气相色谱法测定1,3-环己二酮合成反应液中5-氧代己酸钠含量  

Determination of sodium 5-oxo-caproate content in 1,3-cyclohexanedione synthesis reaction solution by gas chromatography

作　　者：纪晓红 王艳[1] 王瑞菲 董明燕 徐婷 岳涛 JI Xiaohong;WANG Yan;WANG Ruifei;DONG Mingyan;XU Ting;YUE Tao(Shandong Institute of Chemi Technology,Qingdao University of Science&Technology,Jinan 250014,China)

机构地区：[1]青岛科技大学山东化工研究院,济南250014

出　　处：《分析试验室》2024年第11期1626-1631,共6页Chinese Journal of Analysis Laboratory

基　　金：泰山学者建设工程项目基金(ts20130918)资助。

摘　　要：建立了气相色谱直接测定1,3-环己二酮合成反应液中5-氧代己酸钠含量的方法。样品用甲酸-N,N-二甲基乙酰胺溶液溶解,采用程序升温,在DB-FFAP(30 m×0.32 mm×0.5μm)毛细管柱上分离待测物和其它杂质组分,通过氢火焰离子化检测器(FID)检测,以二苯甲酮为内标物,内标法定量。在最佳色谱条件下,5-氧代己酸、二苯甲酮与其他相邻色谱峰之间分离度良好,具有良好的线性关系,相关系数r>0.999,加标回收率范围在97.0%~103.3%之间。本方法可用于1,3-环己二酮合成反应液以及1,3-环己二酮产品中5-氧代己酸含量的测定。A method was established for the direct determination of sodium 5-oxohexanoate in 1,3-cyclohexanedione synthesis reaction solution by gas chromatography.The sample was dissolved with formic acid-N,Ndimethylacetamide solution,and the analytes and other impurity components were separated on a DB-FFAP(30m×0.32 mm×0.5 μm) capillary column using temperature programmed method.Then the samples were detected by hydrogen flame ionization detector(FID) and quantified by internal standard method with benzophenone as the internal standard.Under the optimal chromatographic conditions,5-oxohexanoic acid,benzophenone and other adjacent chromatographic peaks were well separated with good linear relationships,the correlation coefficients(r) was above 0.999,and the recoveries were in the range of 97.0%-103.3%.The method can be used for the determination of sodium 5-oxohexanoate contents in 1,3-cyclohexanedione synthesis reaction solution and 1,3-cyclohexanedione products.

关 键 词：气相色谱 5-氧代己酸钠 1 3-环己二酮合成反应液 二苯甲酮 甲酸 

分 类 号：O656.3[理学—分析化学]