摘要
将毛细管气相色谱与表面发射火焰光度检测器用于甲基锗化合物的形态分析。使用柱头进样装置和ＨＰ－１毛细管，在最佳分离条件下，３种甲基锗化合物可以在７ｍｉｎ内得到基线分离。对甲基锗化合物的衍生和萃取条件进行的研究表明：使用戊基格林试剂衍生是甲基锗化合物衍生较理想的方法；而在９ｍｏｌ·Ｌ－１ＨＣｌ介质中，甲基锗化合物可被定量萃取到有机溶剂中，回收率分别为８６．６％，８７．４％和９６．２％。操作简便、仪器灵敏准确，最低检测限分别为：一甲基锗（ＭＭＧｅ），１００ｐｇ；二甲基锗（ＤＭＧｅ），７００ｐｇ和三甲基锗（ＴＭＧｅ），５０ｐｇ。
This paper describes the speciation analysis of methylgermanium compounds by capillary gas chromatography with flame photometric detector using quartz surface-induced luminescence. By using on-column injection technique and HP-1 capillary column, three methylgermanium compounds were base-line separated within 7 min under the optimized chromatographic conditions. Experiments indicated that the pentylated Grignard reaction is the best choice for the derivatization of methylgermnium compounds and, in 9 mol.L -1 HCl solution, methylgermanium can be quantitative extracted to organic phase, the recoveries for MMGe, DMGe and TMGe are 86.6%,87.4%and 96.2%, respectively. This method is simple, high sensitive and reliable. The minimum detection limits for MMGe, DMGe and TMGe are 100 pg, 70 pg and 50 pg, respectively.
出处
《抚顺石油学院学报》
1996年第3期52-56,共5页
Journal of Fushun Petroleum Institute
基金
国家自然科学基金
关键词
甲基锗
萃取
衍生
形态分析
Methylgermanium
Extraction
Derivatization
GC-FPD
