| 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 |
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| 引用本文： | 刘玉珍,于泓,张仁庆. 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[J]. 色谱, 2012, 30(4): 384-390. DOI: 10.3724/SP.J.1123.2011.12074 |
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| 作者姓名： | 刘玉珍 于泓 张仁庆 |
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| 作者单位： | 哈尔滨师范大学化学化工学院, 黑龙江 哈尔滨 150025 |
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| 基金项目： | 黑龙江省自然科学基金项目(No.B200909);黑龙江省高校科技创新团队建设计划项目(No.2011TD010) |
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| 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。
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| 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 |
| 收稿时间： | 2011-12-20 |
Determination of ionic liquid anions of trifluoroacetate, thiocyanate,tetrafluoroborate and trifluoromethanesulfonate by ion-pair chromatography with direct conductivity detection |
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| LIU Yuzhen,YU Hong,ZHANG Renqing. Determination of ionic liquid anions of trifluoroacetate, thiocyanate,tetrafluoroborate and trifluoromethanesulfonate by ion-pair chromatography with direct conductivity detection[J]. Chinese journal of chromatography, 2012, 30(4): 384-390. DOI: 10.3724/SP.J.1123.2011.12074 |
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| Authors: | LIU Yuzhen YU Hong ZHANG Renqing |
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| Affiliation: | College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China |
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| 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. |
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| Keywords: | ion-pair chromatography conductivity detection trifluoroacetate thiocyanate tetrafluoroborate trifluoromethanesulfonate ionic liquids |
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