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(收稿日期 :1999201204)
(本文编辑 :杨捷)
·监测与检验技术·
二硫化碳的提纯方法
张耀亭
目前空气中低沸点的有机物测定 ,大部分都采用活性炭
管采样、二硫化碳 (CS2)解吸、气相色谱
的方法。在检测
过程中 ,常用的解吸剂 CS2 中往往存有少量的苯和微量的甲
苯 ,有时因该试剂存放时间较长或因生产厂的工艺问题 ,造
成苯、甲苯的本底含量超过被测物含量 ,从而对准确定量带
来一定的干扰。现行的解决办法 : (1) 蒸溜提纯 CS2 ; (2) 不
提纯而用扣本底后再计算法。由于苯和 CS2 沸点较为接近 ,
蒸溜法一次蒸溜往往达到不到效果 ,需几次蒸溜 ,费时而且
试剂损失较大。不提纯而扣试剂本底法 ,如采集的被测物含
量低时 ,定量检测的准确度很差。
若以浓硫酸 - 聚甲醛为提取剂 ,利用苯系物在浓硫酸的
作者单位 :300011 天津市卫生防病中心中心仪器室
环境里可与聚甲醛反应 ,生成红色化合物 ,并溶于硫酸中的
原理 ,可达到从 CS2 中提取苯系物 ,纯化 CS2 的目的。
通过对提取剂浓度 (2 %、10 %) 、用量、提取次数、和提取
次数对提取效率的影响的探讨 ,
40 ml 体积分数为 10 %
的硫酸 - 聚甲醛 ,提取 20 h 以上 ,可将 CS2 中苯系物提净。
提取方法 :将 500 mlCS2 倾入大锥形分液漏斗中 ,加 40
ml 体积分数为 10 %的硫酸 - 聚甲醛提取剂 ,震摇 300 次后
放置分层 ,而后每隔 1 h 震摇 100 次 ,重复 5 次后放置过夜 ,
弃去暗紫色的硫酸 - 聚甲醛层。然后用蒸溜水洗涤提取后
的 CS2 5 次 ,过无水硫酸钠层析柱脱水 ,即可。
(收稿日期 :1999211215)
(本文编辑 :姜云)
46 中华劳动卫生职业病杂志 2000 年 2 月第 18 卷第 1 期 Chin J Ind Hyg Occup Dis ,February 2000 ,Vol. 18 ,No. 1
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