GC Analysis of the Reaction Solution of Preparation of Ethylene Diamine by Reductive Amination of Ethanolamine
摘 要
采用气相色谱法测定乙醇胺还原氨化制乙二胺反应液中乙醇胺、乙二胺、哌嗪及二乙烯三胺的含量。选择手性色谱柱,程序升温及乙二醇内标物作为色谱条件,在此条件下各种物质能很好地分离,该方法的检出限(3S/N)为0.05~0.38 mg·L-1,在3个浓度水平上加入标准溶液作回收试验,测得回收率为86.4%~115.5%,相对标准偏差(n=5)为0.55%~0.83%。
Abstract
Five compounds, i.e., ethanolamine, ethylenediamine, aminoethylpiperazine, piperazine and diethylenetriamine, in the reaction solution of preparation of ethylene diamine by reductive amination of ethanolamine, were determined by gas chromatography, with chiral capillary column. Gradient elevation of column temperature and using of ethylene glycol as internal standard were adopted in the analysis. Clear separation of the compound was attained under the optimized condition. Detection limits (3S/N) of the method were found in the range of 0.05-0.38 mg·L-1. Recovery was tested by addition of mixed standard at 3 concentration levels, the results of recovery and RSD′s (n=5) found were in the ranges of 86.4%-115.5% and 0.55%-0.83% respectively.
中图分类号 O657.7
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基金项目 广西自然科学基金资助项目(桂科自0832192)
收稿日期 2010/4/25
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备注孙果宋(1954-),男,广西横县人,教授级高级工程师,硕士研究生导师,研究方向有机合成及不对称分子催化。
引用该论文: SUN Guo-song,WEI Zhi-ming,LEI Chao-kuai,LI Hua-feng. GC Analysis of the Reaction Solution of Preparation of Ethylene Diamine by Reductive Amination of Ethanolamine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(6): 711~712
孙果宋,韦志明,雷朝快,李华锋. 乙醇胺还原氨化制乙二胺反应液的气相色谱分析[J]. 理化检验-化学分册, 2011, 47(6): 711~712
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参考文献
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【2】CHU S C, TALLANT M J, YANG R S H. Quantitative determination of ethylenediamine in a laboratory rodent diet by high-performance liquid chromatography[J]. J Chromatogr, 1996,280(2):394-399.
【3】BUECHELE R C, REUTTER D J. Determination of ethylenediamine in aqueous solutions by ion chromatography[J]. Anal Chem, 1982,54(12):2113-2114.
【4】KHAMRAKULOV T K, AGASYAN P K, DZHALIOV M U. Automated continuous determination of monoethanolethylenediamine and ethylenediamine in gaseous media[J]. Zavod Lab, 1985,51(2):3-5.
【5】RUKHLYA V A, VOROB′EVA T N. Photometric determination of ethylenediamine[J]. Zavod Lab, 1991,57(10):11-12.
【6】BHATT V. Simultaneous determination of ethyleneamines ,ammoniumand sodium hydroxide in effluent water and industrial waste[J]. Afinidad, 1994,51(454):466-468.
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