吡啶离子液体阳离子的离子色谱法分析  

Analysis of Pyridinium Ionic Liquid Cations by Ion Chromatography with Direct Conductivity Detection

作　　者：陈倩[1] 于泓[1] 孟令敏[1] 黄旭[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》2011年第1期38-42,共5页Journal of Instrumental Analysis

基　　金：黑龙江省自然科学基金资助项目(B200909);黑龙江省教育厅科学技术研究项目(11541088)

摘　　要：建立了离子色谱-直接电导检测法分离测定3种吡啶离子液体阳离子（N-乙基吡啶、N-丁基吡啶和N-己基呲啶阳离子）的方法。采用磺酸型阳离子交换色谱柱，以乙二胺-柠檬酸-乙腈为淋洗液，考察了淋洗液种类和浓度以及色谱柱温度对离子液体阳离子保留的影响。实验发现，吡啶阳离子的保留过程是放热过程，其同系物的保留符合碳数规律。优化的色谱条件为：流动相为0．2mmol／L乙二胺-0．3mmol／L柠檬酸-3％（体积分数）乙腈（pH4．4），流速1．0mL／min，柱温45℃。在此条件下可基线分离3种吡啶离子液体阳离子。所NIgH离子的检出限（SIN=3）分别为0．60、1．59、10．8mg/L，峰面积的相对标准偏差（n=5）在1．2％以下。将该方法用于实验室合成的离子液体的测定，加标回收率为100％～104％。A method of ion chromatography and direct conductivity detection was established to determine three pyridinium ionic liquid cations, e.g. I-ethyl pyridinium eation（ EPy ＋ ） , 1-butyl pyridinium cation （ BPy ＋ ） and 1 -hexyl pyridinium cation （ HPy ＋ ）. The effec.ts of eluent types, eluent coneentration and column temperature on retention of the cations were investigated with sulfonie acid base eation-exehange column using ethylenediamine -citrate acid -acetonitrile as eluent. The result indieated that, with the increase of column temperature, the retention times of pyridinium eations were redueed, so the retention process of pyridinium cations is exothermic. The retentions of pyridinium cations accord with carbon number rule. The optimum chromatographic conditions were as follows： mobile phase： 0.2 mmol/L ethylenediamine -0. 3 mmol/L citrate acid -3% acetonitrile（ pH 4. 4） ; flow rate： 1.0 mL/min; eolumn temperature： 45 ~C. Under the optimum eonditions, three pyridinium cations were successfully separated. The detection limits （ S/N= 3 ） for EPy ＋ , BPy ＋ and HPy＋were 0. 60, 1.59, 10. 8 rag/L, respectively. Relative standard deviations（n = 5） for peak areas were less than 1.2% . The method was applied in the determination of pyridinium ionic liquids synthesized in ehemieal laboratory with spiked reeoveries of 100% - 104% . The good linearity and repeatability of the method made it meet the requirements of quantitative analysis.

关 键 词：离子液体 离子色谱 电导检测 烷基吡啶 

分 类 号：O657.75[理学—分析化学]