用高压液体进样-气相色谱法测定1,3-丁二烯中的二聚物及残留抽提剂  

Determination of dimer and residual extractant in 1,3-butadiene by high pressure liquid injection-gas chromatography

作　　者：陈菲 史得军 薛慧峰 钟鸣 王春燕 曹青 赫丽娜 CHEN Fei;SHI De-jun;XUE Hui-feng;ZHONG Ming;WANG Chun-yan;CAO Qing;HE Li-na(Petrochemical Research Institute,PetroChina,Beijing 102206,China;Shanghai Research Institute of Petrochemical Technology,SINOPEC,Shanghai 201208,China)

机构地区：[1]中国石油石油化工研究院,北京102206 [2]中国石化上海石油化工研究院,上海201208

出　　处：《合成橡胶工业》2021年第4期253-258,共6页China Synthetic Rubber Industry

摘　　要：将使用高压液体进样阀进样与气相色谱相结合,建立了1,3-丁二烯中微量二聚物4-乙烯基环己烯及残留抽提剂乙腈、N,N-二甲基甲酰胺和N-甲基吡咯烷酮的定性定量分析方法。通过优选色谱柱及色谱分析条件确定了最佳的色谱操作方式,并对1,3-丁二烯实际样品进行了分析。结果表明,所建方法目标待测物的回收率在90.7%~109.9%之间,6次重复性的相对标准偏差均小于5.0%,最低检出限均小于1 mg/kg。该方法具有较好的准确性及重复性,可实现对工业用1,3-丁二烯中微量二聚物及残留抽提剂的质量监控。A method for the qualitative and quantitative analysis of typical dimer 4-vinylcyclohexene and residual extractants,acetonitrile,N,N-dimethylformamide and N-methylpyrrolidone in 1,3-butadiene was established by combining high pressure liquid injection valve and gas chromatography.The optimal chromatographic operation mode was determined by optimizing the chromatographic co-lumn and chromatographic analysis conditions,and the actual sample of 1,3-butadiene was analyzed.The results showed that the recovery rate of the target analytes ranged from 90.7%to 109.9%,the relative standard deviations of six repetitions were all less than 5.0%,and the minimum detection limit was less than 1 mg/kg.The method had good accuracy and repeatability and could realize the quality control of trace dimer and residual extractant in 1,3-butadiene for industrial use.

关 键 词：1 3-丁二烯 气相色谱 高压液体进样阀 二聚物 抽提剂 

分 类 号：TQ221.22+3[化学工程—有机化工]