard for the formazinstandard in the turbidity method.Replacement of these two reagentswould remove hazardous or potentiallycarcinogenic chemicals from use in EPAapproved methods.

A. Sample Preparation for TotalRecoverable Elements

EPA is proposing a new broad-purpose digestion procedure for totalrecoverable elements. It has theadvantage of being compatable withseveral of the approved measurementtechniques, which will allowlaboratories to achieve some costsavings by reducing preparations andincreasing flexibility in choosingapproved analytical techniques afterdigestion. This preparation procedure isa variation of the procedures given inthe previously approved EPA 200 SeriesMethods for ‘‘total recoverable’’ metalspublished in ‘‘Methods for ChemicalAnalysis of Water and Wastes’’. Itutilizes the same acid combination(nitric + hydrochloric) as the previous‘‘total recoverable’’ procedures, but theacid concentration has been modified bylowering the amount of hydrochloricacid.

This sample preparation procedurehas been incorporated into three EPAMethods proposed today, including, aMay 1994 revision of the approved ICP/AES Method 200.7, a new measurementtechnology ICP/MS Method 200.8, and astabilized temperature graphite furnaceautomatic absorption (GFAA) method(Method 200.9). In addition, EPA hasprepared a stand-alone version of thedigestion procedure: Method 200.2‘‘Sample Preparation Procedure forSpectrochemical Determination of TotalRecoverable Elements’’. EPA proposesto permit the substitution of Method200.2 for the digestion procedure incertain non-EPA approved directaspiration flame atomic absorptionprocedures. The digestion procedurehas been tested on various matricesusing determinative methods 200.7,200.8 and 200.9 and has been foundcomparable to previously approvedNPDES preparation procedures. Method200.2 was also validated throughinterlaboratory testing in the joint EPA/AOAC International study of Method

200.8. Each of the new EPA proceduresincludes: a list of elements to which itapplies, sample preservation practices,and preparation conditions.

EPA proposes to withdraw the EPAAA direct aspiration and AA furnacemethods contained in ‘‘Methods forChemical Analysis of Water andWastes’’. The methods are out of dateand lack many of the necessaryinstructions included in more recentlyproduced EPA methods. The remainingapproved non-EPA methods for AAdirect aspiration are sufficientlyidentical to the withdrawn methods asto result in no impact on the regulatedcommunity. The EPA furnace methodsare being replaced by EPA Method200.9. Appendix D to this regulation,which contains the interlaboratorymeasures of precision and accuracy forthe EPA methods that are beingwithdrawn, would also be removed bythis proposal.

B. Elemental Analysis by ICP/AESThe EPA proposes to approve the May

1994 revision of Method 200.7,‘‘Determination of Metals and TraceElements in Water and Wastes byInductively Coupled Plasma-AtomicEmission Spectrometry’’ and to cite therevised method by reference.Accordingly, Appendix C to 40 CFR Part136 would be deleted. The May 1994edition of the method has beendemonstrated to produce precision andrecovery for the applicable elementsthat is equal to or better than thatachieved by the currently approvededition and published in Table 4 ofAppendix C. The procedure includes: Alist of elements to which it applies,sample collection practices, preparationconditions, and quality controlpractices. The EMMC inductivelycoupled plasma-atomic emissionspectrometry method being proposedelsewhere is proposed to beinterchangeable with Method 200.7 forthe purposes of this regulation.

C. Elemental Analysis by ICP/MSThe Agency is proposing a new

multielement test procedure, ICP/MS,Method 200.8 ‘‘Determination of TraceElements in Waters and Wastes byInductively Coupled Plasma-MassSpectrometry’’ for the detection andquantification of 20 metals in aqueoussamples. Sample material in solution isintroduced by pneumatic nebulizationinto a radio-frequency plasma whereenergy transfer processes causedesolvation, atomization and ionization.The ions are extracted from the plasmathrough a differentially pumpedvacuum interface and separated on thebasis of their mass-to-charge ratio by a


quadrupole mass spectrometer having aminimum resolution capability of 1 amupeak width at 5% peak height. The ionstransmitted through the quadrupole areregistered by an electron multiplier orFaraday detector and the ioninformation processed by a datahandling system. Interferences relatingto the technique must be identified andresults must be corrected accordingly.Such corrections must includecompensation for isobaric elementalinterferences and interferences frompolyatomic ions derived from theplasma gas, reagents or sample matrix.Instrumental drift, as well assuppressions or enhancements ofinstrument response caused by thesample matrix, must be corrected by theuse of internal standardization.

The Agency developed ICP/MSMethod 200.8 under a contract and incooperation with AOAC Internationaljointly conducted an interlaboratoryvalidation study of the method. Thismethod (May 1994) represents thecurrent state-of-the-art for thedetermination of metals in wastewaterand water related media. The methoddescription includes a list of theelements to which the method applies,sample collection practices,recommended analytical conditions,quality control practices, instrumentaland method detection limits, andperformance criteria based on theinterlaboratory study data.

AOAC-International has approvedand published this ICP/MS methodalong with the study results as AOAC-International Method 993.14. The samemethod is in the final stages of theASTM consensus process. EPA proposesto approve the AOAC-Internationalmethod, as well as, consider approval ofthe ASTM ICP/MS Method if full ASTMSociety acceptance is achieved prior tofinal EPA rulemaking.

D. Elemental Analysis by StabilizedTemperature Platform GFAA

The May 1994 Revision of Method200.9 ‘‘Determination of Trace Metals byStabilized Temperature GraphiteFurnace Atomic Absorption’’ is beingproposed as a replacement for thecurrently approved EPA furnacemethods. Method 200.9 determineselements by stabilized temperaturegraphite furnace atomic absorption(STGFAA). In STGFAA, the sample andrequired matrix modifier are firstpipetted onto the platform or a devicewhich provides delayed atomization.The sample is then dried at a relativelylow temperature (≈120°C) to avoidspattering. Once dried, the sample isnormally pretreated in a char or ashingstep which is designed to minimize the

interference effects caused by theconcomitant sample matrix. After thechar step, the furnace is allowed to coolprior to atomization. The atomizationcycle is characterized by rapid heatingof the furnace to a temperature wherethe metal (analyte) is atomized from thepyrolytic graphite surface. The resultingatomic cloud absorbs the elementspecific atomic emission produced by ahollow cathode lamp or a electrodelessdischarge lamp.

Because the resulting absorbanceusually has a nonspecific componentassociated with the actual analyteabsorbance, an instrumental backgroundcorrection device is necessary tosubtract from the total signal thecomponent which is nonspecific to theanalyte. In the absence of interferences,the background corrected absorbance isdirectly related to the concentration ofthe analyte. Interferences relating tosuppression or enhancement ofinstrument response caused by thesample matrix, must be corrected by themethod of standard addition.

The method description includes alist of elements to which the methodapplies, sample collection practices,recommended analytical conditions,quality control practices, methoddetection limits and performancecriteria based on single laboratory studydata. The EMMC furnace atomicabsorption method being proposedelsewhere is proposed to beinterchangeable with Method 200.9 forthe purposes of this regulation.

E. Anions by Ion ChromatographyEPA developed IC Method 300.0 for

the following anions: Bromide, chloride,fluoride, nitrate-N, nitrite-N, ortho-phosphate, and sulfate. Using IC, awater sample is injected into a stream ofcarbonate-bicarbonate eluent and passedthrough a series of ion exchangers. Theanions of interest are separated on thebasis of their relative affinities for a lowcapacity, strongly basic anion exchanger(guard and separator columns). Theseparated anions are directed through ahollow fiber cation exchangermembrane (fiber suppressor) ormicromembrane suppressor bathed incontinuously flowing strongly acidsolution (regenerant solution). In thesuppressor the separated anions areconverted to their highly conductiveacid forms and the carbonate-bicarbonate eluent is converted toweakly conductive carbonic acid. Theseparated anions in their acid forms aremeasured by conductivity. They areidentified on the basis of retention timeas compared to reference standards.Quantitation is by measurement of peakarea or peak height.

EPA, in cooperation with ASTMCommittee D–19 on Water, hasconducted an interlaboratory validationstudy of EPA method 300.0 ‘‘TheDetermination of Inorganic Anions inWater by Ion Chromatography’’, August1993. The method represents currentstate-of-the-art for determination of theanions listed above. The methoddescription includes: Sample collectionpractices, recommended analyticalconditions, quality control practices andestimated detection limits for theapplicable analytes and performancecriteria based on the interlaboratorystudy data. ASTM, Standard Methods,and AOAC-International have approvedthe method under their consensussystems and have published the methodin their Books of Standards. EPA alsoproposes to approve the ASTM MethodD–4327, as well as, Method 4110 Bpublished in the 18th edition of‘‘Standard Methods for the Examinationof Water and Wastewater’’ (SMEWW)and AOAC-International Method 993.30all of which were derived from EPAMethod 300.0.

F. Cr (VI) by Ion ChromatographyUsing the IC Cr(VI) Method (Method

218.6), an aqueous sample is filteredthrough a 0.45 µm filter and the filtrateis adjusted to a pH of 9 to 9.5 with abuffer solution. A measured volume ofsample (50–250 µl) is introduced intothe ion chromatograph. A guard columnis employed to remove organics fromthe sample prior to separation of Cr(VI)as CrO4

¥2 on an anion exchangeseparator column. Cr(VI) is determinedby post column derivatization withdiphenylcarbazide and passing througha low-volume flow-through cell anddetection of the colored complex with avisible lamp detector at 530 nm.

EPA, in cooperation with ASTMCommittee D–19 on Water, hasconducted an interlaboratory validationstudy of EPA Method 218.6‘‘Determination of Dissolved HexavalentChromium in Drinking Water, GroundWater, and Industrial WastewaterEffluents by Ion Chromatography’’. Themethod description includes: Samplecollection practices, recommendedanalytical conditions, quality controlpractices and method detection limitsfor Cr(VI), as well as performancecriteria based on the interlaboratorystudy data.

ASTM, Standard Methods, andAOAC-International have approved thismethod as a standard test method undertheir consensus systems and havepublished it in their manuals ofmethods. EPA also proposes to approvethe ASTM Method D–5257, StandardMethods Method 3500–Cr E, and


Method 993.23 from the AOAC-International Official Methods ofAnalysis, 16th Edition. All three ofthese methods were derived from EPAMethod 218.6.

G. Method for Determination of LowLevel Residual Chlorine

EPA is proposing to additionallyapprove SMEWW, Method 4500–Cl Efor the detection and quantification oflow levels of chlorine in water. Thismethod is a minor modification of theapproved amperometric Method 4500–Cl D and is capable of measuring downto 10 µg/L chlorine. Federal and Statepermitting authorities have requestedsuch a method in order to assesscompliance with effluent limits basedon EPA and State water quality criteriafor chlorine. Supporting performancedata for the method can be found atJournal of the Water Pollution ControlFederation, Vol. 51, pages 2636–2640(1979), a copy of which is included inthe docket for this proposal.

H. Replacement of Mercury Catalyst inTotal Kjeldahl Nitrogen Methods

Due to demonstrated toxic hazards ofmercuric sulfate, and difficulty ofdisposal of laboratory wastes, EPA isproposing to replace this chemical withcopper sulfate in the total KjeldahlNitrogen Methods. Copper sulfateexhibits significantly less toxicity thanmercuric sulfate. The Europeancommunity has already eliminatedmercuric chloride from their totalnitrogen methods in favor of less toxiccatalysts.

I. EPA is proposing to amend EPAMethod 180.1—Turbidity by acceptingthe use of styrene divinylbenzene beads(AMCO–AEPA–1 Standard) as asubstitute for the presently usedformazine standard, which is preparedfrom hydrazine sulfate. The AEPA–1Standard is an alternate to formazine inthe previously approved StandardMethods, Method 2130 B. Thissubstitution will eliminate the need touse hydrazine sulfate, a knowncarcinogen.

J. EPA is proposing to delete liquid-liquid extraction (LLE) methods,including EPA Methods 611 and 625and Standard Methods Method 6410 B,as approved procedures for 1,2-dichlorobenzene, 1,3-dichlorobenzene,and 1,4-dichlorobenzene. While thesecompounds can be determined by theseLLE methods, due to their volatility,significant losses can occur when usingthe prescribed sample collectionprocedures in the LLE methodsresulting in low recovery of thesecompounds. These compounds are moreproperly analyzed by EPA Method 624

or Method 1625 (an isotope-dilutionmethod that compensates for anyevaporation losses).

K. EPA proposes to delete extraneousmethod citations, including those EPAmethods that reference another sourcefor method details and certain olderEPA methods that are readily availablefrom another source. Somemeasurement technologies are proposedfor removal because they are no longersupported by the group that authoredthem or they use toxic reagents. EPAplans to provide an 18-month transitionperiod after final rule to permitcontinued use of these methodsfollowing the practice of the drinkingwater program (see 59 FR 62456). Thesedeletions include: colorimetric methodsfor cadmium, lead and zinc (dithizone),copper (neocuprione), nickel(heptoxime), nitrate-nitrite (automatedhydrazine), potassium (cobaltinitrite),vanadium (gallic acid); AA furnacemethods for gold, iridium, platinum,rhodium, ruthenium, titanium, andzinc; flame phometric methods forpotassium and sodium; voltametry forcadmium and lead; titration (mercuricnitrate) for chloride; and the AAchelation-extraction for total chromium.Table IB of Part 136(a) would be furtherrevised to reorder and clarify footnotesand method citations.

IV. Request for CommentsThe Agency requests general

comments on its policy to remove orreject methods from this regulation onthe basis of pollution prevention whencomparable approved methods areavailable. Comments on the specificmethods removed today are alsosolicited, as well as, comments on otherpollution prevention changes thatshould be considered by the Agency.EPA considered the elimination of theNessler method for Total Kjeldahlbecause the Nessler reagent contains10% mercuric iodide. However, anassessment of the data submitted byparticipants in recent Water Pollution(WP) performance evaluation studiesindicated that the Nessler method isbroadly used and produces above-average data compared to the otherapproved methods. Further, the Nesslermethod may be necessary to thisregulation because it is more sensitivethan the other methods. The Agencyrequests comments on whether theNessler methods should be removedfrom Part 136.

V. Regulatory Requirements

A. Executive Order 12866

Under Executive Order 12866, EPAmust determine whether a regulation is

‘‘significant’’ and, therefore subject toOMB review and the requirements ofthe Executive Order. EPA hasdetermined that this regulation is not a‘‘significant regulatory action’’ underthe terms of Executive Order 12866 andis therefore not subject to OMB review.This rule will not result in an effect onthe economy of $100 million or more, asignificant increase in cost or prices, orany of the effects described in theExecutive Order. This proposed rulesimply specifies analytical techniqueswhich may be used by laboratories inmeasuring concentrations of certainmetals and, therefore, has no adverseeconomic impacts.

B. Regulatory Flexibility ActThis proposed amendment is

consistent with the objectives of theRegulatory Flexibility Act (5 U.S.C. 601et seq.) because it will not have asignificant economic impact on asubstantial number of small entities.The procedures proposed in this rulegive all laboratories the flexibility to usethe new proposed procedures or alreadyapproved alternate procedures.

C. Paperwork Reduction ActThis proposed rule contains no

requests for information activities and,therefore, no information collectionrequest (ICR) was submitted to theOffice of Management and Budget(OMB) for review in compliance withthe Paperwork Reduction Act, 44 U.S.C.3501 et seq.

D. Unfunded MandatesUnder Section 202 of the Unfunded

Mandates Reform Act of 1995, signedinto law on March 22, 1995, EPA mustprepare a written statement toaccompany rules where the estimatedcosts to State, local, or tribalgovernments, or to the private sectorwill be $100 million or more in any oneyear. Under Section 205, EPA mustselect the most cost-effective and leastburdensome alternative that achievesthe objective of such a rule and that isconsistent with statutory requirements.Section 203 requires EPA to establish aplan for informing and advising anysmall governments that may besignificantly and uniquely affected bythe rule.

EPA estimates that the costs to State,local or tribal governments, or theprivate sector, from this proposed rulewill be far less than $100 million. Thisproposed rule should have minimalimpact, if any, on the existing regulatoryburden imposed on NPDES permitteesrequired to monitor for regulatedpollutants because the proposed rulewould merely make additional options


available to the laboratory analystconducting an existing approved testmethod. EPA has determined that anunfunded mandates statement thereforeis unnecessary. Similarly, the methodsproposed today do not establish anyregulatory requirements that mightsignificantly or uniquely affect smallgovernments.

List of Subjects in 40 CFR Part 136Environmental protection,

Incorporation by reference, Waterpollution control.

Dated: October 10, 1995.Carol M. Browner,Administrator.

In consideration of the preceding,EPA proposes to amend part 136 of title40 of the Code of Federal Regulations asfollows:

PART 136—[AMENDED]

1. The authority citation for part 136continues to read as follows:

Authority: Secs. 301, 304(h), 307, and501(a) Public Law 95–217, Stat. 1566, et seq.

(33 U.S.C. 1251 et seq. (the Federal WaterPollution Control Act Amendments of 1972as amended by the Clean Water Act of 1977).

2. Section 136.3(a) is proposed to beamended by revising Table IB to read asfollows:

§ 136.3 Identification of test procedures.

* * * * *

53993Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed RulesT

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3E

......

......

......

......

......

.....

......

......

......

......

......

......

......

Ele

ctro

de...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...45

00–N

H3

F o

r G

D14

26–9

3(B

)...

......

......

......

......

......

......

......

......

...A

utom

ated

phe

nate

, or

......

......

......

......

......

......

......

......

......

......

..35

0.1

4500

–NH

3H

......

......

......

......

......

..I–

4523

–85

Aut

omat

ed e

lect

rode

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

175.

Ant

imon

y-T

otal

4,

mg/

L:D

iges

tion

56

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/A

ES

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

146.

Ars

enic

-Tot

al4,

mg/

L:D

iges

tion

56

follo

wed

by:

AA

gas

eous

hyd

ride

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

3114

B 4

.dD

2972

–93(

B)

I–30

62–8

5A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

200.

931

13 B

D29

72–9

3(C

)...

......

......

......

......

......

......

......

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

ICP

/MS

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

...20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

Col

orim

etric

(S

DD

C)

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..D

2972

–93(

A)

I–30

60–8

57.

Bar

ium

—T

otal

4m

g/L:

Dig

estio

n5

6fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

D...

......

......

......

......

.....

I–30

84–8

5A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3113

BD

4382

–91

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 16

8. B

eryl

lium

—T

otal

4,

mg/

L:D

iges

tion5

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 D

D36

45–9

3(A

)I–

3095

–85

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

BD

3645

–93(

B)

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

Col

orim

etric

(al

umin

on)

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...35

00–B

e D

......

......

......

......

......

.....

......

......

......

......

......

......

......

9. B

ioch

emic

al o

xyge

n de

man

d (B

OD

5),

mg/

L:D

isso

lved

Oxy

gen

Dep

letio

n...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...52

10 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

973.

44,

p.17

18

53994 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed RulesT

AB

LEIB

.—LI

ST

OF

AP

PR

OV

ED

INO

RG

AN

ICT

ES

TP

RO

CE

DU

RE

S—

Con

tinue

d

Par

amet

er,

Uni

ts a

nd M

etho

dE

PA

1

Ref

eren

ce (

Met

hod

No.

or

Pag

e)

Std

. M

etho

ds 1

8th

Ed.

AS

TM

US

GS

2A

OA

C-in

ter-

natio

nal3

and

othe

rs

10.

Bor

on8—

Tot

al,

mg/

L:C

olor

imet

ric (

curc

umin

)...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

4500

–B B

......

......

......

......

......

..I–

3112

–85

......

......

......

......

..IC

P/A

ES

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...D

CP

....

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

..D

4190

–82(

88)

......

......

......

......

......

......

......

...N

ote

1611

. B

rom

ide,

mg/

L;T

itrim

etric

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

D12

46–8

2(88

)(C

)I–

1125

–85

p. S

4419

Ion

Chr

omat

ogra

phy

......

......

......

......

......

......

......

......

......

......

......

......

.30

0.0

4110

BD

4327

–91

......

......

.....

......

......

......

......

......

......

......

993.

3012

. C

adm

ium

—T

otal

4,

mg/

L:D

iges

tion

5,6

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

or

CD

3557

–90(

A o

r B

)I–

3135

–85

or I

–313

6–85

974.

2 p.

37

18

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

BD

3557

–90(

D)

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

13.

Cal

cium

—T

otal

4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

BD

511–

93(B

)I–

3152

–85

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

DC

P,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

16T

itrim

etric

(E

DT

A)

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3500

–Ca

DD

511–

93(A

)...

......

......

......

......

......

......

......

14.

Car

bona

ceou

s bi

oche

mic

al o

xyge

n de

man

d (C

BO

D5),

mg/

L9...

......

......

......

......

......

......

......

5210

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...D

isso

lved

Oxy

gen

Dep

letio

n w

ith n

itrifi

catio

n in

hibi

tor

15.

Che

mic

al o

xyge

n de

man

d (C

OD

), m

g/L:

Titr

imet

ric,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

410.

315

5220

BD

1252

–88(

A)

I–35

60–8

5, I

–356

2–85

973.

46,

p. 1

718

Spe

ctro

phot

omet

ric,

man

ual o

r au

tom

ated

......

......

......

......

......

......

..41

0.4

5220

DD

1252

–88(

B)

I–35

61–8

5N

otes

20,

21

16.

Chl

orid

e, m

g/L:

Titr

imet

ric (

silv

er n

itrat

e)...

......

......

......

......

......

......

......

......

......

......

....

4500

–Cl B

D51

2–89

(B)

I–11

83–8

5C

olor

imet

ric,

Man

ual,

or...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

I–11

87–8

5...

......

......

......

.....

Aut

omat

ed (

Fer

ricya

nide

), o

r...

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...45

00–C

l-E...

......

......

......

......

.....

I–21

87–8

5...

......

......

......

.....

Ion

Chr

omat

ogra

phy

......

......

......

......

......

......

......

......

......

......

......

......

.30

0.0

4110

BD

4327

–91

......

......

......

......

......

......

......

...99

3.30

17.

Chl

orin

e—T

otal

res

idua

l, m

g/L:

Titr

imet

ric:

Am

pero

met

ric d

irect

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...45

00–C

l D o

r E

D12

53–8

6(92

)...

......

......

......

......

......

......

......

Iodo

met

ric d

irect

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

4500

–Cl B

......

......

......

......

......

.....

......

......

......

......

......

......

......

Bac

k tit

ratio

n ei

ther

end

-poi

nt10

......

......

......

......

......

......

......

......

4500

–Cl C

......

......

......

......

......

.....

......

......

......

......

......

......

......

DP

D-F

AS

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

4500

–Cl F

......

......

......

......

......

.....

......

......

......

......

......

......

......

Spe

ctro

phot

omet

ric (

DP

D),

or

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

4500

–Cl G

......

......

......

......

......

.....

......

......

......

......

......

......

......

Ele

ctro

de...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

2218

. C

hrom

ium

VI

diss

olve

d, m

g/L:

0.45

mic

ron

filtr

atio

n fo

llow

ed b

y:A

A c

hela

tion-

extr

actio

n...

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

3111

C...

......

......

......

......

.....

I–12

32–8

5Io

n C

hrom

atog

raph

y, o

r...

......

......

......

......

......

......

......

......

......

...21

8.6

3500

–Cr

E23

D52

57–9

3...

......

......

......

......

......

......

......

993.

23C

olor

imet

ric (

Dip

heny

lcar

bazi

de)

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3500

–Cr

DD

1687

–92(

A)

I–12

30–8

519

. C

hrom

ium

—T

otal

4,

mg/

L:D

iges

tion

5,6

6fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

D16

87–9

2(B

)I–

3236

–85

974.

27A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

200.

931

13 B

D16

87–9

2(C

)...

......

......

......

......

......

......

......

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

....

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

Col

orim

etric

(D

iphe

nylc

arba

zide

)...

......

......

......

......

......

......

......

....

......

......

......

......

......

...35

00–C

r D

......

......

......

......

......

.....

......

......

......

......

......

......

......

20.

Cob

alt—

Tot

al4,

mg/

L:

53995Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed RulesD

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

B o

r C

D35

58–9

0(A

or

B)

I–32

39–8

5p.

3718

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

BD

3558

–90(

C)

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

21.

Col

or,

plat

inum

cob

alt

units

or

dom

inan

t w

avel

engt

h, h

ue,

lum

i-na

nce

purit

y:C

olor

imet

ric (

AD

MI)

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...21

20 E

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 24

Col

orim

etric

(P

latin

um c

obal

t),

or...

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...21

20B

......

......

......

......

......

..I–

1250

–85

......

......

......

......

..S

pect

roph

otom

etric

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...21

20 C

......

......

......

......

......

.....

......

......

......

......

......

......

......

22.

Cop

per—

Tot

al4,

mg/

L:D

iges

tion

5,6

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

or

CD

1688

–90(

A o

r B

)I–

3270

–85

or I

–327

1–85

974.

27p.

3718

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

BD

1688

–90(

C)

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

ICP

/MS

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

DC

P,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

......

..D

4190

–82(

88)

......

......

......

......

......

......

......

...N

ote

16C

olor

imet

ric (

Bic

inch

onin

ate)

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

2523

. C

yani

de—

Tot

al,

mg/

L:M

anua

l dis

tilla

tion1

1w

ith M

gCl 2

follo

wed

by:

335.

445

00–C

N C

D20

36–9

1(A

)...

......

......

......

......

......

......

......

Titr

imet

ric...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...45

00–C

N D

......

......

......

......

......

.....

......

......

......

......

......

......

......

p.22

19

Spe

ctro

phot

omet

ric,

man

ual o

r...

......

......

......

......

......

......

......

....

......

......

......

......

......

......

4500

–CN

ED

2036

–91(

A)

I–33

00–8

5S

pect

roph

otom

etric

, au

tom

ated

......

......

......

......

......

......

......

......

335.

4...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

24.

Cya

nide

am

enab

le t

o ch

lorin

atio

n, m

g/L:

Man

ual

dist

illat

ion

with

M

gCl 2

, fo

llow

ed

by

titrim

etric

or

spec

trop

hoto

met

ric.

......

......

......

......

......

......

4500

–CN

GD

2036

–91(

B)

......

......

......

......

......

......

......

......

......

25.

Flu

orid

e—T

otal

, m

g/L:

Man

ual d

istil

latio

n7,

follo

wed

by:

......

......

......

......

......

......

4500

–F B

......

......

......

......

......

.....

......

......

......

......

......

......

......

Ele

ctro

de,

Man

ual.

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...45

00–F

CD

1179

–93(

B)

......

....

......

......

......

......

......

......

......

...E

lect

rode

, A

utom

ated

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

I–43

27–8

5C

olor

imet

ric (

SP

AD

NS

)...

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

4500

–F D

D11

79–9

3(A

)...

......

......

......

......

......

......

......

Col

orim

etric

(A

uto

com

plex

one)

, or

......

......

......

......

......

......

......

....

......

......

......

......

......

...45

00–F

-E...

......

......

......

......

.....

......

......

......

......

......

......

......

...Io

n C

hrom

atog

raph

y...

......

......

......

......

......

......

......

......

......

......

...30

0.0

4110

BD

4327

–91

......

......

......

......

......

......

......

...99

3.30

26.

Gol

d—T

otal

4,

mg/

L:D

iges

tion5

follo

wed

by:

AA

dire

ct a

spira

tion,

or

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...31

11 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

DC

P...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

1627

. H

ardn

ess—

Tot

al,

as C

aCO

3,

mg/

L:A

utom

ated

col

orim

etric

......

......

......

......

......

......

......

......

......

......

......

...13

0.11

5...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Titr

imet

ric (

ED

TA

), o

r...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...23

40 B

or

CD

1126

–86(

92)

I–13

38–8

597

3.52

BC

a pl

us M

g as

the

ir ca

rbon

ates

, by

IC

P/A

ES

, A

A d

irect

asp

iratio

n,or

DC

P.

(Par

amet

ers

13 a

nd 3

3).

28.

Hyd

roge

n io

n (p

H),

pH

uni

ts:

Ele

ctro

met

ric m

easu

rem

ent,

or...

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

4500

–H+

BD

1293

–84(

90)

(A o

rB

)I–

1586

–85

973.

41

Aut

omat

ed e

lect

rode

......

......

......

......

......

......

......

......

......

......

......

......

.15

0.2

15

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

2629

. Ir

idiu

m—

Tot

al4,

mg/

L:D

iges

tion5

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

30.

Iron

—T

otal

4,

mg/

L:D

iges

tion5

,6fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

B D

D10

68–9

0(A

or

B)

I–33

81–8

597

4.27

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

BD

1068

–90(

C)

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...D

CP

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

Col

orim

etric

(P

hena

nthr

olin

e)...

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 27

31.

Kje

ldah

l nitr

ogen

—T

otal

, (a

s N

), m

g/L:

Dig

estio

n12

and

dist

illat

ion.


AB

LEIB

.—LI

ST

OF

AP

PR

OV

ED

INO

RG

AN

ICT

ES

TP

RO

CE

DU

RE

S—

Con

tinue

d

Par

amet

er,

Uni

ts a

nd M

etho

dE

PA

1

Ref

eren

ce (

Met

hod

No.

or

Pag

e)

Std

. M

etho

ds 1

8th

Ed.

AS

TM

US

GS

2A

OA

C-in

ter-

natio

nal3

and

othe

rs

follo

wed

by:

......

......

......

......

......

......

4500

–Norg

B o

r C

...D

3590

–89(

A)

......

......

......

......

......

......

......

...T

itrat

ion

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...45

00–N

H3

ED

3590

–89(

A)

......

......

......

......

......

......

......

...97

3.48

Nes

sler

izat

ion,

or

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

4500

–NH

3C

D35

90–8

9(A

)...

......

......

......

......

......

......

......

Ele

ctro

de...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...45

00–N

H3

F o

r G

......

......

......

......

......

...

Col

orim

etric

(A

utom

ated

phe

nate

)12

......

......

......

......

......

......

......

......

l351

.115

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...S

emi-a

utom

ated

blo

ck d

iges

tor1

2co

lorim

etric

, or

......

......

......

......

...35

1.2

......

......

......

......

......

..D

3590

–89(

B)

......

......

......

......

......

......

......

...M

anua

l or

bloc

k di

gest

or12

pote

ntio

met

ric...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..D

3590

–89(

A)

......

......

......

......

......

......

......

...B

lock

dig

esto

r, f

ollo

wed

by:

Aut

o di

still

atio

n an

d T

itrat

ion,

or

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

28N

essl

eriz

atio

n or

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 29

Flo

w in

ject

ion

gas

diffu

sion

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 30

32.

Lead

—T

otal

4,

mg/

L:D

iges

tion

56

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

or

CD

3559

–90(

A o

r B

)I–

3399

–85

974.

27A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

200.

931

13 B

D35

59–9

0(D

)...

......

......

......

......

......

......

......

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

ICP

/MS

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

...20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

DC

P...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

..D

4190

–82(

88)

......

......

......

......

......

......

......

...N

ote

1633

. M

agne

sium

—T

otal

4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

BD

511–

93(B

)I–

3447

–85

974.

27IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 16

Gra

vim

etric

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...35

00-M

g D

......

......

......

......

......

.....

......

......

......

......

......

......

......

34.

Man

gane

se—

Tot

al4,

mg/

L:D

iges

tion

5,6

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

D85

8–90

(A o

r B

)I–

3454

–85

974.

27A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

200.

931

13 B

D85

8–90

(C)

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

Col

orim

etric

(P

ersu

lfate

), o

r...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

920.

203

Col

orim

etric

(P

erio

date

)...

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

3135

. M

ercu

ry—

Tot

al4,

mg/

LC

old

vapo

r, m

anua

l, or

......

......

......

......

......

......

......

......

......

......

......

...24

5.1

3112

BD

3223

–91

I–34

62–8

597

7.22

Col

d va

por,

aut

omat

ed...

......

......

......

......

......

......

......

......

......

......

......

245.

2...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

36.

Mol

ybde

num

—T

otal

4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

D...

......

......

......

......

.....

I–34

90–8

5A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3113

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

OR

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

DC

P...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

1637

. N

icke

l—T

otal

4,

mg/

L:D

iges

tion

56

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

or

CD

1886

–90(

A o

r B

)I–

3499

–85

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

BD

1886

–90(

C)

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

......

......

......

......

......

Not

e 16

38.

Nitr

ate

(as

N),

mg/

L:C

olor

imet

ric (

Bru

cine

sul

fate

)...

......

......

......

......

......

......

......

......

......

..15

352.

1...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

973.

50,

p.28

18

53997Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed RulesIo

n C

hrom

atog

raph

y, o

r...

......

......

......

......

......

......

......

......

......

......

.....

300.

041

10 B

D43

27–9

1...

......

......

......

......

......

......

......

993.

30N

itrat

e-ni

trite

N m

inus

Nitr

ite N

(S

ee p

aram

eter

s 39

and

40)

39.

Nitr

ate-

nitr

ite (

sum

as

N),

mg/

L:C

adm

ium

red

uctio

n, M

anua

l...

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

4500

–NO

3E

D38

67–9

0(B

)...

......

......

......

......

......

......

......

Cad

miu

m r

educ

tion,

Aut

omat

ed,

or...

......

......

......

......

......

......

......

.....

353.

245

00–N

O3

FD

3867

–90(

A)

I–45

45–8

5Io

n C

hrom

atog

raph

y...

......

......

......

......

......

......

......

......

......

......

......

....

300.

041

10 B

D43

27–9

1...

......

......

......

......

......

......

......

993.

3040

. N

itrite

(as

N),

mg/

L:S

pect

roph

otom

etric

, M

anua

l, or

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...45

00–N

O2

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

32A

utom

ated

(D

iazo

tizat

ion)

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

..I–

4540

–85

Cad

miu

m r

educ

tion,

Man

ual

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...45

00–N

O3

E...

......

.D

3867

–90(

B)

......

......

......

......

......

......

......

...C

adm

ium

red

uctio

n, A

utom

ated

, or

......

......

......

......

......

......

......

......

..35

3.2

4500

–NO

3F

D38

67–9

0(A

)I–

4545

–85

Ion

Chr

omat

ogra

phy

......

......

......

......

......

......

......

......

......

......

......

......

.30

0.0

4110

BD

4327

–91

......

......

......

......

......

......

......

...99

3.30

41.

Oil

and

grea

se—

Tot

al r

ecov

erab

le,

mg/

L:G

ravi

met

ric (

extr

actio

n)...

......

......

......

......

......

......

......

......

......

......

.....

413.

155

20–B

33

......

......

......

......

......

.....

......

......

......

......

......

......

......

42.

Org

anic

car

bon—

Tot

al (

TO

C),

mg/

L:C

ombu

stio

n or

oxi

datio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

5310

–B,C

or

DD

2579

–93(

A o

r B

)...

......

......

......

......

......

......

......

973.

47,

p.14

35

43.

Org

anic

nitr

ogen

(as

N),

mg/

L:T

otal

Kje

ldah

l N (

Par

amet

er 3

1) m

inus

am

mon

ia N

(P

aram

eter

4)

44.

Ort

hoph

osph

ate

(as

P),

mg/

L:A

scor

bic

acid

met

hod:

Aut

omat

ed,

or...

......

......

......

......

......

......

......

......

......

......

......

......

.36

5.1

4500

–P F

......

......

......

......

......

..I–

4601

–85

973.

56M

anua

l sin

gle

reag

ent

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...45

00–P

ED

515–

88(A

)...

......

......

......

......

......

......

......

973.

55M

anua

l tw

o re

agen

t, or

......

......

......

......

......

......

......

......

......

......

.36

5.3

15

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...Io

n C

hrom

atog

raph

y...

......

......

......

......

......

......

......

......

......

......

......

....

300.

041

10 B

D43

27–9

1...

......

......

......

......

......

......

......

993.

3045

. O

smiu

m—

Tot

al,4

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n, o

r...

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

3111

D...

......

......

......

......

.....

......

......

......

......

......

......

......

...A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...46

. O

xyge

n di

ssol

ved,

mg/

L:W

inkl

er (

Azi

de m

odifi

catio

n),

or...

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

4500

–O C

D88

8–92

(A)

......

......

......

......

......

......

......

...97

3.45

BE

lect

rode

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...45

00–O

GD

888–

92(B

)...

......

......

......

......

......

......

......

47.

Pal

ladi

um—

Tot

al,4

mg/

L:D

iges

tion5

follo

wed

by:

AA

dire

ct a

spira

tion,

......

......

......

......

......

......

3111

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...p.

S27

19

AA

gra

phite

fur

nace

, or

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

..p.

S28

19.

DC

P...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

1648

. (R

eser

ved)

49.

Phe

nols

, m

g/L:

Man

ual d

istil

latio

n,13

follo

wed

by

Col

orim

etric

(4A

AP

) m

anua

l, or

......

......

......

......

......

......

......

......

15

420.

1...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 35

Col

orim

etric

(4A

AP

) A

utom

ated

......

......

......

......

......

......

......

......

420.

4...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

50.

Pho

spho

rus

(ele

men

tal),

mg/

L G

as-li

quid

chr

omat

ogra

phy

......

......

.....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 36

51.

Pho

spho

rus—

Tot

al,

mg/

L:P

ersu

lfate

dig

estio

n fo

llow

ed b

y:...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...45

00–P

B,5

......

......

......

......

......

.....

......

......

......

......

......

......

......

973.

55A

scor

bic

acid

red

uctio

n, M

anua

l, or

......

......

......

......

......

......

......

365.

315

4500

–P E

D51

5–88

(A)

......

......

......

......

......

......

......

...A

utom

ated

......

......

......

......

......

......

......

......

......

......

......

......

......

...36

5.1

4500

–P F

......

......

......

......

......

..I–

4600

–85

......

......

......

......

..97

3.56

Sem

i-aut

omat

ed b

lock

dig

esto

r...

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

......

..D

515–

88(B

)...

......

......

......

......

......

......

......

52.

Pla

tinum

—T

otal

4,

mg/

L;D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n, o

r...

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

3111

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 16

53.

Pot

assi

um—

Tot

al4,

mg/

L;D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n, o

r...

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

3111

B...

......

......

......

......

.....

I–36

30–8

597

3.53

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

54.

Res

idue

—T

otal

, m

g/L:

Gra

vim

etric

, 10

3–10

5°...

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...25

40 B

......

......

......

......

......

..I–

3750

–85

55.

Res

idue

—fil

tera

ble,

mg/

L;G

ravi

met

ric,

180°

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

2540

C...

......

......

......

......

.....

I–17

50–8

5


AB

LEIB

.—LI

ST

OF

AP

PR

OV

ED

INO

RG

AN

ICT

ES

TP

RO

CE

DU

RE

S—

Con

tinue

d

Par

amet

er,

Uni

ts a

nd M

etho

dE

PA

1

Ref

eren

ce (

Met

hod

No.

or

Pag

e)

Std

. M

etho

ds 1

8th

Ed.

AS

TM

US

GS

2A

OA

C-in

ter-

natio

nal3

and

othe

rs

56.

Res

idue

—no

nfilt

erab

le (

TS

S),

mg/

L:G

ravi

met

ric,

103–

105°

pos

t w

ashi

ng o

f re

sidu

e...

......

......

......

......

......

......

......

......

......

......

...25

40 D

......

......

......

......

......

..I–

3765

–85

57.

Res

idue

—se

ttlea

ble,

mg/

L:V

olum

etric

(Im

hoff

cone

), o

r G

ravi

met

ric...

......

......

......

......

......

......

.....

......

......

......

......

......

...25

40 F

......

......

......

......

......

.....

......

......

......

......

......

......

......

58.

Res

idue

—V

olat

ile,

mg/

L:G

ravi

met

ric,

550°

C...

......

......

......

......

......

......

......

......

......

......

......

.....

160.

415

......

......

......

......

......

.....

......

......

......

......

.....

I–37

53–8

559

. R

hodi

um—

Tot

al4,

mg/

L:D

iges

tion5

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

60.

Rut

heni

um—

Tot

al4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...61

. S

elen

ium

—T

otal

4,

mg/

L:D

iges

tion5

,6fo

llow

ed b

y:A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

200.

931

13 B

D38

59–9

3(B

)...

......

......

......

......

......

......

......

AA

gas

eous

hyd

ride

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

3114

B38

59–9

3(A

)I–

3667

–85

ICP

/AE

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

ICP

/MS

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

62.

Sili

ca8

Dis

solv

ed,

mg/

L:0.

45 m

icro

n fil

trat

ion

follo

wed

by:

Col

orim

etric

, M

anua

l, or

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

4500

–Si D

D85

9–88

I–17

00–8

5A

utom

ated

(M

olyb

dosi

licat

e),

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

..I–

2700

–85

ICP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...63

. S

ilver

—T

otal

4,

mg/

L:D

iges

tion5

,14

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

or

C...

......

......

......

......

.....

......

......

......

......

......

......

......

...97

4.27

, p.

3718

AA

gra

phite

fur

nace

......

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/A

ES

......

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...IC

P/M

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

200.

8...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

993.

14D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 16

64.

Sod

ium

—T

otal

4,

mg/

L:D

iges

tion5

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 B

......

......

......

......

......

..I–

3735

–85

973.

54IC

P/A

ES

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

3120

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...D

CP

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 16

65.

Spe

cific

con

duct

ance

, m

icro

mho

s/cm

at

25°C

:W

heat

ston

e br

idge

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

2510

BD

1125

–91(

A)

I–17

80–8

597

3.40

66.

Sul

fate

(as

SO

4),

mg/

L:C

olor

imet

ric,

Aut

omat

ed (

Bar

ium

chl

oran

ilate

)...

......

......

......

......

......

375.

115

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...G

ravi

met

ric...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...45

00–S

O4¥

2C

or

D...

......

......

......

......

.....

......

......

......

......

......

......

......

...92

5.54

Tur

bidi

met

ric,

or...

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

4500

–SO

4¥

2E

D51

6–90

......

......

....

......

......

......

......

......

......

......

...Io

n C

hrom

atog

raph

y...

......

......

......

......

......

......

......

......

......

......

......

....

300.

041

10 B

D43

27–9

1...

......

......

......

......

......

......

......

993.

3067

. S

ulfid

e (a

s S

), m

g/L:

Titr

imet

ric (

iodi

ne),

or

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

4500

–S¥

2E

......

......

......

......

......

..I–

3840

–85

Col

orim

etric

(m

ethy

lene

blu

e)...

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...45

00–S

¥2

D...

......

......

......

......

.....

......

......

......

......

......

......

......

...68

. S

ulfit

e (a

s S

O3),

mg/

L:T

itrim

etric

(io

dine

-ioda

te)

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

4500

–SO

3¥

2B

......

......

......

......

......

.....

......

......

......

......

......

......

......

69.

Sur

fact

ants

, m

g/L:

Col

orim

etric

(m

ethy

lene

blu

e)...

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

...55

40 C

D23

30–8

8...

......

.....

......

......

......

......

......

......

......

...70

. T

empe

ratu

re,

°C:

53999Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed RulesT

herm

omet

ric...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...25

50 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 37

71.

Tha

llium

—T

otal

4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

B...

......

......

......

......

.....

......

......

......

......

......

......

......

...A

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

200.

9...

......

......

......

......

.....

......

......

......

......

......

.....

......

......

......

......

......

......

......

ICP

/AE

S,

or...

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

......

......

......

......

......

.....

......

......

......

......

......

......

......

ICP

/MS

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

72.

Tin

—T

otal

4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n,...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...31

11 B

AA

gra

phite

fur

nace

, or

......

......

......

......

......

......

......

......

......

......

.20

0.9

3113

B.

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

7.

73.

Tita

nium

—T

otal

4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

DIC

P/A

ES

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

.20

0.7

DC

P...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...N

ote

1674

. T

urbi

dity

, N

TU

:N

ephe

lom

etric

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

180.

121

30 B

D18

89–8

8(A

)I–

3860

–85

75.

Van

adiu

m—

Tot

al4,

mg/

L:D

iges

tion

5fo

llow

ed b

y:A

A d

irect

asp

iratio

n...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

3111

DA

A g

raph

ite f

urna

ce...

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

..D

3373

–93

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

ICP

/MS

, or

......

......

......

......

......

......

......

......

......

......

......

......

......

...20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

DC

P...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

.....

D41

90–8

2(88

)...

......

......

.....

Not

e 16

76.

Zin

c—T

otal

4,

mg/

L:D

iges

tion

5,6

follo

wed

by:

AA

dire

ct a

spira

tion

......

......

......

......

......

......

......

......

......

......

......

....

......

......

......

......

......

...31

11 (

B o

r C

)D

1691

–90

(A o

r B

)I–

3900

–85

974.

27,

p. 3

718

ICP

/AE

S...

......

......

......

......

......

......

......

......

......

......

......

......

......

....

200.

731

20 B

ICP

/MS

......

......

......

......

......

......

......

......

......

......

......

......

......

......

..20

0.8

......

......

......

......

......

.....

......

......

......

......

.....

......

......

......

......

......

......

......

...99

3.14

DC

P,

or...

......

......

......

......

......

......

......

......

......

......

......

......

......

.....

......

......

......

......

......

......

......

......

......

......

......

..D

4190

–82(

88)

......

.....

......

......

......

......

......

......

......

Not

e 16

Col

orim

etric

(zi

ncon

)...

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

......

...35

00–Z

n F

......

......

......

......

......

.....

......

......

......

......

......

......

......

Not

e 38

Tab

le I

B—

No

tes

1‘‘M

etho

ds f

or t

he D

eter

min

atio

n of

Met

als

in E

nviro

nmen

tal

Sam

ples

’’, S

uppl

emen

t I,

EM

SL–

CI,

EP

A/6

00/R

–94/

111,

May

199

4; a

nd ‘

‘Met

hods

for

the

Det

erm

inat

ion

of I

norg

anic

Sub

-st

ance

s in

Env

ironm

enta

l Sam

ples

’’, E

MS

L–C

I, E

PA

/600

/R–9

3/10

0, A

ugus

t, 19

93.

2F

ishm

an,

M.

J.,

et a

l., ‘‘

Met

hods

for

Ana

lysi

s of

Ino

rgan

ic S

ubst

ance

s in

Wat

er a

nd F

luvi

al S

edim

ents

’’, U

.S.

Dep

artm

ent

of t

he I

nter

ior,

Tec

hniq

ues

of W

ater

—R

esou

rce

Inve

stig

atio

ns o

fth

e U

.S.

Geo

logi

cal S

urve

y (U

SG

S),

Den

ver,

CO

, R

evis

ed 1

989.

3‘‘O

ffici

al M

etho

ds o

f A

naly

sis

of t

he A

ssoc

iatio

n of

Offi

cial

Ana

lytic

al C

hem

ists

’’, m

etho

ds m

anua

l, 16

th e

d (1

995)

.4

For

the

det

erm

inat

ion

of t

otal

met

als

the

sam

ple

is n

ot f

ilter

ed b

efor

e pr

oces

sing

and

a d

iges

tion

proc

edur

e is

req

uire

d a)

to

solu

biliz

e an

alyt

es i

n th

e su

spen

ded

mat

eria

l an

d b)

to

rend

er t

he a

naly

te a

vaila

ble

for

anal

ysis

whe

n co

lorim

etric

met

hods

are

use

d.5

For

non

-pla

tform

gra

phite

fur

nace

ato

mic

abs

orpt

ion

dete

rmin

atio

ns a

dig

estio

n us

ing

nitr

ic a

cid

is r

egui

red

prio

r to

ana

lysi

s. T

he p

roce

dure

use

d sh

ould

sub

ject

the

sam

ple

to g

entle

,ac

id r

eflu

xing

and

at

no t

ime

shou

ld t

he s

ampl

e be

tak

en t

o dr

ynes

s. F

or d

irect

asp

iratio

n fla

me

atom

ic a

bsor

ptio

n de

term

inat

ions

(F

LAA

) a

com

bina

tion

acid

(ni

tric

and

hyd

roch

loric

aci

ds)

dige

stio

n is

pre

ferr

ed p

rior

to a

naly

sis.

Suc

h a

dige

stio

n is

des

crib

ed a

s M

etho

d 20

0.2

in S

uppl

emen

t I

of ‘‘

Met

hods

for

the

Det

erm

inat

ion

of M

etal

s in

Env

ironm

enta

l Sam

ples

’’ E

PA

–600

/R–

94/1

11 M

ay,

1994

. H

owev

er,

whe

n us

ing

the

gase

ous

hydr

ide

tech

niqu

e or

for

the

det

erm

inat

ion

of c

erta

in e

lem

ents

suc

h as

ant

imon

y, a

rsen

ic,

sele

nium

, si

lver

, an

d tin

by

non-

EP

A g

raph

-ite

fur

nace

ato

mic

abs

orpt

ion

met

hods

, m

ercu

ry b

y co

ld v

apor

ato

mic

abs

orpt

ion,

the

nob

le m

etal

s an

d tit

aniu

m b

y F

LAA

, a

spec

ific

or m

odifi

ed s

ampl

e di

gest

ion

proc

edur

e m

ay b

e re

quire

dan

d in

all

case

s th

e re

fere

nced

met

hod

writ

e-up

sho

uld

be c

onsu

lted

for

spec

ific

inst

ruct

ion

and/

or c

autio

ns.

For

ana

lyse

s us

ing

indu

ctiv

ely

coup

led

plas

ma-

atom

ic e

mis

sion

spe

ctro

met

ry(I

CP

–AE

S),

the

dire

ct c

urre

nt p

lasm

a (D

CP

) te

chni

que

or t

he E

PA

spe

ctro

chem

ical

tec

hniq

ues

(pla

tform

fur

nace

AA

, IC

P–A

ES

, an

d IC

P–M

S)

the

appr

opria

te s

ampl

e di

gest

ion

proc

edur

e to

be u

sed

is in

clud

ed in

the

ref

eren

ced

Sta

ndar

d M

etho

ds,

AS

TM

, F

ison

s, o

r E

PA

met

hods

, re

spec

tivel

y.6

The

dig

estio

n pr

oced

ure

‘‘Clo

sed

Ves

sel

Mic

row

ave

Dig

estio

n of

Was

tew

ater

Sam

ples

for

Det

erm

inat

ion

of M

etal

s’’,

CE

M C

orpo

ratio

n, P

.O.

Box

200

, M

atth

ews,

NC

281

06–0

200,

Apr

il16

, 19

92,

is a

ccep

tabl

e fo

r us

e w

ith a

ny A

A d

irect

asp

iratio

n, I

CP

/AE

S,

or D

CP

mea

sure

men

t sy

stem

list

ed f

or t

his

para

met

er.

Ava

ilabl

e fr

om t

he C

EM

Cor

pora

tion.

7M

anua

l di

still

atio

n is

not

req

uire

d if

com

para

bilit

y da

ta o

n re

pres

enta

tive

efflu

ent

sam

ples

are

on

com

pany

file

to

show

tha

t th

is p

relim

inar

y di

still

atio

n st

ep i

s no

t ne

cess

ary;

how

ever

,m

anua

l dis

tilla

tion

will

be

requ

ired

to r

esol

ve a

ny c

ontr

over

sies

.8

Whe

n de

term

inin

g bo

ron

and

silic

a, o

nly

plas

tic,

PF

TE

, or

qua

rtz

labw

are

may

be

used

fro

m s

tart

unt

il co

mpl

etio

n of

the

ana

lysi

s.9

Car

bona

ceou

s bi

oche

mic

al o

xyge

n de

man

d (C

BO

D5)

mus

t no

t be

con

fuse

d w

ith t

he t

radi

tiona

l B

OD

5te

st w

hich

mea

sure

s ‘‘t

otal

BO

D’’.

The

add

ition

of

the

nitr

ifica

tion

inhi

bito

r is

not

apr

oced

ural

opt

ion,

but

mus

t be

inc

lude

d to

rep

ort

the

CB

OD

5pa

ram

eter

. A

dis

char

ger

who

se p

erm

it re

quire

s re

port

ing

the

trad

ition

al B

OD

5m

ay n

ot u

se a

nitr

ifica

tion

inhi

bito

r in

the

pro

ce-

dure

for

rep

ortin

g th

e re

sults

. O

nly

whe

n a

disc

harg

er’s

per

mit

spec

ifica

lly s

tate

s C

BO

D5

is r

equi

red

can

the

perm

ittee

rep

ort

data

usi

ng t

he n

itrifi

catio

n in

hibi

tor.

10

The

bac

k tit

ratio

n m

etho

d w

ill b

e us

ed t

o re

solv

e co

ntro

vers

y.11

Whe

n us

ing

EP

A d

iges

tion

proc

edur

e, m

ust

use

EP

A d

eter

min

ativ

e pr

oced

ure.

Whe

n us

ing

Sta

ndar

d M

etho

ds d

iges

tion

proc

edur

e, m

ust

use

Sta

ndar

d M

etho

ds d

eter

min

ativ

e pr

oce-

dure

.12

Cop

per

sulfa

te o

r ot

her

mer

cury

-fre

e ca

taly

st s

how

n to

be

effe

ctiv

e m

ust

be u

sed

in p

lace

of

mer

curic

sul

fate

in t

he d

iges

tion

step

.

54000 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules13

Just

prio

r to

dis

tilla

tion,

adj

ust

the

sulfu

ric-a

cid-

pres

erve

d sa

mpl

e to

pH

4 w

ith 1

+ 9

NaO

H.

14

The

dig

estio

n pr

oced

ures

in t

he a

ppro

ved

Sta

ndar

d M

etho

ds d

irect

asp

iratio

n fla

me

atom

ic a

bsor

ptio

n an

d in

duct

ivel

y co

uple

d pl

asm

a-at

omic

em

issi

on s

pect

rom

etry

met

hods

are

use

ful

for

the

anal

ysis

of

silv

er u

p to

con

cent

ratio

ns o

f 1

mg/

l. H

owev

er,

whe

re s

ilver

con

cent

ratio

ns >

1 m

g/L

exis

t as

an

inor

gani

c ha

lide

the

refe

renc

ed m

etho

ds s

ampl

e pr

epar

atio

n pr

oced

ures

are

inad

equa

te.

For

sam

ple

prep

arat

ion

in t

hese

situ

atio

ns a

wel

l-mix

ed r

epre

sent

ativ

e 20

ml s

ampl

e al

iquo

t sh

ould

be

dilu

ted

to 1

00 m

L by

add

ing

40 m

L ea

ch o

f 2

M N

a 2S

2O

3an

d N

aOH

prio

r to

ana

lysi

s by

dire

ct a

spira

tion

flam

e at

omic

abs

orpt

ion.

Cal

ibra

tion

stan

dard

s sh

ould

be

prep

ared

in t

he s

ame

man

ner.

The

app

rove

d E

PA

met

hods

are

use

ful f

or t

he a

naly

sis

of s

ilver

up t

o co

ncen

trat

ions

of

0.1

mg/

L.15

‘‘Met

hods

for

Che

mic

al A

naly

sis

of W

ater

and

Was

tes’

’, U

.S.

Env

ironm

enta

l P

rote

ctio

n A

genc

y, E

nviro

nmen

tal

Mon

itorin

g S

yste

ms

Labo

rato

ry-C

inci

nnat

i (E

MS

L-C

I),

Cin

cinn

ati,

OH

,E

PA

–600

/4–7

9–02

0, R

evis

ed M

arch

198

3 an

d 19

79 w

here

app

licab

le.

16

‘‘Dire

ct C

urre

nt P

lasm

a (D

CP

) O

ptic

al E

mis

sion

Spe

ctro

met

ric M

etho

d fo

r T

race

Ele

men

tal

Ana

lysi

s of

Wat

er a

nd W

aste

s, M

etho

d A

E50

029’

’, 19

86—

Rev

ised

199

1, F

ison

Ins

trum

ents

,In

c.,

32 C

omm

erce

Cen

ter,

Che

rry

Hill

Driv

e, D

anve

rs,

MA

019

23.

17

Am

mon

ia,

Aut

omat

ed E

lect

rode

Met

hod,

Ind

ustr

ial M

etho

d N

umbe

r 37

9–75

WE

, da

ted

Feb

ruar

y 19

, 19

76,

Bra

n &

Lue

bbe

(Tec

hnic

on)

Aut

o A

naly

zer

II, B

ran

& L

uebb

e A

naly

zing

Tec

h-no

logi

es,

Inc.

, E

lmsf

ord,

NY

105

23.

18

Am

eric

an N

atio

nal S

tand

ard

on P

hoto

grap

hic

Pro

cess

ing

Effl

uent

s, A

pr.

2, 1

975.

Ava

ilabl

e fr

om A

NS

I, 14

30 B

road

way

, N

ew Y

ork,

NY

100

18.

19

‘‘Sel

ecte

d A

naly

tical

Met

hods

App

rove

d an

d C

ited

by t

he U

nite

d S

tate

s E

nviro

nmen

tal P

rote

ctio

n A

genc

y’’,

Sup

plem

ent

to t

he F

iftee

nth

Edi

tion

of S

tand

ard

Met

hods

for

the

Exa

min

atio

nof

Wat

er a

nd W

aste

wat

er (

1981

).20

OIC

Che

mic

al O

xyge

n D

eman

d M

etho

d O

cean

ogra

phy

Inte

rnat

iona

l Cor

pora

tion,

512

Wes

t Lo

op,

P.O

. B

ox 2

980,

Col

lege

Sta

tion,

TX

778

40.

21

Che

mic

al O

xyge

n D

eman

d, M

etho

d 80

00,

Hac

h H

andb

ook

of W

ater

Ana

lysi

s, 1

979,

Hac

h C

hem

ical

Com

pany

, P

.O.

Box

389

, Lo

vela

nd,

CO

805

37.

22

Orio

n R

esea

rch

Inst

ruct

ion

Man

ual,

Res

idua

l Chl

orin

e E

lect

rode

Mod

el 9

7–70

, 19

77,

Orio

n R

esea

rch

Inco

rpor

ated

, 84

0 M

emor

ial D

rive,

Cam

brid

ge,

MA

021

38.

23

‘‘Sta

ndar

d M

etho

d fo

r th

e E

xam

inat

ion

of W

ater

and

Was

tew

ater

—S

uppl

emen

t to

the

18t

h E

ditio

n’’,

1994

.24

Nat

iona

l Cou

ncil

of t

he P

aper

Ind

ustr

y fo

r A

ir an

d S

trea

m I

mpr

ovem

ent

(Inc

.),

Tec

hnic

al B

ulle

tin 2

53,

Dec

embe

r 19

71.

25

Cop

per,

Bio

cinc

honi

nate

Met

hod,

Met

hod

8506

, H

ach

Han

dboo

k of

Wat

er A

naly

sis,

197

9, H

ach

Che

mic

al C

ompa

ny,

P.O

. B

ox 3

89,

Love

land

, C

O 8

0537

.26

Hyd

roge

n io

n (p

H)

Aut

omat

ed E

lect

rode

Met

hod,

Ind

ustr

ial M

etho

d N

umbe

r 37

8–75

WA

, O

ctob

er 1

976,

Tec

hnic

on A

utoA

naly

zer

II, T

echn

icon

Ind

ustr

ial S

yste

ms,

Tar

ryto

wn,

NY

105

91.

27

Iron

, 1,

10-P

hena

nthr

olin

e M

etho

d, M

etho

d 80

08,

1980

, H

ach

Che

mic

al C

ompa

ny,

P.O

.Box

389

, Lo

vela

nd,

CO

805

37.

28

Nitr

ogen

, T

otal

Kje

ldah

l, M

etho

d P

AI–

DK

01 (

Blo

ck D

iges

tion,

Ste

am D

istil

latio

n, T

itrim

etric

Det

ectio

n),

revi

sed

12/2

2/94

, P

erst

op A

naly

tical

.29

Nitr

ogen

, T

otal

Kje

ldah

l, M

etho

d P

AI–

DK

02 (

Blo

ck D

iges

tion,

Ste

am D

istil

latio

n, C

olor

imet

ric D

etec

tion)

, re

vise

d 12

/22/

94,

Per

stop

Ana

lytic

al.

30

Nitr

ogen

, T

otal

Kje

ldah

l, M

etho

d P

AI–

DK

03 (

Blo

ck D

iges

tion,

Aut

omat

ed F

IA G

as D

iffus

ion)

, re

vise

d 12

/22/

94,

Per

stop

Ana

lytic

al.

31

Man

gane

se,

Per

ioda

te O

xida

tion

Met

hod,

Met

hod

8034

, H

ach

Han

dboo

k of

Was

tew

ater

Ana

lysi

s, 1

979,

pag

es 2

–113

and

2–1

17,

Hac

h C

hem

ical

Com

pany

, Lo

vela

nd,

CO

805

37.

32

Nitr

ogen

, N

itrite

, M

etho

d 85

07,

Hac

h C

hem

ical

Com

pany

, P

.O.

Box

389

, Lo

vela

nd,

CO

805

37.

33

Onl

y th

e tr

ichl

orot

riflu

oroe

than

e ex

trac

tion

solv

ent

optio

n is

app

rove

d.34

Wer

shaw

, R

.L.,

et a

l, ‘‘M

etho

ds f

or A

naly

sis

of O

rgan

ic S

ubst

ance

s in

Wat

er’’,

Tec

hniq

ues

of W

ater

-Res

ourc

es I

nves

tigat

ion

of t

he U

.S.

Geo

logi

cal

Sur

vey,

Boo

k 5,

Cha

pter

A3

(197

2R

evis

ed 1

987)

, p.

14.

35

The

app

rove

d m

etho

d is

cite

d in

Sta

ndar

d M

etho

ds f

or t

he E

xam

inat

ion

of W

ater

and

Was

tew

ater

, 14

th E

ditio

n. T

he c

olor

imet

ric r

eact

ion

is c

ondu

cted

at

a pH

of

10.0

±0.2

. T

he a

p-pr

oved

m

etho

ds

are

give

n on

pp

57

6–81

of

th

e 14

th

Edi

tion:

M

etho

d 51

0A

for

dist

illat

ion,

M

etho

d 51

0B

for

the

man

ual

colo

rimet

ric

proc

edur

e,

or

Met

hod

510C

fo

r th

e m

anua

lsp

ectr

opho

tom

etric

pro

cedu

re.

36

R.

F.

Add

ison

and

R.

G.

Ack

man

, ‘‘D

irect

Det

erm

inat

ion

of E

lem

enta

l Pho

spho

rus

by G

as-L

iqui

d C

hrom

atog

raph

y’’,

Jour

nal o

f C

hrom

atog

raph

y, v

ol.

47,

No.

3,

pp.

421–

426,

197

0.37

Ste

vens

, H

. H

., F

icke

, J.

F.,

and

Sm

oot,

G.

F.,

‘‘Wat

er T

empe

ratu

re—

Influ

entia

l F

acto

rs,

Fie

ld M

easu

rem

ent

and

Dat

a P

rese

ntat

ion’

’, U

.S.

Geo

logi

cal

Sur

vey,

Tec

hniq

ues

of W

ater

Re-

sour

ces

Inve

stig

atio

ns,

Boo

k 1,

Cha

pter

D1,

197

5.38

Zin

c, Z

inco

n M

etho

d, M

etho

d 80

09,

Hac

h H

andb

ook

of W

ater

Ana

lysi

s, 1

979,

pag

es 2

–231

and

2–3

33,

Hac

h C

hem

ical

Com

pany

, Lo

vela

nd,

CO

805

37.


3. Section 136.3(a) is proposed to beamended by revising entries 35–37 ofTable IC to read:

136.3 Identification of Test Procedures.

* * * * *

TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS

Parameter 1EPA Method Number 2, 7

Standard methods18th Ed. ASTM Other

GC GC/MS HPLC

* * * * * * *35. 1,2-Dichlorobenzene ........... 601,602 624, 1625 ......... — ...................... 6220 B, 6230 B.36. 1,3-Dichlorobenzene ........... 601,602 624, 1625 ......... — ...................... 6220 B, 6230 B.37. 1,4-Dichlorobenzene ........... 601,602 624, 1625 ......... — ...................... 6220 B, 6230 B.

* * * * * * *

Table 1C Notes1 All parameters are expressed in micrograms per liter (µg/L).2 The full text of Methods 601–613, 624, 625, 1624, and 1625, are given at Appendix A, ‘‘Test Procedures for Analysis of Organic Pollutants,’’

of this Part 136. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given atAppendix B, ‘‘Definition and Procedure for the Determination of the Method Detection Limit’’ of this Part 136.

* * * * * * *7 Each Analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601–

603, 624, 625, 1624, and 1625 (See Appendix A of this Part 136) in accordance with procedures in section 8.2 of each of these Methods. Addi-tionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for Methods 1624 and1625) of all samples to monitor and evaluate laboratory data quality in accordance with sections 8.3 and 8.4 of these Methods. When the recov-ery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot bereported to demonstrate regulatory compliance. Note: These warning limits are promulgated as an ‘‘interim final action with a request for com-ments.’’

* * * * * * *

4. Section 136.3(b) is proposed to beamended by revising references 1through 38 and adding references 39and 40 to read as follows:

§ 136.3 Identification of test procedures.

* * * * *(b) * * *

References, Sources, Costs, and TableCitations

(1) The full text of Methods 601–613,624, 625, 1624, and 1625 are printed inappendix A of this part 136. The fulltext for determining the methoddetection limit when using the testprocedures is given in appendix B ofthis part 136. Table IC, Note 7; andTable ID, Note 2.

(2) ‘‘Microbiological Methods forMonitoring the Environment, Water andWastes,’’ U.S. Environmental ProtectionAgency, EPA–600/8–78–017, 1978.Available from: ORD Publications, CERI,U.S. Environmental Protection Agency,Cincinnati, Ohio 45268. Table IA. Note2.

(3) ‘‘Methods for Chemical Analysis ofWater and Wastes,’’ U.S. EnvironmentalProtection Agency, EPA 600/4–79–020,March 1979, or ‘‘Methods for ChemicalAnalysis of Water and Wastes, U.S.Environmental Protection Agency, EPA–600/4–79–020, Revised March 1983.Available from: ORD Publications, CERI,U.S. Environmental Protection Agency,Cincinnati, Ohio 45268. Table IB, Note15.

(4) ‘‘Methods for Benzidine,Chlorinated Organic Compounds,Pentachlorophenol and Pesticides inWater and Wastewater,’’ U.S.Environmental Protection Agency, 1978.Available from: ORD Publications, CERI,U.S. Environmental Protection Agency,Cincinnati, Ohio 45268, Table IC, Note3; Table D, Note 3.

(5) ‘‘Prescribed Procedures forMeasurement of Radioactivity inDrinking Water,’’ U.S. EnvironmentalProtection Agency, EPA–600/4–80–032,1980. Available from: ORD Publications,CERI, U.S. Environmental ProtectionAgency, Cincinnati, Ohio 45268, TableIE, Note 1.

(6) ‘‘Standard Methods for theExamination of Water and Wastewater’’,Joint Editorial Board, American PublicHealth Association, American WaterWorks Association, and WaterEnvironment Federation, 18th Edition,1992. Available from: American PublicHealth Association, 1015 FifteenthStreet, NW., Washington, DC 20005,Cost $160.00. Table IA, IB, IC, ID and IE.

(7) (Reserved)(8) Ibid, 14th Edition, 1975. Table IB,

Note 35.(9) ‘‘Selected Analytical Methods

Approved and Cited by the UnitedStates Environmental Protection AgencySupplement to the 15th Edition ofStandard Methods for the Examinationof Water and Wastewater, 1981.Available from: American Public HealthAssociation, 1015 Fifteenth Street NW.,

Washington, DC 20036. Cost availablefrom publisher. Table IB, Note 19; TableIC, Note 6; Table ID, Note 6.

(10) ‘‘Annual Book of Standards—Water and Environmental Technology’’,Section 11, Parts 11.01 Water (I) and11.02 Water (II), American Society forTesting and Materials, 1994. 1916 RaceStreet, Philadelphia, PA 19103. Costavailable from publisher. Tables IB, IC,ID, and IE.

(11) ‘‘Methods for Collection andAnalysis of Aquatic Biological andMicrobiological Samples,’’ edited byBritton, L.J. and P.E. Greason,Techniques of Water ResourcesInvestigations, of the U.S. GeologicalSurvey, Book 5, Chapter A4 (1989).Available from: U.S. Geological Survey,Denver Federal Center, Box 25425,Denver, CO 80225. Cost: $9.25 (subjectto change). Table IA.

(12) ‘‘Methods for Determination ofInorganic Substances in Water andFluvial Sediments,’’ by M.J. Fishmanand Linda C. Friedman, Techniques ofWater-Resources Investigations of theU.S. Geological Survey, Book 5 ChapterA1 (1989). Available from: U.S.Geological Survey, Denver FederalCenter, Box 25425, Denver, CO 80225.Cost $108.75 (subject to change). TableIB, Note 2.

(13) (Reserved)(14) ‘‘Methods for the Determination

of Organic Substances in Water andFluvial Sediments, Wershaw, R.L., et al.,Techniques of Water-Resources


Investigations of the U.S. GeologicalSurvey, Book 5, Chapter A3 (1987).Available from: U.S. Geological Survey,Denver Federal Center, Box 25425. Cost:$0.90 (subject to change). Table IB, Note34, Table ID, Note 4.

(15) ‘‘Water Temperature-InfluentialFactors, Field Measurement and DataPresentation,’’ by H.H. Stevens, Jr., J.Ficke, and G.F. Smoot, Techniques ofWater Resources Investigations of theU.S. Geological Survey, Book 1, ChapterD1, 1975. Available from: U.S.Geological Survey, Denver FederalCenter, Box 25425, Denver, CO 80225,Cost: $1.60 (subject to change). Table IB,Note 37.

(16) ‘‘Selected Methods of the U.S.Geological Survey of Analysis ofWastewaters, by M.J. Fishman andEugene Brown; U.S. Geological SurveyOpen File Report 76–77 (1976).Available from: U.S. Geological Survey,Branch of Distribution, 1200 South EadsStreet, Arlington, VA 22202. Cost:$13.50 (subject to change). Table IE,Note 2.

(17) ‘‘Official Methods of Analysis ofAOAC-International’’, 16th Edition(1995). Price: $359.00. Available from:AOAC-International, 1970 Chain BridgeRd., Dept. 0742, McLean, VA 22109–0742. Table IB, Note 3.

(18) ‘‘American National Standard onPhotographic Processing Effluents,’’April 2, 1975. Available from: AmericanNational Standards Institute, 1430Broadway, New York, New York 10018.Table IB, Note 18.

(19) ‘‘An Investigation of ImprovedProcedures for Measurement of MillEffluent and Receiving Water Color,NCASI Technical Bulletin No. 253,December 1971. Available from:National Council of the Paper Industryfor Air and Stream Improvements, Inc.,260 Madison Avenue, New York, NY10016. Cost available from publisher.Table IB, Note 24.

(20) Ammonia, Automated ElectrodeMethod, Industrial Method Number379–75WE, dated February 19, 1976.Technicon Auto Analyzer II. Methodand price available from TechniconIndustrial Systems, Tarrytown, NewYork 10591. Table IB, Note 17.

(21) Chemical Oxygen Demand,Method 8000, Hach Handbook of WaterAnalysis, 1979. Method price availablefrom Hach Chemical Company, P.O. Box389, Loveland, Colorado 80537. TableIB, Note 21.

(22) OIC Chemical Oxygen DemandMethod, 1978. Method and priceavailable from OceanographyInternational Corporation, 512 WestLoop, P.O. Box 2980, College Station,Texas 77840. Table IB, Note 20.

(23) ORION Research InstructionManual, Residual Chlorine ElectrodeModel 97–70, 1977. Method and priceavailable from ORION ResearchIncorporation, 840 Memorial Drive,Cambridge, Massachusetts 02138. TableIB, Note 22.

(24) Bicinchoninate Method forCopper. Method 8506, Hach Handbookof Water Analysis, 1979. Method andprice available from Hach ChemicalCompany, P.O. Box 300, Loveland,Colorado 80537. Table IB, Note 25.

(25) Hydrogen Ion (pH) AutomatedElectrode Method, Industrial MethodNumber 378–75WA. October 1976. Bran& Luebbe (Technicon) Auto Analyzer II.Method and price available from Bran &Luebbe Analyzing Technologies, Inc.Elmsford, N.Y. 10523. Table IB, Note 26.

(26) 1,10–Phenanthroline Methodusing FerroVer Iron Reagent for Water,Hach Method 8008, 1980. Method andprice available from Hach ChemicalCompany, P.O. Box 389, Loveland,Colorado 80537. Table IB, Note 27.

(27) Periodate Oxidation Method forManganese, Method 8034, HachHandbook for Water Analysis, 1979.Method and price available from HachChemical Company, P.O. Box 389,Loveland, Colorado 80537. Table IB,Note 31.

(28) Nitrogen, Nitrite-Low Range,Diazotization Method for Water andWastewater, Hach Method 8507, 1979.Method and price available from HachChemical Company, P.O. Box 389,Loveland, Colorado 80537. Table IB,Note 32.

(29) Zincon Method for Zinc, Method8009, Hach Handbook for WaterAnalysis, 1979. Method and priceavailable from Hach ChemicalCompany, P.O. Box 389, Loveland,Colorado 80537. Table IB, Note 38.

(30) ‘‘Direct Determination ofElemental Phosphorus by Gas-LiquidChromatography,’’ by R.F. Addison andR.G. Ackman, Journal ofChromatography, Volume 47, No. 3, pp.421–426, 1970. Available in most publiclibraries. Back volumes of the Journal ofChromatography are available fromElsevier/North-Holland,Inc., JournalInformation Center, 52 VanderbiltAvenue, New York, NY 10164. Costavailable from publisher, Table IB, Note36.

(31) ‘‘Direct Current Plasma (DCP)Optical Emission Spectrometric Methodfor Trace Elemental Analysis of Waterand Wastes’’, Method AES 0029, 1986–Revised 1991. Fison Instruments, Inc.,32 Commerce Center, Cherry Hill Drive,Danvers, MA 01923. Table IB, Note 16.

(32) ‘‘Closed Vessel MicrowaveDigestion of Wastewater Samples for

Determination of Metals, CEMCorporation, P.O. Box 200, Matthews,North Carolina 28106–0200, April 16,1992. Available from the CEMCorporation. Table IB, Note 6.

(33) Reserved.(34) ‘‘Organochlorine Pesticides and

PCB’s in Wastewater Using EmporeTM

Disk’’, Test Method 3M 0222, Revised10/28/94. 3M Corporation, 3M CenterBuilding 220–9E–10, St. Paul, MN55144–1000. Method available from 3MCorporation. Tables IC and ID, Note 9.

(35) ‘‘Nitrogen, Total Kjeldahl,Method PAI-DK01 (Block Digestion,Steam Distillation, TitrimetricDetection)’’, revised 12/22/94, PerstopAnalytical. Method available fromPerstorp Analytical Corporation, P.O.Box 648, Wilsonville, OR 97070. TableIB, Note 28.

(36) ‘‘Nitrogen, Total Kjeldahl,Method PAI-DK02 (Block Digestion,Steam Distillation, ColorimetricDetection)’’, revised 12/22/94, PerstopAnalytical. Method available fromPerstorp Analytical Corporation, P.O.Box 648, Wilsonville, OR 97070. TableIB, Note 29.

(37) ‘‘Nitrogen, Total Kjeldahl,Method PAI-DK03 (Block Digestion,Automated FIA Gas Diffusion)’’, revised12/22/94, Perstop Analytical. Methodavailable from Perstorp AnalyticalCorporation, P.O. Box 648, Wilsonville,OR 97070. Table IB, Note 30.

(38) Methods for the Determination ofMetals in Environmental Samples,Environmental Monitoring SystemsLaboratory, Office of Research andDevelopment, U.S. EnvironmentalProtection Agency, Cincinnati, OH45268, EPA 600 R–94/111, May 1994.Table IB, Notes 1 and 5.

(39) ‘‘Methods for the Determinationof Inorganic Substances inEnvironmental Samples’’,Environmental Monitoring SystemsLaboratory, Office of Research andDevelopment, U.S. EnvironmentalProtection Agency, Cincinnati, OH45268, Revised EPA 600 R–93/100August 1993. Table IB, Note 1.

(40) ‘‘Standard Methods for theExamination of Water and Wastewater’’,American Public Health Association,American Water Works Association,Water Environment Federation, 18thEdition Supplement, 1994. Table IB,Note 23.

5. Section 136.3 (e) is proposed to beamended by revising Table II to read asfollows:

136.3 Identification of test procedures.

* * * * *(e) * * *


TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES

Test procedure table parameter number/name Container 1 Preservation proce-dure 2–4

Maximumholding time 5

Table IA—Biological Tests

1. Coliform (fecal) ........................................................................................................... P,G a,b 6 6 hours.2. Coliform (fecal), Pres. of chlorine ............................................................................... P,G a,b 6 6 hours.3. Coliform (total) ............................................................................................................ P,G a,b 6 6 hours.4. Coliform (total), Pres. of chlorine ................................................................................ P,G a,b 6 6 hours.5. Fecal streptococci ....................................................................................................... P,G a,b 6 6 hours.

Table IB—Inorganic Tests

1. Acidity ......................................................................................................................... P,G a 14 days.2. Alkalinity ...................................................................................................................... P,G a 14 days.3. Aluminum 7 .................................................................................................................. P,G c 6 months.4. Ammonia ..................................................................................................................... P,G a,d 28 days.5. Antimony 7 ................................................................................................................... P,G c 6 months.6. Arsenic 7 ...................................................................................................................... P,G c 6 months.7. Barium 7 ...................................................................................................................... P,G c 6 months.8. Beryllium 7 ................................................................................................................... P,G c 6 months.9. Biochemical oxygen demand (BOD) .......................................................................... P,G a 48 hours.10. Boron 7 ...................................................................................................................... P,G c 6 months.11. Bromide ..................................................................................................................... P,G e 28 days.12. Cadmium 7 ................................................................................................................ P,G c 6 months.13. Calcium 7 ................................................................................................................... P,G c 6 months.14. Carbonaceous biochemical oxygen demand (CBOD) ............................................. P,G a 48 hours.15. Chemical oxygen demand (COD) ............................................................................ P,G a,d 28 days.16. Chloride ..................................................................................................................... P,G e 28 days.17. Chlorine ..................................................................................................................... P,G e Immediate.18. Chromium VI (dissolved) .......................................................................................... P,G a 24 hours.19. Chromium 7 ............................................................................................................... P,G c 6 months.20. Cobalt 7 ..................................................................................................................... P,G c 6 months.21. Color ......................................................................................................................... P,G a 48 hours.22. Copper 7 .................................................................................................................... P,G c 6 months.23. Cyanide ..................................................................................................................... P,G a,f 6,g 14 days.824. Cyanide amenable .................................................................................................... P,G a,f 6,g 14 days.825. Fluoride ..................................................................................................................... P e 28 days.26. Gold 7 ........................................................................................................................ P,G c 6 months.27. Hardness ................................................................................................................... P,G c or d 6 months.28. Hydrogen ion (pH) .................................................................................................... P,G e Immediate.29. Iridium 7 ..................................................................................................................... P,G c 6 months.30. Iron 7 .......................................................................................................................... P,G c 6 months.31. Kjeldahl nitrogen ....................................................................................................... P,G a,d 28 days.32. Lead 7 ........................................................................................................................ P,G c 6 months.33. Magnesium 7 ............................................................................................................. P,G c 6 months.34. Manganese 7 ............................................................................................................. P,G c 6 months.35. Mercury ..................................................................................................................... P,G c 28 days.36. Molybdenum 7 ........................................................................................................... P,G c 6 months.37. Nickel 7 ...................................................................................................................... P,G c 6 months.38. Nitrate ....................................................................................................................... P,G a 48 hours.39. Nitrate-nitrite ............................................................................................................. P,G a,d 28 days.40. Nitrite ......................................................................................................................... P,G a 48 hours.41. Oil and grease .......................................................................................................... G a; d or h 28 days.42. Organic carbon ......................................................................................................... P,G a; d or h or i 28 days.43. Organic nitrogen ....................................................................................................... P,G a,d 28 days.44. Orthophosphate ........................................................................................................ P,G a,j 48 hours.45. Osmium 7 .................................................................................................................. P,G c 6 months.46. Oxygen, dissolved:

By probe .................................................................................................................. G e Immediate.By winkler ................................................................................................................ G bottle and top k 8 hours. 4

47. Palladium 7 ................................................................................................................ P,G c 6 months.48. (Reserved) ................................................................................................................49. Phenols ..................................................................................................................... G a,d 28 days.50. Phosphorus (elemental) ............................................................................................ G a 48 hours.51. Phosphorus ............................................................................................................... P,G a,d 28 days.52. Platinum 7 .................................................................................................................. P,G c 6 months.53. Potassium 7 ............................................................................................................... P,G c 6 months.54. Residue, total ............................................................................................................ P,G a 7 days.55. Residue, filterable ..................................................................................................... P,G a 7 days.56. Residue, nonfilterable (TSS) .................................................................................... P,G a 7 days.57. Residue, settleable ................................................................................................... P,G a 48 hours.58. Residue, Volatile ....................................................................................................... P,G a 7 days.


TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued



59. Rhodium 7 ................................................................................................................. P,G c 6 months.60. Ruthenium 7 .............................................................................................................. P,G c 6 months.61. Selenium 7 ................................................................................................................. P,G c 6 months.62. Silica 7 ....................................................................................................................... P a 28 days.63. Silver 7 ....................................................................................................................... P,G c 6 months.64. Sodium 7 .................................................................................................................... P,G c 6 months.65. Specific conductance ................................................................................................ P,G a 28 days.66. Sulfate ....................................................................................................................... P,G a 28 days.67. Sulfide ....................................................................................................................... P,G a,l,m 7 days.68. Sulfite ........................................................................................................................ P,G e Immediate.69. Surfactants ................................................................................................................ P,G a 48 hours.70. Temperature. ............................................................................................................ P,G e Immediate.71. Thallium 7 .................................................................................................................. P,G c 6 months.72. Tin 7 ........................................................................................................................... P,G c 6 months.73. Titanium 7 .................................................................................................................. P,G c 6 months.74. Turbidity .................................................................................................................... P,G a 48 hours.75. Vanadium 7 ................................................................................................................ P,G c 6 months.76. Zinc 7 ......................................................................................................................... P,G c 6 months.

Table IC—Non-Pesticide Organic Compounds 9, 10

1. Acenaphthene ............................................................................................................. G,T a,b 6,n 7 days.11

2. Acenaphthylene .......................................................................................................... G,T a,b 6,n 7 days.11

3. Acrolein ....................................................................................................................... G,T a,o 6,p 14 days.12

4. Acrylonitrile ................................................................................................................. G,T a,o 6 14 days.5. Anthracene .................................................................................................................. G,T a,b 6,n 7 days.11

6. Benzene ...................................................................................................................... G,T a,h,o 6 14 days.7. Benzidine .................................................................................................................... G,T a,b 6, 13 7 days.14

8. Benzo(a)anthracene ................................................................................................... G,T a,b 6,n 7 days.11

9. Benzo(a)pyrene .......................................................................................................... G,T a,b 6,n 7 days.11

10. Benzo(b)fluoranthene ............................................................................................... G,T a,b 6,n 7 days.11

11. Benzo(g,h,i)perylene ................................................................................................. G,T a,b 6,n 7 days.11

12. Benzo(k)fluoranthene ................................................................................................ G,T a,b 6,n 7 days.11

13. Benzyl chloride ......................................................................................................... G,T a,o 6 14 days.14. Benzyl butyl phthalate .............................................................................................. G,T a 7 days.11

15. Bis(2-chloroethoxy) methane .................................................................................... G,T a,b 6 7 days.11

16. Bis(2-chloroethyl) ether ............................................................................................. G,T a,b 6 7 days.11

17. Bis(2-ethylhexyl) phthalate ....................................................................................... G,T a 7 days.11

18. Bromodichloromethane ............................................................................................. G,T a,o 6 14 days.19. Bromoform ................................................................................................................ G,T a,o 6 14 days.20. Bromomethane ......................................................................................................... G,T a,o 6 14 days.21. 4-Bromophenylphenyl ether ...................................................................................... G,T a,b 6 7 days.11

22. Carbon tetrachloride ................................................................................................. G,T a,o 6 14 days.23. 4-Chloro-3-methylphenol .......................................................................................... G,T a,b 6 7 days.11

24. Chlorobenzene .......................................................................................................... G,T a,o 6 14 days.25. Chloroethane ............................................................................................................ G,T a,o 6 14 days.26. 2-Chloroethylvinyl ether ............................................................................................ G,T a,o 6 14 days.27. Chloroform ................................................................................................................ G,T a,o 6 14 days.28. Chloromethane ......................................................................................................... G,T a,o 6 14 days.29. 2-Chloronaphthalene ................................................................................................ G,T a 7 days.11

30. 2-Chlorophenol ......................................................................................................... G,T a,b 6 7 days.11

31. 4-Chlorophenylphenyl ether ...................................................................................... G,T a,b 6 7 days.11

32. Chrysene ................................................................................................................... G,T a,b 6,n 7 days.11

33. Dibenzo(a,h)anthracene ........................................................................................... G,T a,b 6,n 7 days.11

34. Dibromochloromethane ............................................................................................. G,T a,o 6 14 days.35. 1,2-Dichlorobenzene ................................................................................................. G,T a,o 6 14 days.36. 1,3-Dichlorobenzene ................................................................................................. G,T a,o 6 14 days.37. 1,4-Dichlorobenzene ................................................................................................. G,T a,h,o 6 14 days.38. 3,3-Dichlorobenzidine ............................................................................................... G,T a,b 6 7 days.13

39. Dichlorodifluoromethane ........................................................................................... G,T a,o 6 14 days.40. 1,1-Dichloroethane .................................................................................................... G,T a,o 6 14 days.41. 1,2-Dichloroethane .................................................................................................... G,T a,o 6 14 days.42. 1,1-Dichloroethene .................................................................................................... G,T a,o 6 14 days.43. trans-1,2-Dichloroethene .......................................................................................... G,T a,o 6 14 days.44. 2,4-Dichlorophenol .................................................................................................... G,T a,b 6 7 days.11

45. 1,2-Dichloropropane ................................................................................................. G,T a,o 6 14 days.46. cis-1,3-Dichloropropene ............................................................................................ G,T a,o 6 14 days.47. trans-1,3-Dichloropropene ........................................................................................ G,T a,o 6 14 days.48. Diethyl phthalate ....................................................................................................... G,T a 7 days.11

49. 2,4-Dimethylphenol ................................................................................................... G,T a,b 6 7 days.11

50. Dimethyl phthalate .................................................................................................... G,T a 7 days.11


TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued



51. Di-n-butyl phthalate ................................................................................................... G,T a 7 days.11

52. Di-n-octyl phthalate ................................................................................................... G,T a 7 days.11

53. 2,4-Dinitrophenol ....................................................................................................... G,T a,b 6 7 days.11

54. 2,4-Dinitrotoluene ...................................................................................................... G,T a,b 6,n 7 days.11

55. 2,6-Dinitrotoluene ...................................................................................................... G,T a,b 6,n 7 days.11

56. Epichlorohydrin ......................................................................................................... G,T a,o 6 14 days.57. Ethylbenzene ............................................................................................................ G,T a,h,o 6 14 days.58. Fluoranthene ............................................................................................................. G,T a,b 6,n 7 days.11

59. Fluorene .................................................................................................................... G,T a,b 6,n 7 days.11

60. Hexachlorobenzene .................................................................................................. G,T a 7 days.11

61. Hexachlorobutadiene ................................................................................................ G,T a 7 days.11

62. Hexachlorocyclopentadiene ...................................................................................... G,T a,b 6 7 days.11

63. Hexachloroethane ..................................................................................................... G,T a,b 6 7 days.11

64. Ideno(1,2,3-cd)pyrene ............................................................................................... G,T a,b 6,n 7 days.11

65. Isophorone ................................................................................................................ G,T a,b 6,n 7 days.11

66. Methylene chloride .................................................................................................... G,T a,o 6 14 days.67. 2-Methyl-4,6-dinitrophenol ........................................................................................ G,T a,b 6 7 days,11

68. Naphthalene .............................................................................................................. G,T a,b 6,n 7 days.11

69. Nitrobenzene ............................................................................................................. G,T a,b 6,n 7 days.11

70. 2-Nitrophenol ............................................................................................................ G,T a,b 6 7 days.11

71. 4-Nitrophenol ............................................................................................................ G,T a,b 6 7 days.11

72. N-Nitrosodimethylamine ............................................................................................ G,T a,b 6,n 7 days.11

73. N-Nitrosodi-n-propylamine ........................................................................................ G,T a,b 6,n 7 days.11

74. N-Nitrosodiphenylamine ............................................................................................ G,T a,b 6,n 15 7 days.11

75. 2,2-Oxybis(1-chloropropane) .................................................................................... G,T a,b 6 7 days.11

76. PCB–1016 ................................................................................................................. G,T a,b 6 7 days.11

77. PCB–1221 ................................................................................................................. G,T a,b 6 7 days.11

78. PCB–1232 ................................................................................................................. G,T a,b 6 7 days.11

79. PCB–1242 ................................................................................................................. G,T a,b 6 7 days.11

80. PCB–1248 ................................................................................................................. G,T a,b 6 7 days.11

81. PCB–1254 ................................................................................................................. G,T a,b 6 7 days.11

82. PCB–1260 ................................................................................................................. G,T a,b 6 7 days.11

83. Pentachlorophenol .................................................................................................... G,T a,b 6 7 days.11

84. Phenanthrene ........................................................................................................... G,T a,b 6,n 7 days.11

85. Phenol ....................................................................................................................... G,T a,b 6 7 days.11

86. Pyrene ....................................................................................................................... G,T a,b 6,n 7 days.11

87. 2,3,7,8-Tetrachlorodibenzo-p-dioxin ......................................................................... G,T a,b 6 7 days.11

88. 1,1,2,2-Tetrachloroethane ......................................................................................... G,T a,o 6 14 days.89. Tetrachloroethene ..................................................................................................... G,T a,o 6 14 days.90. Toluene ..................................................................................................................... G,T a,h,o 6 14 days.91. 1,2,4-Trichlorobenzene ............................................................................................. G,T a,o 6 14 days.92. 1,1,1-Trichloroethane ................................................................................................ G,T a,o 6 14 days.93. 1,1,2-Trichloroethane ................................................................................................ G,T a,o 6 14 days.94. Trichloroethene ......................................................................................................... G,T a,o 6 14 days.95. Trichlorofluoromethane ............................................................................................. G,T a,o 6 14 days.96. 2,4,6-Trichlorophenol ................................................................................................ G,T a,b 6 7 days.11

97. Vinyl chloride ............................................................................................................ G,T a,o 6 14 days.

Table ID—Pesticides 9, 10

1–70. Pesticides .............................................................................................................. G,T a,q 16 7 days.11

Table IE—Radiologic Tests

1–5. Alpha, beta and radium .......................................................................................... P,G c 6 months.

Table II Notes1 Container abbreviations: P = Polyethylene, G = Glass and T = PTFE-lined cap or septum.2 Sample preservation should be performed immediately upon sample collection. For composite chemical samples each aliquot should be pre-

served at the time of collection. When use of an automated sampler makes it impossible to preserve each aliquot, then chemical samples maybe preserved by maintaining at 4°C until compositing and sample splitting is completed.

3 Procedure abbreviations:a: Cool 4°Cb: 0.008% Na2S2O3

6

c: HNO3 to pH<2d: H2SO4 to pH<2e: None requiredf: 0.6 g ascorbic acid 6

g: NaOH to pH>12h: HCl to pH<2i: H3PO4 to pH <2j: Filter immediately


k: Fix on site and store in darkl: Add zinc acetatem: NaOH to pH>9n: Store in darko: 0.025 g ascorbic acid 6

p: Adjust pH to 4–5 10

q: Adjust pH to 5–94 When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply with the Department of Trans-

portation Hazardous Materials Regulations (49 CFR part 172). The person offering such material for transportation is responsible for ensuringsuch compliance. For the preservation requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Departmentof Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) inwater solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HNO3) in water solutions at concentrationsof 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pHabout 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less).

5 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held beforeanalysis and still be considered valid. Samples may be held for longer periods only if the permittee, or monitoring laboratory, has data on file toshow that for the specific types of samples under study, the analytes are stable for the longer time, and has received a variance from the Re-gional Administrator under § 136.3(e). Some samples may not be stable for the maximum time period given in the table. A permittee, or monitor-ing laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability.See § 136.3(e) for details. The term ‘‘analyze immediately’’ usually means within 15 minutes or less of sample collection.

6 Should only be used in the presence of residual chlorine.7 Samples should be filtered immediately on-site before adding preservative for dissolved metals.8 Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead acetate paper before pH adjust-

ments in order to determine if sulfide is present. If sulfide is present, it can be removed by the addition of cadmium nitrate powder until a nega-tive spot test is obtained. The sample is filtered and then NaOH is added to pH 12.

9 Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.10 When samples are to be extracted and analyzed for multiple analytes, the most stringent preservation procedures and shortest maximum

holding times should be observed for optimum safeguard of sample integrity. Samples extracted for a wide range of analytes may be preservedby cooling to 4°C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6–9; samples preservedin this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and hold-ing time procedure are noted in footnotes 6,13, and 14.

11 Samples must be extracted within seven days of collection. The extract must be analyzed within 40 days of extraction.12 Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling.13 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0± 0.2 to prevent rearrangement to benzidine.14 Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free) atmosphere.15 Adjust pH to 7–10 with NaOH within 24 hours of sampling.16 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of col-

lection. For the analysis of aldrin, add 0.008% N2S2O3.

Appendices C and D—[Removed]

6. In Part 136, Appendices C and Dare proposed to be removed.

[FR Doc. 95–25775 Filed 10–17–95; 8:45 am]BILLING CODE 6560–50–P

53988 federal register /vol. 60, no. 201/wednesday ... federal register/vol. 60, no. 201/wednesday,...

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