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1、2014‘}l1』J色譜Vo1.32N0.1INovember20l4ChineseJournalofChromatographyl280~l285技術(shù)與應(yīng)用DOI:10.3724/SP.J,Il23.20l4.06043摘要:采川JC18?十fi_篳取技術(shù)對合成C制烯烴(SGTO)的J物進(jìn)f顱處,將產(chǎn)物分離為禽氧化介物與炎,采H】柑色-質(zhì)譜法(GC—MS)努察分離效蚪鑒定J物中的氧化介物,使EtJ焰離r化檢測(FID)定計際樣一},的禽鋱化介物.他川其正佝2一俐、Il構(gòu)醇的響啦子作為Ⅲ碳數(shù)、雕的FID響應(yīng)f優(yōu)化Cl8
2、小洗脫條什.他月j懷準(zhǔn)樣品比較預(yù)處前后的‘法回收牢醇類川收率為88%~98%,州炎標(biāo)準(zhǔn)^^同收為64%~87%l197~4785mg/L范?內(nèi),準(zhǔn)『1『具有較女r的線父系,卡¨父系數(shù)均人于0.99定性Jf定:l;=測定rSGTO物巾的67種鋱化合物,發(fā)脫JF卡勾、I卜構(gòu)2.州為SGTO產(chǎn)物I,的:ii要含鈑化合物,¨[1If仔少他蚌構(gòu)怵陔力‘法操作簡、怏速、樣求節(jié)小,f:能夠l0min成佯1f的顧處分析果為SGTO『:藝化卉lJ、動力:深入研究提供r必要的j礎(chǔ)數(shù)拂j關(guān)鍵詞:川f¨萃??;C相色譜;質(zhì)譜;氯焰離了化愉測;含
3、氰化物;成0烯中圖分類號:0658文獻(xiàn)標(biāo)識碼:A文章編號:l000·87l3(20l4)Il—l280—06Abstract:Thesyngas—to—olefin(SGTO)productsmainlyconsistofhydrocarbonsalongwithsmallamountsofoxygenatesasthebyproducts.AC18solid—phaseextraction(SPE)columnwasusedforoxygenatesenrichmentinSGTOproducts.Asthehydr
4、ophobiccompounds,thehydrocarbonshadstrongerinteractionwithaC18SPEcolumnthanoxygenates.Undertheopti—mizedelutionconditions,theoxygenateswerefirstelutedfrointheC18SPEcolunmwith60%(v/v)methanolsolution.Thefractionofoxygenateswasthenanalyzedwithgaschromatogra—phy—ma
5、ssspectrometry(GC—MS)forqualificationandgaschromatography—hydrogenflameion—izationdetection(GC—FID)forquantificati0n.TheFIDresponsefactorsof竹一alkanoland一ketonewereusedforalkanolsandketonesquantitativecalculationandthemethodrecoverieswere88%一98%and64%一87%respecti
6、vely.Intherangeofl97—4785mg/L.goodlinearrela-tionshipsoftheFIDresponseswiththecOrrespOndingmassconcentrationsofthestandardsaul—pieswereobtainedwiththelinearregressioncoeficientsgreaterthan0.99.Sixty—sevenoxygen—ateswereanalyzedqualitativelyandquantitatively.Ther
7、esultsshowedthatthefractionoftheoxygenatesmainlyconsistsofalkanolsandketones.ThetotalcontentoftheoxygenatesinSGTOproductswas6.2%.Theenrichmentmethodonlyrequiresaverysmallamountofsampleandthetotalprocesscanbecompletedwithinl0min.TheanalysisresultsofSGTOproductstu
8、diescanprovidethenecessarybasicdataforSGTOcatalystsanddynamicsstudies.Keywords:solid—phaseextraction(SPE);gaschromatography(GC);massspectrometry(MS);hydrogenflameioni