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1、Chapter4GasChromatographyGraspingthecharacteristicandtheinstrumentalcomponentsofGC(2)Understandingthetheoryofcommondetectorsandtheirapplication(3)Knowingtheoperationconditionsofmobilephase(4)Graspingthequalitativeandquantitativemethods(5)AdeepreadofadvancementofGC(GC?GC,HGC,PrGC,CGC)學(xué)時(shí)安排:3學(xué)
2、時(shí)Objectives:4.1ThePrincipleofGCMixtureswouldbesampledwithasyringe,vaporizedattheelevatedoventemperature,andwassweptalongthecolumnbythecarriergas.Asimpledetectorattheeffluentendofthecolumnproducedasignalproportionaltotheamountofanalyteineachelutingpeak.GS-GCGL-GCClassfication:Twomajortypes?G
3、as-solidchromatography(stationaryphase:solid)?Gas-liquidchromatography(stationaryphase:immobilizedliquid)PackedcolumnsOpentubularcolumn(capillarycolumns)P750-751Theadvantagesofcapillarycolumns(1)Thecapacityofthecapillaryismuchlessthanthatofthepackedcolumn.Leadingorfrontingpeaks?(2)Ionizatio
4、ndetectorsweredeveloped.(3)Injectionvolumeof0.5-2uL,andtheflowratewasslower.Splitinjection(4)LongcapillarycolumnscanbecoiledtofitinaGCoven.4.2InstrumentsforGCP753SampleInjectionSystemColumnsandColumnOvensCarrierGasSystemDetectionSystemsSchematicdiagramofagaschromatographyH2,N2或Ar氣路系統(tǒng)進(jìn)樣系統(tǒng)檢測(cè)系
5、統(tǒng)分離系統(tǒng)溫控系統(tǒng)4.2.1AppearanceoftheInjectionSystemP753Syringe:5-25?LVaporation(a)syringeThemostcommonwayofintroducingasampleintoaGCinstrument.(b)autosamplersMostGCinstrumentscansequentiallyanalyzeupto100ormoreliquidsampleswithoutmanualinternention.Thevialholdermovestopresenteachvialsequentiallyto
6、aGCsyringemountedinaroboticassembly.(c)Solidphasemicroexaction?Self-study!!P754(d)SplitandsplitlessinjectionsP756Splitinjection:routinemethod0.1-1%sampletocolumnremaindertowasteSplitlessinjection:allsampletocolumnbestforquantitativeanalysisonlyfortraceanalysis,low[sample](e)rotarysamplevalv
7、ewithsampleloop4.2.1CarrierGasSystemGas:N2,H2,HePurification:H2O,organiccompoundsRatecontrol:flowmeter4.2.3ColumnofGCOven4.2.4.溫度控制系統(tǒng)溫度是色譜分離條件的重要選擇參數(shù);氣化室、分離室、檢測(cè)器三部分在色譜儀操作時(shí)均需控制溫度;氣化室:保證液體試樣瞬間氣化;檢測(cè)器:保證被分離后的組分通過時(shí)不在此冷凝;分離室:準(zhǔn)確控制分離需要的溫度。當(dāng)試樣復(fù)雜時(shí),分離室溫度需要按一定程序控制溫度