Designation:D3447–00aAnAmericanNationalStandardStandardTestMethodforPurityofHalogenatedOrganicSolvents1ThisstandardisissuedunderthefixeddesignationD3447;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(e)indicatesaneditorialchangesincethelastrevisionorreapproval.ThisstandardhasbeenapprovedforusebyagenciesoftheDepartmentofDefense.1.Scope1.1Thistestmethodcoversthedeterminationofcommonimpuritiesfoundinhalogenatedorganicsolventsintroducedduringthemanufacturingofthesolvent.Althoughtheabsolutesensitivitymayvary,sensitivityinthepartspermillionrangemaybeachievedunderthechromatographicconditionsspeci-fiedinthistestmethod.1.2Thisstandarddoesnotpurporttoaddressallofthesafetyconcerns,ifany,associatedwithitsuse.Itistheresponsibilityoftheuserofthisstandardtoestablishappro-priatesafetyandhealthpracticesanddeterminetheapplica-bilityofregulatorylimitationspriortouse.2.SummaryofTestMethod2.1Thistestmethodisbasedonatemperature-programmedgaschromatographicseparationachievedonapackedcolumncontaining30%byweightsiliconeoilon80/100meshdiatomaceousearth.23.SignificanceandUse3.1Thistestmethodcanbeusedtocheckthepurityofhalogenatedorganicsolventsbydeterminingtheimpuritiespresentunderthechromatographicconditionsspecified.3.2Thistestcanbeusedforestablishingmanufacturingandpurchasingspecifications.4.Apparatus4.1GasChromatograph,equippedwitha1-mvrecorderorelectronicintegratorandathermalconductivityorflameionizationdetector.4.2Column,6-mby3.2-mmoutsidediameterstainlesssteeltubingpackedwith30%byweightsiliconefluid2on80/100meshdiatomaceousearthorsimilarcapillary.34.3Syringe,10-µLgaschromatographic.4.4FlowMeter,soap-bubbletypeorequivalent.4.5Helium,researchgradecarriergas.5.Procedure5.1Installthecolumnandadjusttheheliumcarriergasflowto40mL/min.5.2Setupthegaschromatographaccordingtotheparam-eterslistedasfollows:Injectionporttemperature:200°CDetectortemp...
