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1、METHOD3610BALUMINACLEANUP1.0SCOPEANDAPPLICATION1.1Aluminaisahighlyporousandgranularformofaluminumoxide.ItisavailableinthreepHranges(basic,neutral,andacidic)foruseinchromatographiccleanupprocedures.Itisusedtoseparateanalytesfrominterferingcompoundsofad
2、ifferentchemicalpolarity.1.2EachofthethreepHrangesofaluminahasdifferentusesanddisadvantagesasacleanupprocedure.1.2.1BasicaluminahasapHof9-10.Itisusedtoseparatebasicandneutralcompoundsthatarestabletoalkali,alcohols,hydrocarbons,steroids,alkaloids,natur
3、alpigments.Itsdisadvantagesarethatitcancausepolymerization,condensation,anddehydrationreactions,andonecannotuseacetoneorethylacetateaseluants.1.2.2NeutralaluminahasapHof6-8.Itisusedtoseparatealdehydes,ketones,quinones,esters,lactones,glycoside.Itsdisa
4、dvantageisthatisitconsiderablylessactivethanthebasicform.1.2.3AcidicaluminahasapHof4-5.Itisusedtoseparateacidicpigments(naturalandsynthetic),andstrongacids(thatotherwisechemisorbtoneutralandbasicalumina).Thismethoddoesnotaddresstheuseofacidalumina.1.3
5、Basic,neutral,andacidicaluminacanbepreparedinvariousactivitygrades(ItoV),basedontheBrockmannscalereproducedbelow.GradeIispreparedbyheatingaluminauntilnomorewaterislost(typicallyovernightat400-450EC,butothertime-temperaturerelationshipsmaybeemployed).T
6、heothergrades(II-V)arepreparedbyaddingwatertoGradeItodeactivateit.ActivitygradeIIIIIIIVVWateradded(wt.%)0361015RF(p-aminoazobenzene)0.00.130.250.450.55whereRFistheretentionfactorforp-aminoazobenzene.1.4Aluminacleanupmaybeaccomplishedusingaglasschromat
7、ographiccolumnpackedwithaluminaorusingsolid-phaseextractioncartridgescontainingalumina.1.5Thismethodincludesproceduresforcleanupofsampleextractscontainingphthalateestersandnitrosamines.SeeMethod3611,AluminaColumnCleanupofPetroleumWastes,foraluminaclea
8、nupofpetroleumwastes.1.6Thismethodisrestrictedtousebyorunderthesupervisionoftrainedanalysts.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.CD-ROM3610B-1Revision2December19962.0SUMMARYOFMETHOD2.1Thismethoddescribe
