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[采用直接电导检测离子色谱法分析哌啶鎓离子液体阳离子]

[Analysis of piperidinium ionic liquid cations by ion chromatography with direct conductivity detection].

作者信息

Zhang Renqing, Yu Hong, Liu Yuzhen

机构信息

College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China.

出版信息

Se Pu. 2012 Jul;30(7):728-32. doi: 10.3724/sp.j.1123.2012.02031.

Abstract

A method of ion chromatography with direct conductivity detection was established to determine three piperidinium ionic liquid cations, i. e. N-methyl, ethyl piperidinium cation ([MEPi]+), N-methyl, propyl piperidinium cation ([MPPi]+) and N-methyl, butyl piperidinium cation ([MBPi]+). The effects of eluent types, eluent concentration and column temperature on the retention of the cations were investigated with sulfonic acid base cation exchange column using ethylenediamine-citric acid-acetonitrile as eluent. The results indicated that, with the increase of column temperature, the retention times of piperidinium cations were reduced, so the retention process of piperidinium cations was exothermic. The retentions of piperidinium cation homologue accorded with carbon number rule. The successful separation of the three piperidinium cations within 7 min was achieved using the optimized eluent of 0.2 mmol/L ethylenediamine-0.3 mmol/L citric acid-3% acetonitrile (pH 4.4) at a flow rate of 1.0 mL/min and the column temperature of 30 degrees C. Under these conditions, the detection limits at a signal-to-noise ratio of 3 for [MEPi]+, [MPPi] and [MBPi]+ were 0.14, 0.20 and 0.56 mg/L, respec-tively. The relative standard deviations (n = 5) for peak areas were less than 1.2%. The method has been applied to the determination of piperidinium ionic liquids synthesized in chemical laboratory with the spiked recoveries of 97.6% to 105.1%. The method is accurate, reliable, rapid, and has better practicability.

摘要

建立了一种直接电导检测离子色谱法,用于测定3种哌啶鎓离子液体阳离子,即N-甲基乙基哌啶鎓阳离子([MEPi]+)、N-甲基丙基哌啶鎓阳离子([MPPi]+)和N-甲基丁基哌啶鎓阳离子([MBPi]+)。以乙二胺-柠檬酸-乙腈为洗脱液,磺酸基阳离子交换柱,考察了洗脱液类型、洗脱液浓度和柱温对阳离子保留行为的影响。结果表明,随着柱温升高,哌啶鎓阳离子的保留时间缩短,其保留过程为放热过程。哌啶鎓阳离子同系物的保留行为符合碳数规律。在流速1.0 mL/min、柱温30℃条件下,采用优化后的洗脱液0.2 mmol/L乙二胺-0.3 mmol/L柠檬酸-3%乙腈(pH 4.4),7 min内实现了3种哌啶鎓阳离子的成功分离。在此条件下,[MEPi]+、[MPPi]+和[MBPi]+的信噪比为3时的检出限分别为0.14、0.20和0.56 mg/L。峰面积的相对标准偏差(n = 5)小于1.2%。该方法已应用于化学实验室合成的哌啶鎓离子液体的测定,加标回收率为97.6%~105.1%。该方法准确、可靠、快速,具有较好的实用性。

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