桥式四氢双环戊二烯中有机杂质的色谱行为
陈智群,胡银,康莹,宁艳利,王歌阳,王民昌
西安近代化学研究所,西安 710065
Chromatographic behavior of organic impurities of endo-tetrahydrodicyclopentadiene
陈智群,胡银,康莹,宁艳利,王歌阳,王民昌
Xi'an Modern Chemistry Research Institute, Xi'an 710065, China
摘要:采用毛细管气相色谱及色谱-质谱联用法研究了由DCPD催化加氢制备桥式四氢双环戊二烯(endo-THDCPD)中有机杂质的色谱行为,确定了endo-THDCPD中有机杂质的分析条件。选用金刚烷作为内标,挂式四氢双环戊二烯(exo-THDCPD)纯度标准物质为外标对3种有机杂质进行分析,exo-THDCPD含量在0~3%范围内具有良好的线性,线性相关系数为0.9971,加标回收率为99.19%~100.85%,各组分测定结果的相对标准偏差小于1.5%(n=6)。endo-THDCPD和exo-THDCPD在EI电离作用下的四级杆质谱行为相同,因为该质谱条件下无法分辨立体异构、热稳定性差异小,可使用已知标准品的色谱保留行为进一步确证。
Abstract:The chromatographic behavior of organic impurities of endo-tetrahydrodicyclopentadienecatalytic (endo-THDCPD)prepared by catalytic hydrogenation of dicyclopentadiene (DCPD) was studied by capillary gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). The analytical condition of organic impurities of endo-THDCPD was determinated. Adamantane was used as internal standard for the analysis of three organic impurities, exo-THDCPD was as external standard. The method had good linearity in the range of 0-3% for exo-THDCPD, the linear correlation coefficients was 0.9971. The recovery was 99.19%-100.85%. The relative standard deviations for three organic impurities detetion results were less than 1.5%(n=6). MS characteristics of endo-THDCPD under electron impact ionization (EI) condition was the same as exo-THDCPD's. It can be further confirmed by GC retention time of known standard compound due to the indiscernibility of stereo isomerizaion and the small difference of thermal stability under the MS condition.
关键词:桥式四氢双环戊二烯;毛细管气相色谱法;色谱-质谱联用法
Keywords:endo-tetrahydrodicyclopentadiene; capillary gas chromatography; gas chromatography-mass spectrometry
本文引用格式:
陈智群,胡银,康莹,等.桥式四氢双环戊二烯中有机杂质的色谱行为[J].化学分析计量,2018,27(Z1):40-44.
CHEN Z Q,HU Y,KANG Y,et al. Chromatographic behavior of organic impurities of endo-tetrahydrodicyclopentadiene[J].Chemical Analysis and Meterage,2018,27(Z1):40-44.
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