环氧氯丙烷中有机杂质组分的气相色谱法测定

介绍了在环氧氯丙烷国家标准制定过程中对环氧氯丙烷中有机杂质组分测定方法的改进。通过采用毛细管柱气相色谱法,对分离条件、毛细管柱选择等进行了试验和讨论。试验结果表明,采用毛细管柱气相色谱法,选用N2作为载气,分流比50∶1,并采用程序升温:柱初温40℃(保持5 min)→10℃/min→180℃(保持30 min)的条件下可获得更好的分离效果及准确度,该方法测得各杂质组分的相对标准偏差为0.0113%~0.0377%,回收率为93.3%~102.9%。能满足生产中质量控制和产品出厂分析的需要,保证了国家标准分析方法的先进性。

Determine of components of organic impurity in ECH by gas phase chromatography

In this article,the improvement of test method about the content of organic impurity in ECH during fixing national standard test was introduced and the separation condition and capillary column selection by using capillary column gas phase chromatography was discussed.Result showed that a better separate effect and accuracy experiment result could be obtained using capillary column gas phase chromatography in which,N2 used as carrier gas,split ratio=50∶1,temperature programing was that initial temperature of column was 40 ℃ and maintained 5 min,then warmed-up by 10 ℃/min to 180 ℃ and maintained 30 min and the relative standard deviation about the components of each impurity and recovery rate were 0.0113%～0.0377% and 93.3%～102.9% seperatively by this method.It could satisfy the requirement of quality control and production exworks analysis and ensure the advanced character of analytical method in national standards.