EPA Method 8332 Nitroglycerine by High Performance Liquid Chromatograph

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1、METHOD8332NITROGLYCERINEBYHIGHPERFORMANCELIQUIDCHROMATOGRAPHY1.0SCOPEANDAPPLICATION1.1Method8332isusedtodeterminetheconcentrationofnitroglycerine(CASNo.55-63-0)inaqueousmatricessuchaswastewater,groundwater,andsurfacewater.Thismethodmayalsobeapplicableto

2、othermatrices.Method8332alsoprovidesaqualitativeprocedurefordeterminingthepresenceorabsenceofnitroglycerine(SeeAppendixA).1.2Thismethodisrestrictedtouseby,orunderthesupervisionof,analystsexperiencedintheuseofHPLCinstrumentationandskilledintheinterpretat

3、ionofHPLCchromatograms.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1Samplesareinjectedontoareversephasehighperformanceliquidchromatograph(HPLC)columnandthenitroglycerineconcentrationisquantitatedusin

4、gaUVdetector.3.0INTERFERENCES3.1Solvents,reagents,glasswareandothersampleprocessinghardwaremayyielddiscreteartifactsand/orelevatedbaselines,causingmisinterpretationofthechromatograms.Allofthesematerialsmustbedemonstratedtobefreefrominterferences.3.2Ifso

5、lidmatricesareextractedusinganultrasonicbathastheextractiontechnique,theperiodofextractionshouldnotexceed2hoursordegradationofnitroglycerinemayoccur.Acetonitrilemaybeusedasasolvent.4.0APPARATUSANDMATERIALS4.1HPLCsystem4.1.1HPLC(isocratic)-equippedwithap

6、ump,adirectinjectionportor20µLloopinjectoranda214nmUVdetector.4.1.2Column-WatersRadial-PakCN,10µmparticlesize(orequivalent).4.1.3Confirmationcolumns:LC-18Reverse-phaseHPLCcolumn(octadecyldimethylsilyl),250x4.6mmwitha5µmparticlesize(SupelcoInc.orequivale

7、nt)using3:2MeOH/Water@1.5mL/min.LC-CNReverse-phaseHPLCcolumn(cyanopropylmethylmethyl-silyl),250x4.6mmwitha5µmparticlesize(SupelcoInc.orequivalent)using1:1MeOH/Water@1.5mL/min.4.1.4Integrator.CD-ROM8332-1Revision0December19964.2Injectionsyringe.4.3Membra

8、nefilter-0.45µm5.0REAGENTS5.1Reagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicated,itisintendedthatallreagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchsp