固相萃取-气相色谱法测定合成气制烯烃产物中的含氧化合物.pdf

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1、2014‘}l1』J色谱Vo1．32N0．1INovember20l4ChineseJournalofChromatographyl280～l285技术与应用DOI：10．3724／SP．J，Il23．20l4．06043摘要：采川JC18⋯十fi_筚取技术对合成C制烯烃(SGTO)的J物进f颅处，将产物分离为禽氧化介物与炎，采H】柑色-质谱法(GC—MS)努察分离效蚪鉴定J物中的氧化介物，使EtJ焰离r化检测(FID)定计际样一}，的禽铽化介物．他川其正佝2一俐、Il构醇的响啦子作为Ⅲ碳数、雕的FID响应f优化Cl8

2、小洗脱条什．他月j怀准样品比较预处前后的‘法回收牢醇类川收率为88％～98％，州炎标准^^同收为64％～87％l197～4785mg／L范⋯内，准『1『具有较女r的线父系，卡¨父系数均人于0．99定性Jf定：l；=测定rSGTO物巾的67种铽化合物，发脱JF卡勾、I卜构2．州为SGTO产物I，的：ii要含钣化合物，¨[1If仔少他蚌构怵陔力‘法操作简、怏速、样求节小，f：能够l0min成佯1f的顾处分析果为SGTO『：艺化卉lJ、动力：深入研究提供r必要的j础数拂j关键词：川f¨萃取；C相色谱；质谱；氯焰离了化愉测；含

3、氰化物；成0烯中图分类号：0658文献标识码：A文章编号：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