离子色谱-直接电导检测法分离测定吗啉离子液体阳离子  

Determination of Morpholinium Ionic Liquid Cations by Ion Chromatography with Direct Conductivity Detection

作　　者：孙晓娇[1] 于泓[1] 张仁庆[1] 

机构地区：[1]哈尔滨师范大学化学化工学院,黑龙江哈尔滨150025

出　　处：《分析测试学报》2013年第6期705-709,共5页Journal of Instrumental Analysis

基　　金：黑龙江省教育厅科学技术研究项目(12531192)

摘　　要：建立了离子色谱-直接电导检测法分析N-甲基乙基吗啉([MEMo]+)、N-甲基丙基吗啉([MPMo]+)2种吗啉离子液体阳离子的方法。采用磺酸型阳离子交换色谱柱,以乙二胺-乙腈为流动相,研究了色谱柱、流动相、色谱柱温度对吗啉阳离子保留的影响,并讨论了保留规律。结果表明,吗啉阳离子的保留基本属于离子交换模式,是一个放热过程。在柱温30℃,流速1.0 mL/min,以0.1 mmol/L乙二胺-0.5%乙腈(用盐酸调节至pH 5.0)为流动相条件下,[MEMo]+和[MPMo]+阳离子可在4 min内得到基线分离,检出限(S/N=3)分别为0.08、0.13 mg/L,峰面积的相对标准偏差(RSD,n=5)不大于1.5%。将此方法用于测定实验室合成的吗啉离子液体样品,加标回收率为94.0%～106.0%。方法准确、可靠、快速,具有较好的实用性,可满足离子液体样品的检测要求。An ion chromatographic method with direct conductivity detection for the determination of N-methyl，ethyl morpholinium cation（［MEMo］＋），N-methyl，propyl morpholinium cation（［MPMo］＋） two morpholinium ionic liquid cations was developed using a cation-exchange column and ethylenediamine-acetonitrile as mobile phase.The effects of column type，mobile phase and column temperature on retention and separation of the cations were investigated.The retention rules of the cations under different chromatographic conditions were formulated.The results indicated that the retention process of morpholinium cations retained in line with the ion-exchange mode，wihich was an exothermic process.The successful separation of the two morpholinium ionic liquid cations was achieved using the optimized mobile phase of 0.1 mmol/L ethylenediamine-0.5% acetonitrile（adjusted to pH 5.0 with hydrochloric acid） at a flow rate of 1.0 mL/min and a column temperature of 30 ℃.Under the optimal conditions，the two morpholinium ionic liquid cations could be successfully separated in 4 min.The detection limits（S/N=3） for ［MEMo］＋ and ［MPMo］＋ were 0.08 mg/L and 0.13 mg/L，respectively.The relative standard deviations（RSDs，n=5） of the chromatographic peak areas for the cations were no more than 1.5%.The method was successfully applied in the determination of morpholinium bromide ionic liquid samples synthesized by chemistry laboratory.The recoveries of morpholinium cations after spiked were in the range of 94.0%-106.0%.The method was proved to be accurate，reliable and rapid，and could meet the requirements for quantitative analysis of morpholinium ionic liquid samples.

关 键 词：离子液体 吗啉阳离子 离子色谱 电导检测 乙二胺 

分 类 号：O657.75[理学—分析化学] TQ425.231[理学—化学]