EPA Method 8325 Solvent Extractable Nonvolatile Compounds

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1、METHOD8325SOLVENTEXTRACTABLENONVOLATILECOMPOUNDSBYHIGHPERFORMANCELIQUIDCHROMATOGRAPHY/PARTICLEBEAM/MASSSPECTROMETRY(HPLC/PB/MS)1.0SCOPEANDAPPLICATION1.1Thismethoddescribestheuseofhighperformanceliquidchromatography(HPLC),coupledwithparticlebeam(PB)mass

2、spectrometry(MS),forthedeterminationofbenzidinesandnitrogen-containingpesticidesinwaterandwastewater.Thefollowingcompoundscanbedeterminedbythismethod:aCompoundCASNo.Benzidine92-87-5Benzoylpropethyl33878-50-1Carbaryl63-25-2o-Chlorophenylthiourea5344-82-

3、13,3'-Dichlorobenzidine91-94-13,3'-Dimethoxybenzidine119-90-43,3'-Dimethylbenzidine612-82-8Diuron330-54-1Linuron(Lorox)330-55-2Monuron150-68-5Rotenone83-79-4Siduron1982-49-6aChemicalAbstractServiceRegistryNumber1.2Themethodalsomaybeappropriatefortheana

4、lysisofbenzidinesandnitrogen-containingpesticidesinnon-aqueousmatrices.Themethodmaybeapplicabletoothercompoundsthatcanbeextractedfromasamplewithmethylenechlorideandareamenabletoseparationonareversephaseliquidchromatographycolumnandtransferabletothemass

5、spectrometerwithaparticlebeaminterface.1.3Preliminaryinvestigationindicatesthatthefollowingcompoundsalsomaybeamenabletothismethod:Aldicarbsulfone,Carbofuran,Methiocarb,Methomyl(Lannate),Mexacarbate(Zectran),andN-(1-Naphthyl)thiourea.Ethylenethioureaand

6、o-ChlorophenylthioureahavebeensuccessfullyanalyzedbyHPLC/PB/MS,buthavenotbeensuccessfullyextractedfromawatermatrix.1.4Tables4-6presentmethoddetectionlimits(MDLs)forthetargetcompounds,rangingfrom2to25µg/L.TheMDLsarecompound-andmatrix-dependent.1.5Thisme

7、thodisrestrictedtouseby,orunderthesupervisionof,analystsexperiencedintheuseofHPLCandskilledintheinterpretationofparticlebeammassspectrometry.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.CD-ROM8325-1Revision0December1996

8、2.0SUMMARYOFMETHOD2.1Thetargetcompoundsforthismethodmustbeextractedfromthesamplematrixpriortoanalysis.2.1.1Benzidinesandnitrogen-containingpesticidesareextractedfromaqueousmatricesataneutralpHwithmethylenechloride,usingaseparatoryfunnel