色谱

色谱 ›› 2012, Vol. 30 ›› Issue (04): 384-390.DOI: 10.3724/SP.J.1123.2011.12074

• 特别策划 • 上一篇    下一篇

离子液体的阴离子三氟乙酸根、硫氰酸根、四氟硼酸根和三氟甲磺酸根的离子对色谱-直接电导检测法分析

刘玉珍, 于泓*, 张仁庆   

  1. 哈尔滨师范大学化学化工学院, 黑龙江 哈尔滨 150025
  • 收稿日期:2011-12-20 修回日期:2012-02-28 出版日期:2012-04-28 发布日期:2012-04-28
  • 通讯作者: 于泓,博士,教授,主要从事离子色谱和液相色谱的分析研究. Tel: (0451) 88060570
  • 基金资助:

    黑龙江省自然科学基金项目(No. B200909)和黑龙江省高校科技创新团队建设计划项目(No. 2011TD010).

Determination of ionic liquid anions of trifluoroacetate, thiocyanate, tetrafluoroborate and trifluoromethanesulfonate by ion-pair chromatography with direct conductivity detection

LIU Yuzhen, YU Hong*, ZHANG Renqing   

  1. College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China
  • Received:2011-12-20 Revised:2012-02-28 Online:2012-04-28 Published:2012-04-28

PDF

611

被引次数

23

摘要： 建立了同时测定离子液体的阴离子三氟乙酸根、硫氰酸根、四氟硼酸根和三氟甲磺酸根的反相离子对色谱-直接电导检测方法。采用Diamonsil C18分离柱,以离子对试剂-苹果酸-乙腈水溶液为流动相,从流动相组成和色谱柱温度两方面讨论并确定了优化的色谱条件,即以0.15 mmol/L氢氧化四丁铵-0.099 mmol/L苹果酸-20%(v/v)乙腈混合水溶液(pH 6.5)为流动相,柱温25 ℃。在此条件下,三氟乙酸根、硫氰酸根、四氟硼酸根和三氟甲磺酸根离子均达到基线分离,且不受其他常见阴离子氟离子、氯离子、溴离子、硝酸根、硫酸根的干扰。三氟乙酸根、硫氰酸根、四氟硼酸根和三氟甲磺酸根离子的检出限(信噪比为3)分别为0.21、0.07、0.36、0.12 mg/L。将方法应用于测定离子液体中三氟乙酸根、硫氰酸根、四氟硼酸根和三氟甲磺酸根离子,加标回收率为95.0%～104.6%。该法简便、快速、灵敏度较高,可满足离子液体样品的检测要求。

关键词: 电导检测, 离子对色谱, 离子液体, 硫氰酸根, 三氟甲磺酸根, 三氟乙酸根, 四氟硼酸根

Abstract: An ion-pair chromatographic method with direct conductivity detection was established on a reversed-phase silica-based column for the simultaneous determination of ionic liquid anions of trifluoroacetate, thiocyanate, tetrafluoroborate and trifluoromethanesulfonate. The analytes were separated using a mobile phase of ion pair reagent-malic acid-acetonitrile on the Diamonsil C18 column. The effects of mobile phase composition and column temperature on the retention of the anions were investigated. The optimized chromatographic conditions were as follows: 0.15 mmol/L tetrabutylammonium hydroxide-0.099 mmol/L malic acid-20% (v/v) acetonitrile aqueous solution (pH 6.5) as mobile phase, a column temperature of 25 ℃. Under the optimal conditions, the baseline separation of trifluoroacetate, thiocyanate, tetrafluoroborate and trifluoromethanesulfonate was achieved without any interference by other ordinary anions (fluoride, chloride, bromide, nitrate, sulfate). The detection limits (S/N=3) were 0.21, 0.07, 0.36 and 0.12 mg/L for trifluoroacetate, thiocyanate, tetrafluoroborate and trifluoromethanesulfonate, respectively. The method has been applied to the determination of the four anions in ionic liquids. The spiked recoveries of the anions were from 95.0% to 104.6%. The results demonstrate that the convenience, rapidity, sensitivity and accuracy are fit for the requirements of quantitative analysis of trifluoroacetate, thiocyanate, tetrafluoroborate and trifluoromethanesulfonate in ionic liquids.

Key words: conductivity detection, ionic liquids, tetrafluoroborate, thiocyanate, trifluoroacetate, trifluoromethanesulfonate, ion-pair chromatography