| 同系物季铵盐离子液体阳离子的离子交换色谱法分析 |
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| 基金项目:哈尔滨师范大学大学生实践创新基金项目；黑龙江省教育厅科学技术研究项目(12531192) |
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| 中文摘要:建立了离子交换色谱-直接电导检测法分离测定3种同系物季铵盐离子液体阳离子(四甲基铵、四乙基铵和四丙基铵阳离子)的方法。采用磺酸型阳离子交换色谱柱，以乙二胺-柠檬酸-乙腈为淋洗液，考察了淋洗液种类、浓度及色谱柱温度对3种阳离子保留的影响。并根据测定对象不同，调整乙二胺浓度及乙腈含量以改善分离效果。淋洗液中增加乙腈含量，可明显缩短四丙基铵阳离子的保留时间，并改善其色谱峰形。季铵阳离子同系物的保留符合碳数规律。优化的色谱条件为：流速1.0 mL/min，色谱柱温度40 ℃；以0.02 mmol/L乙二胺-0.12 mmol/L 柠檬酸(pH 4.0)为淋洗液分离测定四甲基铵；以0.2 mmol/L乙二胺-0.4 mmol/L 柠檬酸-1%乙腈(pH 4.0)为淋洗液分离测定四乙基铵和四丙基铵。所测阳离子的检出限(S/N=3) 分别为0.015，0.22，1.88 mg/L，相对标准偏差(n=5) 均小于2.3%。将方法应用于表面活性剂和实验室合成的离子液体的分析，加标回收率为99% ～104%。本方法简单、准确、可靠，具有良好的实用性。 |
| 中文关键词:季铵阳离子 离子交换色谱 电导检测 离子液体 |
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| Analysis of Homologous Quaternary Ammonium Ionic Liquid Cations by Ion-exchange Chromatography |
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| Abstract:A method of ion-exchange chromatography with direct conductivity detection to determine three homologous quaternary ammonium cations(tetramethyl-ammonium cation,tetraethyl-ammonium cation and tetrapropyl-ammonium cation) was developed Three homologous quaternary ammonium cations were separated on a sulfonic acid base cation-exchange column using ethylenediamine-citric acid-acetonitrile as eluent.Effects of eluent types,eluent concentrations and column temperatures on retention and separation of three cations were discussed.The separations of the cations were improved by changing concentration of ethylenediamine and acetonitrile in eluents.With the increase of acetonitrile concentration,the retention time of tetrapropyl ammonium cation was obviously reduced,and the chromatogrophic peaks of the cations were improved.The retentions of homologous quaternary ammonium cations accord with carbon number rule.The suitable eluents for analysis of tetramethyl-ammonium cation and tetraethyl-ammonium,tetrapropyl ammonium cations were 0.02 mmol/L ethylenediamine-0.12 mmol/L citric acid(pH 4.0) and 0.2 mmol/L ethylenediamine-0.4 mmol/L citric acid-1% acetonitrile(pH 4.0),respectively.The flow rate and column temperature were 1.0 mL/min and 40 ℃,respectively.The detection limits(S/N=3) for three cations were 0.015,0.22,1.88 mg/L,respectively.Relative standard deviations(n=5) for peak areas were less than 2.3%.The method was successfully applied in the determination of quaternary ammonium ionic liquids synthesized in chemical laboratory and surfacetant tetramethyl-ammonium hydroxide,with recoveries of 99%-104%.The method is simple,accurate,reliable and practical. |
| Key Words:quaternary ammonium cations ion-exchange chromatography conductivity detection ionic liquids |
| 引用本文：刘永强,陈倩,于泓,唐慧慧.同系物季铵盐离子液体阳离子的离子交换色谱法分析[J].分析测试学报,2014,33(10):1154-1159. |
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