摘要
以聚甲基硅橡胶毛细管柱为色谱柱 ,乙醇为溶剂 ,氢火焰离子检测器检测 ,分别对工业三乙醇胺中一乙醇胺、二乙醇胺、三乙醇胺进行分离 ,进而测出其含量。并对色谱柱、载气流速、柱温溶剂、进样量等色谱条件的选择 ,以及试样与溶剂的体积比的选择进行了实验。利用保留时间定性 ,对归一化法、内标法、外标法进行了对比实验 ,结果归一化法快速可行。在选定的最佳色谱条件下 ,三乙醇胺样品回收率的测定结果在 98.72 %~ 1 0 3.2 %之间。精密度为 CV=0 .40 3%。对实际样品测试结果 ,色谱法相对标准偏差 CV=0 .1 35% ,化学法相对标准偏差 CV=1 .81 % ,而色谱法不用对分析样品处理 ,操作简单、快速 ,便于工业实际生产监测。
The aminoethyl alcohol,diethanolamine,triethanolamine were separated from industrial triethanolamine and determinated the content by using hydrogen flame ionization detector,polymethylated silastic capillary column as chromatographic column and alcohol as solvent.The selection of chromatographic column,flow rate of carrier gas,column temperature,solvent,sample size and the column ratio of sample and solvent were experimented.It has made a contrastive experiment with normalization method,internal standard method and external standard method using retention time to qualitative test.The result showed that normalization method was rapid.On the best chromatographic condition,the recovery of triethanolamine sample was 98.72%~103.2%,precision was 0.403%.The actual sample test showed that chromatography was 0.135% without disposal.
出处
《广西化工》
2000年第1期39-41,54,共4页
Guangxi Chemical Industry
关键词
气相色谱法
三乙醇胺
分离
毛细管柱
gas chromatography
triethanolamine
separation
capillary column
determination