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《化学分析计量》 2019年第05期
DOI:10.3969/j.issn.1008-6145.2019.05.013
气相色谱法测定丁二烯中微量乙腈、4-乙烯基环己烯、甲苯、叔丁基邻苯二酚
许秋燕,朱淑军,张春峰,丁宁
淄博齐翔腾达化工股份有限公司,山东淄博 255400 
Determination of acetonitrile, 4-vinyl cyclohexene, toluene and tert-butyl catechol in butadiene by gas chromatography
XU Qiuyan, ZHU Shujun, ZHANG Chunfeng, DING Ning
Zibo Qixiangtengda Chemical Co., LTD., Zibo 255400, China 
摘要:建立毛细管柱气相色谱法测定工业丁二烯中微量杂质抽提剂乙腈、4-乙烯基环己烯、甲苯、阻聚剂叔丁基邻苯二酚的方法。将丁二烯样品采集到钢瓶中,调节钢瓶压力在0.5~1.5 MPa下进样,采用Aglient HP-1柱(50 m ×0.25 mm,0.50 μm)为分离色谱柱,气相色谱法测定。乙腈、4-乙烯基环己烯、甲苯、叔丁基邻苯二酚的含量分别在1~200,1~1 000,1~200,2~300 mg/kg 范围内与色谱峰面积呈良好的线性关系,线性相关系数均大于0.999,检出限分别为0.4,0.5,0.2,1.0 mg/kg。测定结果的相对标准偏差为0.69%~1.74%(n=6),加标回收率为97.5%~105.0%。该方法准确快速,检出限低,具有良好的精密度,适合于工业丁二烯中微量杂质乙腈、4-乙烯基环己烯、甲苯、叔丁基邻苯二酚的测定。 
Abstract:A method for determining trace acetonitrile, 4-vinyl cyclohexene, toluene and tert-butyl catechol in industrial butadiene by capillary column gas chromatography was established. Samples of butadiene were collected in a steel cylinder, and samples were injected in the pressure range of 0.5-1.5 MPa. Aglient HP-1 column (50 m×0.25 mm, 0.50 μm) was used as the separation column, and determined by gas chromatography. The contents of acetonitrile, 4-vinyl cyclohexene, toluene and tert-butyl catechol had good linear relationship with the chromatographic peak area in the range of 1-200, 1-1 000, 1-200, 2-300 mg/kg, respectively, the linear correlation coefficients were more than 0.999, and the detection limits of acetonitrile, 4-vinyl cyclohexene, toluene and tert-butyl catechol were 0.4, 0.5, 0.2, 1.0 mg/kg, respectively. The relative standard deviation of determination results was 0.69%-1.74%(n=6), and the recovery was 97.5%-105.0%. The method is accurate, rapid with low detection limit and good precision, which is suitable for determination of acetonitrile, 4-vinyl cyclohexene, toluene and tert-butyl catechol in industrial butadiene. 
关键词:气相色谱法;丁二烯;乙腈;4-乙烯基环己烯;甲苯;叔丁基邻苯二酚 
Keywords:gas chromatography; butadiene; acetonitrile; 4-vinyl cyclohexene; toluene; tert-butyl catechol 
本文引用格式:
许秋燕,朱淑军,张春峰,等.气相色谱法测定丁二烯中微量乙腈、4-乙烯基环己烯、甲苯、叔丁基邻苯二酚[J].化学分析计量,2019,28(5):53-56. XU Q Y,ZHU S J,ZHANG C F,et al. Determination of acetonitrile,4-vinyl cyclohexene,toluene and tert-butyl catechol in butadiene by gas chromatography[J]. Chemical analysis and meterage,2019,28(5):53-56. 

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