2023年全國碩士研究生考試考研英語一試題真題（含答案詳解+作文范文）_第1頁
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1、CDROM83311Revision0September1994METHOD8331TETRAZENEBYREVERSEPHASEHIGHPERFMANCELIQUIDCHROMATOGRAPHY(HPLC)1.0SCOPEAPPLICATION1.1Thismethodisintendedftheanalysisoftetrazeneanexplosiveresidueinsoilwater.Thismethodislimitedto

2、usebyanalystsexperiencedinhlinganalyzingexplosivematerials.Thefollowingcompoundscanbedeterminedbythismethod:___________________________________________________________________________CompoundCASNoa_______________________

3、____________________________________________________Tetrazene31330639___________________________________________________________________________ChemicalAbstractsServiceRegistrynumbera1.2Tetrazenedegradesrapidlyinwatermet

4、hanolatroomtemperature.Specialcaremustbetakentorefrigeratecoolallsolutionsthroughouttheanalyticalprocess.1.3Tetrazeneinitsdryfmisextremelyexplosive.Cautionmustbetakenduringpreparationofstards.1.4Theestimatedquantitationl

5、imit(EQL)ofMethod8331fdeterminingtheconcentrationoftetrazeneisapproximately7gLinwaterapproximately1mgkginsoil.1.5ThismethodisrestrictedtousebyunderthesupervisionofanalystsexperiencedintheuseofHPLCskilledintheinterpretati

6、onofchromatogramsexperiencedinhlingexplosivematerials.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.2.0SUMMARYOFMETHOD2.1A10mLwatersampleisfilteredelutedonaC18columnusingionpairingreversep

7、haseHPLCquantitatedat280nm.2.22gofsoilareextractedwith55:45vvmethanolwater1decanesulfonicacidonaplatfmshakerfilteredelutedonaC18columnusingionpairingreversephaseHPLCquantitatedat280nm.CDROM83313Revision0September19944.4P

8、reparation4.4.1PrepareallmaterialsasdescribedinChapter4fvolatileganics.5.0REAGENTS5.1HPLCgradechemicalsshallbeusedinalltests.ItisintendedthatallreagentsshallconfmtothespecificationsoftheCommitteeonAnalyticalReagentsofthe

9、AmericanChemicalSocietywheresuchspecificationsareavailable.Othergradesmaybeusedprovideditisfirstertainedthatthereagentisofsufficientlyhighpuritytopermititsusewithoutloweringtheaccuracyofthedetermination.5.2General5.2.1Me

10、thanolCHOHHPLCgrade.35.2.2ganicfreereagentwaterAllreferencestowaterinthismethodrefertoganicfreereagentwaterasdefinedinChapterOne.5.2.31DecanesulfonicacidsodiumsaltCHSONaHPLCgrade.102135.2.4Aceticacid(glacial)CHCOOHreagen

11、tgrade.35.3StardSolutions5.3.1TetrazeneStardAnalyticalReferenceMaterial.5.3.2StockstardsolutionDrytetrazenetoconstantweightinavacuumdesiccatinthedark.(Tetrazeneisextremelyexplosiveinthedrystate.Donotdrymereagentthanisnec

12、essarytopreparestocksolutions.)Placeabout0.0010g(weighedto0.0001g)intoa100mlvolumetricflaskdilutetovolumewithmethanol.Invertflaskseveraltimesuntiltetrazeneisdissolved.Steinfreezerat10EC.Stocksolutionisabout100mgL.Replace

13、stockstardsolutioneveryweek.5.3.3Intermediatestardsolutions5.3.3.1Preparea4mgLstardbydilutingthestocksolution125vvwithmethanol.5.3.3.2Pipet0.51.02.05.010.020.0mLofthe4mgLstardsolutioninto6separate100mLvolumetricflasksmak

14、euptovolumewithmethanol.Pipet25.0mLofthe4mgLstardsolutionintoa50mLvolumetricflaskmakeuptovolumewithmethanol.Thisresultsinintermediatestardsofabout0.020.040.080.20.40.824mgL.5.3.3.3Coolimmediatelyonpreparationinrefrigerat

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