色谱

色谱

• 研究论文 • 上一篇    下一篇

离子色谱法同时测定离子液体中的三氟乙酸根、氟硼酸根及卤素离子

李偲文1, 张小东2, 于泓1*   

  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:2010-02-24 修回日期:2010-04-24 出版日期:2010-07-28 发布日期:1980-03-25
  • 通讯作者: 于泓

Simultaneous determination of trifluoroacetate, tetrafluoroborate and halide ions in ionic liquid by ion chromatography

LI Siwen1, ZHANG Xiaodong2, YU Hong1*   

  1. 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:2010-02-24 Revised:2010-04-24 Online:2010-07-28 Published:1980-03-25
  • Contact: YU Hong

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摘要： 采用离子色谱-直接电导检测法同时测定了离子液体中的三氟乙酸根(CF3COO~)、氟硼酸根(BF4~)及卤素离子(F~、Cl~、Br~)。实验采用Shim-pack IC-A3阴离子交换色谱柱,分别选用邻苯二甲酸氢钾、邻苯二甲酸+三(羟甲基)氨基甲烷、对羟基苯甲酸+三(羟甲基)氨基甲烷+硼酸为淋洗液,考察了淋洗液种类和浓度、乙腈浓度、色谱柱温度对分离测定三氟乙酸根、氟硼酸根及卤素离子的影响。确定的最佳色谱条件为: 以1.2 mmol/L邻苯二甲酸氢钾为淋洗液,柱温45 ℃,流速1.0 mL/min。在此条件下,可同时分离上述5种阴离子,且色谱峰形对称。所测阴离子的检出限(以信噪比为3计)为0.01～0.50 mg/L,保留时间和峰面积的相对标准偏差(n=5)分别不大于0.2%和1.2%。将方法应用于测定离子液体中的三氟乙酸根、氟硼酸根及卤素离子,加标回收率为98.0%～103.2%。该方法简单、准确、可靠,具有较好的实用性。

关键词: 氟硼酸根, 离子色谱, 离子液体 , 卤素离子, 三氟乙酸根

Abstract: A method was developed for the simultaneous determination of trifluoroacetate, tetrafluoroborate and halide ions (F~, Cl~, Br~) by ion chromatography with direct conductivity detection. The chromatographic separation was performed on a Shim-pack IC-A3 anion-exchange column with potassium biphthalate, phthalic acid+tris(hydroxymethyl)-aminomethane, and p-hydroxybenzoic acid+tris(hydroxymethyl)-aminomethane+boric acid as eluent, separately. The effects of the nature of eluent, eluent concentration, acetonitrile concentration and column temperature on the separation and the retention factors of the anions were investigated. The optimized chromatographic conditions for the determination of the anions were as follows: 1.2 mmol/L potassium biphthalate as eluent, a column temperature of 45 ℃ and a flow rate of 1.0 mL/min. Under the optimal conditions, the anions were baseline separated. Moreover, the symmetries of peaks were better. The limits of detection (S/N=3) for the anions were in the range of 0.01~0.50 mg/L. The relative standard deviations (RSDs) of the chromatographic retention time and peak area for the anions were not more than 0.2% and 1.2% (n=5), respectively. The method has been applied to the determination of trifluoroacetate, tetrafluoroborate and halide ions in ionic liquids. The spiked recoveries of the anions were from 98.0% to 103.2%. The method is simple, accurate and reliable, and has better practicability.

Key words: halide ions, ionic liquid , tetrafluoroborate, trifluoroacetate, ion chromatography