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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
53990 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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
53991Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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
53992 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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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D14
26–9
3(A
)I–
3520
–85
......
......
......
......
..97
3.49
Titr
atio
n...
......
......
......
......
......
......
......
......
......
......
......
......
......
.....
......
......
......
......
......
......
4500
–NH
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.
53996 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
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
53998 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
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
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.
54001Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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
54002 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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) * * *
54003Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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.
54004 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued
Test procedure table parameter number/name Container 1 Preservation proce-dure 2–4
Maximumholding time 5
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
54005Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued
Test procedure table parameter number/name Container 1 Preservation proce-dure 2–4
Maximumholding time 5
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
54006 Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / Proposed Rules
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