PVC中有机锡化合物的气相色谱测定

The Determination of Organotin Compounds in PVC by GC Method

本文介绍了聚氯乙烯(PVC)树脂中有机锡化合物的气相色谱(GC)分析方法。即将PVC树脂溶于四氢呋喃(THF)中,提取有机锡化合物,然后加到丙基镁溴化物(PMB)的THF溶液中,进行丙基化,反应液中残存的过量PMB,用0.5m硫酸分解,生成的四烷基锡化合物用己烷提取,过滤、脱水、浓缩,进行GC分析。利用本法有机锡化合物的检出限量(换算成氯化物)是0.1ng,处理1g树脂试样,其定量检出限量为2μg/g。测定了9种有机锡稳定剂,其添加实验的回收率为88.3～99.6%,相对标准偏差分别是2.2～6.8%。

A GC analytical methods for organotin compounds in PVC resin is introduced in this paper. The PVC resin was dissolved in tetrahydrofuran (THF), the extracted organotin compounds were extracted and then added to THF solution of propylmagnesium bromide (PMB)for alkylation. The residual PMB was decomposed by 0.5m H SO,resulted in tetralkyltin compounds,which was extracted with hexane,filtered,dehydrated,concentrated and then analyzed by GC. The examining limit of the organotin compounds by this method was 0.1ng. The examining limit of the treatment for 1g resin sample was 2g/g. The recovery of organotin compounds in 9 test was 88,3—99.6% ,RSD was 2.2—6.8%.