整体柱和填充柱离子对色谱-间接紫外检测法分析四乙基铵根离子

doi:10.3724/SP.J.1123.2015.03043

色谱 ›› 2015, Vol. 33 ›› Issue (7): 759-764.DOI: 10.3724/SP.J.1123.2015.03043

整体柱和填充柱离子对色谱-间接紫外检测法分析四乙基铵根离子

邹春苗¹, 张小东², 于泓¹, 关超¹, 王淼煜¹

1. 哈尔滨师范大学化学化工学院, 黑龙江哈尔滨 150025;
2. 黑龙江省齐齐哈尔矿产勘查开发总院, 黑龙江齐齐哈尔 161006

收稿日期:2015-03-31 出版日期:2015-07-08 发布日期:2015-07-27
通讯作者: 于泓
基金资助:
黑龙江省自然科学基金项目(B201307);哈尔滨师范大学硕士研究生创新科研项目(HSDSSCX2014-22).

Ion-pair chromatography-indirect ultraviolet detection for determination of tetraethyl ammonium using a monolithic column and a packed column

ZOU Chunmiao¹, ZHANG Xiaodong², YU Hong¹, GUAN Chao¹, WANG Miaoyu¹

1. College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China;
2. Qiqihar Mineral Exploration and Development General Institute of Heilongjiang Province, Qiqihar 161006, China

Received:2015-03-31 Online:2015-07-08 Published:2015-07-27

摘要/Abstract

摘要：

建立了整体柱离子对色谱-间接紫外检测和填充柱离子对色谱-间接紫外检测分析四乙基铵根离子的两种方法。用反相整体柱和反相填充柱,以咪唑离子液体-离子对试剂-有机溶剂为流动相,研究了背景紫外吸收试剂、检测波长、离子对试剂、有机溶剂、柱温和流速对测定四乙基铵根离子的影响,比较了两种色谱柱的差异,并讨论了保留规律。在优化的实验条件下,两种方法测定四乙基铵根离子的保留时间分别是2.40和3.02 min;检出限分别是0.04和0.07 mg/L;峰面积的相对标准偏差分别是0.16%和0.11%;保留时间的相对标准偏差分别是0.02%和0.01%。将这两种方法用于分析实验室合成的溴化四乙基铵离子液体,加标回收率分别为98.2%和99.1%。两种方法均能满足四乙基铵根离子测定的需要。

关键词: 间接紫外检测, 离子对色谱, 咪唑离子液体, 四乙基铵根离子, 填充柱, 整体柱

Abstract:

Two methods were developed for the determination of tetraethyl ammonium by ion-pair chromatography-indirect ultraviolet detection using a monolithic column and a packed column with ionic liquid as additive in mobile phase. Chromatographic separations were performed on a monolithic column and a packed column both on reversed phase using imidazolium ionic liquid aqueous solution-ion-pair reagent-organic solvent as mobile phase. The effects of the background ultraviolet absorption reagent, detection wavelength, ion-pair reagent, organic solvent, column temperature and flow rate on the determination of tetraethyl ammonium were investigated. The difference between the two chromatographic columns was compared and the retention rules were discussed. Under the optimized chromatographic conditions, for tetraethyl ammonium on monolithic column and packed column, the retention times were 2.40 and 3.02 min; the detection limits (S/N=3), 0.04 and 0.07 mg/L; the RSDs (n=5) for peak areas, 0.16% and 0.11%; and the RSDs (n=5) for retention times, 0.02% and 0.01%, respectively. The two methods have been successfully applied to the determination of tetraethyl ammonium ionic liquids synthesized by laboratory. The recoveries of the tetraethyl ammonium after spiking were 98.2% and 99.1%, respectively. The two methods can meet the requirements for the quantitative analysis of tetraethyl ammonium.

Key words: imidazolium ionic liquids, indirect ultraviolet detection, ion-pair chromatography, monolithic column, packed column, tetraethyl ammonium

中图分类号:

O658

邹春苗, 张小东, 于泓, 关超, 王淼煜. 整体柱和填充柱离子对色谱-间接紫外检测法分析四乙基铵根离子[J]. 色谱, 2015, 33(7): 759-764.

ZOU Chunmiao, ZHANG Xiaodong, YU Hong, GUAN Chao, WANG Miaoyu. Ion-pair chromatography-indirect ultraviolet detection for determination of tetraethyl ammonium using a monolithic column and a packed column[J]. Chinese Journal of Chromatography, 2015, 33(7): 759-764.

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整体柱和填充柱离子对色谱-间接紫外检测法分析四乙基铵根离子

Ion-pair chromatography-indirect ultraviolet detection for determination of tetraethyl ammonium using a monolithic column and a packed column

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