第 38 卷第 3 期Vol. 38 No. 3
2008 年 6 月Jun 2008

所属栏目:分析与测试

气相色谱同时测定环氧氯丙烷及其中间体
贾朝辉1,胡德禹1,陈默然2,孙 岗2,石 霞1,杨 松1,薛 伟1,宋宝安1 (1.贵州大学 精细化工研究开发中心 绿色农药与农业生物工程教育部重点实验室,贵州 贵阳,550025;2.贵州大学理学院,贵州 贵阳,550025)
摘 要:采用HP-INNOWax(30 m×0.32 mm,0.5 μm)毛细管柱,建立气相色谱-氢火焰离子化检测器(GC-FID)外标法,同时测定由生物柴油副产物甘油制备环氧氯丙烷反应体系中环氧氯丙烷、1,3-二氯丙醇和2,3-二氯丙醇的含量。通过对环氧氯丙烷、1,3-二氯丙醇和2,3-二氯丙醇的线性关系、精密度和回收率试验,获得了满意的结果。线性相关系数分别为环氧氯丙烷0.999 9、1,3-二氯丙醇0.999 9、2,3-二氯丙醇0.999 9;平均回收率:环氧氯丙烷99.86%、1,3-二氯丙醇98.24%、2,3-二氯丙醇102.26%。方法简便、快速、准确率高、重现性好。
关键词:气相色谱;环氧氯丙烷;1,3-二氯丙醇;2,3-二氯丙醇
中图分类号:O657.7  文献标识码:B  文章编号:1009-9212(2008)03- 0068-03
Determination of Epichlorohydrin and Its Intermediate by Gas Chromatography
IA Zhao-hui1,HU De-yu1,CHEM Mo-ran2,SUN Gang2,SHI Xia1,YANG Song1,XUE Wei1,SONG Bao-an1 (1. Center for Research and Development of Fine Chemicals,Key Laboratory of Green Pesticide and Agriculture Bioengineering,Ministry of Education,Guizhou University,Guiyang 550025,China;2. The College of Science of Guizhou University,Guiyang 550025,China)
Abstract:A gas chromatography and external standard methods was developed for detecting simultaneously epichlorohydrin and its intermediates such as 1,3-dichloro-2-propanol and 2,3-dichloro-1-propanol. Samples in the reaction system were detected by GC-FID with HP-INNOWAX(30 m×0.32 mm,0.5 μm) capillary column. The results showed that the linear correlation coefficients for epichlorohydrin,1,3-dichloro-2-propanol and 2,3-dichloro-1-propanol were 0.999 9,0.999 9 and 0.999 9. Recoveries for epichlorohydrin,1,3-dichloro-2-propanol and 2,3-dichloro-1-propanol were 99.86%,98.24% and 102.26%,respectively. The experimental results showed that this method was effective,quick,accurate and stable.
Key words:gas chromatography;epichlorohydrin;1,3-dichloro-2-propanol;2,3-dichloro-1-propanol
基金项目:贵州省重大专项项目(黔科合重大专项字[2007]6004)。
作者简介:贾朝辉(1984-),男,河北邢台人,硕士研究生,主要从事有机农药分析研究。
联 系 人:胡德禹(1965-),女,副教授,硕士生导师。研究方向:精细化工及中间体分析。
收稿日期:008-05-12