全自动固相萃取-气相色谱-质谱联用分析测定催化裂化柴油烃类组成  

SIMULTANEOUS DETERMINATION OF HYDROCARBON TYPES OF LCO BY AUTOMATIC SOLID-PHASE EXTRACTION AND GAS CHROMATOGRAPHY-MASS SPECTROMETRY

作　　者：韩亚梅 余强 李兰婷 马宇春 Han Yamei;Yu Qiang;Li Lanting;Ma Yuchun(SINOPEC Shanghai Research Institute of Petrochemical Technology Co.,Ltd.,Shanghai 201208)

机构地区：[1]中石化(上海)石油化工研究院有限公司,上海201208

出　　处：《石油炼制与化工》2023年第7期130-136,共7页Petroleum Processing and Petrochemicals

基　　金：中国石油化工股份有限公司合同项目(418024-2)。

摘　　要：建立了全自动固相萃取-气相色谱-质谱联用分析测定催化裂化柴油(LCO)中各类烃组成的分析方法。通过全自动固相萃取进行样品的萃取分离预处理,优化了萃取溶液种类、样品处理量和固定相添加量比、洗脱萃取溶液流速和空气体积等萃取条件。结果表明:当样品处理量为0.1 mL、饱和烃组分萃取溶液为正己烷且其加入量为1.8 mL,芳烃组分萃取溶液为二氯甲烷乙醇体积比为5.0/1.5的混合溶液、且其加入量为2 mL,固相萃取柱中固定相填料量为1.65 g,洗脱萃取溶液流速为1.5 mL/min,饱和烃组分洗脱空气体积为0.6 mL、芳烃组分洗脱空气体积为18 mL时,LCO组分回收率为98.5%~100.5%,相对标准偏差(RSD)(试验次数为6)不大于7%。该方法适合对LCO进行组成分析,全自动固相萃取仪自动化程度高,提高了分析效率,在优化条件下分析结果准确、重复性好。A method for the determination of hydrocarbon types in light cycle oil(LCO)by automated solid-phase extraction(SPE)coupled with gas chromatography-mass spectrometry was developed.Samples were extracted and pretreated by automatic solid-phase extraction.The extraction conditions,such as the kind of the type of extraction solution,the ratio of sample treatment amount and fixed phase addition amount,the flow rate of elution extraction solution and the volume of air,were optimized.The results showed that when the sample treatment amount was 0.1 mL,the extraction solution of saturated hydrocarbon component was 1.8 mL n-hexane,the extraction solution of aromatic component was 2 mL mixed solution with the volume ratio of dichloromethane to ethanol of 5.0/1.5,the fixed-phase packing in the SPE column was 1.65 g,the flow rate of extraction solution was 1.5 mL min,the volume of the air eluted by the saturated hydrocarbon component was 0.6 mL,and the volume of the air eluted by the aromatic hydrocarbon component was 18 mL,the recoveries ranged from 98.5%to 100.5%with RSD(n=6)≤7%.The method was suitable for the composition analysis of LCO.The automatic solid-phase extractor was highly automatic,and the analysis efficiency was improved.Under optimized conditions,the analysis results were accurate and repeatable.

关 键 词：固相萃取 气相色谱-质谱 催化裂化柴油 饱和烃 芳烃 

分 类 号：O657.63[理学—分析化学] TE626.24[理学—化学]