气相色谱法分析1,3-丁二烯产品中的二聚物及痕量抽提剂含量

Analysis of dimer and trace extraction agent in 1,3- butadiene product by gas chromatography method

利用GC-MS确定了1,3-丁二烯中二聚物的3种存在形态,通过对色谱柱的筛选、分析条件的优化,使用高压液体进样阀与Rtx-200毛细管色谱柱,建立了测定1,3-丁二烯中3种二聚物,3种痕量抽提剂乙腈、N,N-二甲基甲酰胺、N-甲基吡咯烷酮及甲苯等组分的色谱分析方法。实验结果表明,各组分的回收率在86.9%~108.2%之间,6次重复测定的相对标准偏差均小于8.4%,3种抽提剂的检出限均小于1.0 mg/kg,所建立的方法定量结果准确可靠,数据重复性良好,满足工业上对1,3-丁二烯中二聚物和痕量抽提剂杂质的分析需求。

Three forms of dimer in 1,3-butadiene were confirmed by utilizing GC-MS.A gas chromatographic analysis method of three dimers,three trace extraction agent acetonitrile,N,N-dimethylformamide,1-methyl-2-pyrrolidinone,and toluene components in 1,3-butadiene was established via screening of the chromatography column,and optimizing operation conditions.A high-pressure liquid injection valve and an Rtx-200 capillary column were applied in the method.The experimental results show that the recovery rate of each compound is between 86.9%and 108.2%,the relative standard deviation of the six repeated measurements is less than 8.4%,and the detection limits of the three extract agents were less than 1.0 mg/kg.The analyze method provides an accurate and reliable result,and the data present excellent in precision indicating that the method can meet the industrial requirements of analyzing dimers and trace extraction agent impurities in 1,3-butadiene.