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<br /> Federal Register / Vol. 45, No. 212 / Thursday, October 30, 1980 / Proposed Rulel r
<br /> I'll ql
<br /> trivalent chromium to hhis exavalent Agency,26 W"St.Clair lStreet,Cincinnati, 6.1.3 ,Pasteur pipets,Borosilicate glass t3 8
<br /> 46,19801.
<br /> O(2o 45268)For chromium um(VI):Method 8.545 in. cm
<br /> 6.2 Centrifuge:any centrifuge capable
<br /> restultt of inciium be neration
<br /> r w will
<br /> i as
<br /> n n „ c thing a tubes described n ing t e be
<br /> ed he
<br /> the s a 2 e of,
<br /> tion or a `Test Methods for the Evaluation of Solid reaching 2000 rpm and accepting the
<br /> the incinerator ash?How effective are Waste,Physical/Chemical Methods. Solid used g Y
<br /> available stack scrubbing devices in Waste Information,U.S.Environmental used.
<br /> Protection Agency,26 W.St.Clair Street, 6.3 pH Meter:a wide variety of
<br /> removing any chromium from the off- Cincinnati,Ohio 45268: instruments are commerically available and
<br /> gases? "iuitable for this work.
<br /> 2.If chromium-bearing wastes are to Appendix A-Method of Analysis for 6.4 Test Tube Mixer:any mixer capable
<br /> Hexavalent Chromium of thorough vortex is acceptable.
<br /> •' be regulated as hazardous when
<br /> g P
<br /> Incinerated or when subjected to similar Method 8.545 Hexavalent Chromium by 7.Reagents
<br /> destructive oxidation processes,what Coprecipitation With Lead Sulfate 7.1 Lead Nitrate Solution:Dissolve 33.1
<br /> should be . grams of,lead nitrate,Pb(NO.),(analytical
<br /> concentration chromium, 1.Scope and Application reagent grade),in deionized distilled water
<br /> triggerregulatory method covers the determination
<br /> and dilute to 100 till.
<br /> controls?What is the correlation to of dissolved hexavalent chromium Cqn in 7.2 ,Ammonium Sulfate Solution:Dissolve
<br /> between concentrations of total Extraction Procedure EP)extracts. 2.7 grams of ammonium sulfate,(NH.)ZSO.
<br /> chromium to a waste,and 1.2 'The method may be used to analyze (analytical reagent grade)in deionized
<br /> concentrations of hexavalent chromium samples containing more than 5µg of Cr(VI) distilled water and dilute to 100 ml.
<br /> in Incinerator emissions?Do conditions Per liter.In many cases,dilution of the 7.3. Calcium Nitrate Solution:Dissolve
<br /> of r pyrolysis affect this extract will be necessary to achieve an 11.8 grams of calcium nitrate,Ca(NN2�4Hzo
<br /> ratio?
<br /> atitl?iflcratiOn optimal concentration range for Furnace y g grade)'
<br /> ti What min gement standards
<br /> P g (analytical reagent rade m deionized
<br /> Atomic Absorptionspectrometry.The distilled water and dilute to 100 m1.1 m1.-20
<br /> g dilution of the sample extract is desirable ting Ca.
<br /> incinerating applied to facilities re 7.4 Nitric Acid,Concentrated,distilled
<br /> b pp � since it will reduce the likelihood of
<br /> in chromimum-bearing wastes interferences from sulfate and chloride tons agent grade or spectrograde quality.
<br /> during the interim status period?Are (see 4.1)which are present in many extracts 7.5 Acetic Acid,Glacial:ACS reagent
<br /> Subparts A.B.C,D.E.G.H.and O of the and to increase the reproducibility of the grade 7.5.1 Acetic Acid,10%(v/v):Dilute 10
<br /> Part 265 interim status standards method. ml glacial acetic acid to 100 ml with
<br /> 2.Summary of the Method deionized distilled water.
<br /> appropriate?
<br /> d Oct©ber 27 1980. 0'2.1 The method� based on the separation 7.6 Ammonium Hydroxide,10%(v/v):
<br /> Y concentrated ammonium
<br /> r9e
<br /> Douglas
<br /> I a in coprecipitation, ution h droxide,NH.OH(analytical reagent.grade),
<br /> Dquglas i<4.Cos41e, f aceticoacid.After s p ration the supe nae tot 100 ml with deionized distilled water.
<br /> ad chromate
<br /> tiaitralor.
<br /> It Is proposed to amend Title 40 CFR (containing Cr(III))is drawn off,the 7.7 Hydrogen Peroxide,30%:ACS reagent
<br /> part 1„as folio,„
<br /> precipitate is resolubilized in nitric acid as grade. ,
<br /> tv
<br /> trivalent chromium Cr[III)and quantified try 7.8 Potassium Dichromate Standard
<br /> 28t�
<br /> 1.In 261.24.Charnetertstte furnace atomic absorption spectrometry. Solution:Dissolve 2.8285 grams of dried
<br /> o EP 7� a and reagent
<br /> gr and Preservation potassium dichromate,deionized
<br /> distilled
<br /> laza oay Waste g the ert y 3.1 3. aro l cleaning
<br /> Handling
<br /> sample handling and nddi grade),it deionized distilled water
<br /> I ������,ame�, s � glassware cleamng proceduras spe Section 1), dilute to 1 liter.1 nil=I mg Cr(1000 mg/
<br /> same Trivalent Chromium Working Stock,
<br /> Table I as Follows Extraction
<br /> xtr a too dPred,du instead lusted for the 7u
<br /> Y.2 The �„ le to be evaluated
<br /> not 50 ml of the potassium
<br /> transported a Solution:ate standard solution(7.8)add 1 ml
<br /> omaxonaira stored at 4'C until analysis.characteristic shouldand of 0%H. o(a7)and 1 m!concentrated
<br /> .., p
<br /> ntxa+�r tion 3.3p Since stability of Cr(VI)is not HNO.(7.4)and dilute to 100 ml with g
<br /> Contarnkra+>t
<br /> tmd!iktrams completely,understood at this time,the deionized distilled,water.1 m1-0.5 m Cr(III).
<br /> w. Pet 1eo analysis should be carried out as soon as Prepare fresh monthly or as needed.
<br /> possible. 8.Calibration
<br /> • �'' 4. p g e or blank 1 At the time of anlaysis,prepare a
<br /> 0007 . ..M..-,...< 5.0„
<br /> Samples
<br /> 8.
<br /> ���NO-,
<br /> ' ink and a series of at least four calibration
<br /> 41 ern,con
<br /> s contamin above 1000 ,g/ standards from the Cr(III)working stock(7.9)
<br /> either sulfa
<br /> m
<br /> -&� - ore proceeding to that will adequately bracket the sample and
<br /> I " liter should dilutedibef„
<br /> Absorption Spectrometry) ance Atomic before d d to the b ion range of 5 standard,nd ug
<br /> 2.in Appendix II to Part 261 EP the blank and each standard,
<br /> ToxicityTest Procedure,revise 5,Instrument Parameters urn,
<br /> fluting to final volume,l m1 30%H2OZ
<br /> Analytical Procedures for analyzing 5.1 Drying Time and Temperature:30 sec (7.7),5 ml concentrated HNO.(7.4),and 1 ml
<br /> Extsal ttctrl Procell as""Y' ' Extract at 1 Cshing Time and Temperature: of prcalciumepared
<br /> nitrate solution se for each 100 ml
<br /> Catatatic Contaminantsu follows: m erature:30 sec standards ds shouldibe These calibration
<br /> Contaminants tis For r
<br /> P
<br /> tits prepared fresh wEekly,
<br /> The test methods for analyzing the extract 5:3 Atomizing Time and Temperature:10 or as needed.
<br /> c at 2700°C. 8.2 The listed instrument condition(5)
<br /> el f follows:
<br /> epic `Barium,cad i m,lead,sE'S.4 Purge Gas Atmosphere:Argon and calibration concentration range are for a
<br /> mercury,selenium,silver,endrin,lindane, 5:5 Wavelength:357.9 nm Perkin-Elmer HGA-2100 based on the use of a
<br /> methoxychlor:toxaphene.2.4-D[2,4- 5.6 Other operating parameters-should be 20 ul injection,continuous flow purge gas and
<br /> dich[oro'�?henoxyacetic acid),or 2,4,5-TP(2, set as specified by the particular instrument non-pyrolytic graphite.The use of
<br /> 4.5-trirhlorophenoxypropionic acid);"Test manufacturer. simultaneous background correction is
<br /> Methods for the Evaluation of Solid Waste, 6.Special Apparatus required for both calibration and sample
<br /> Wate Y analysis.
<br /> Protection 6.1 Glassware liter 9.Procedure
<br /> Information, capacityp Filteringask,heav 11,flit 9.1 Transfer a 50 ml portion of the filtered
<br /> Mt}4slcat U.S.tJ.3 aEn�Environmental P®t„ I "
<br /> 6.1.2 Centrifuge tubes,heavyduty, sample to a 100 ml Griffin beaker and adjust
<br /> 'Flute:.See FR Doc.80-33871 published at the end conical,graduated,glass stoppered,10 ml to a pH of 3.5±0.3 by adding dropwise
<br /> of th"s Pail IX of the Federal Reglster. capacity volumes of 10%acetic acid.Note:Care must
<br /> 1111„ ., .,. ,
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