直接电导检测-离子色谱法分离测定氟硼酸根及常见无机阴离子  

Determination of Tetrafluoroborate and Common Inorganic Anions by Ion Chromatography with Direct Conductivity Detection

作　　者：周爽[1] 于泓[1] 艾红晶[1] 

机构地区：[1]哈尔滨师范大学化学化工学院,哈尔滨150025

出　　处：《分析化学》2008年第11期1521-1525,共5页Chinese Journal of Analytical Chemistry

基　　金：黑龙江省高校骨干教师创新能力资助计划项目(No.1054G022);黑龙江省研究生创新科研基金(No.YJSLX2008160HLJ);黑龙江省教育厅科学技术研究项目(No.10551103)资助

摘　　要：研究了直接电导检测-离子色谱法分离测定BF4-及常见无机阴离子（F^-、Cl^-、Br^-、NO3^-、SO24^-）。实验采用Shim-pack IC-A3阴离子交换色谱柱,分别选用邻苯二甲酸氢钾、对羟基苯甲酸＋三（羟甲基）氨基甲烷＋硼酸、邻苯二甲酸＋三（羟甲基）氨基甲烷为淋洗液,考察了淋洗液种类、浓度、色谱柱温度、流速对分离测定BF4-及常见无机阴离子的影响。确定最佳色谱条件为：以1.25 mmol/L邻苯二甲酸氢钾为淋洗液,流速1.5 mL/min,柱温45℃。在此条件下可同时基线分离6种阴离子,且色谱峰形对称。所测阴离子的检出限为0.02-0.58 mg/L;峰面积的相对标准偏差（RSD,n=5）小于0.8%。将方法应用于测定离子液体中的BF4^-及其它无机阴离子,加标回收率在98.2%-102.7%之间。A method for the determination of tetrafluoroborate （BF4^- ） and common inorganic anions （F^-, Cl^- , Br^- , NO3^- , SO24^- ） by ion chromatography using direct conductivity detection was proposed. Chromatographic separation was performed on a Shim-pack IC-A3 anion-exchange column （150 mm ×4.6 mmi. d. ）. Potassium biphthalate, p-hydroxybenzoic acid ＋ tris （hydroxymethyl） -aminomethane ＋ boric acid, phthalic acid ＋ tris（hydroxymethyl）-aminomethane were used as eluent, respectively. The effects of the types of eluent, eluent concentration, column temperature and flow rate on separation and retention time of the anions were investigated. The optimized chromatographic conditions for the separation and determination of tetrafluoroborate and common inorganic anions were as follows： 1.25 mmol/L potassium biphthalate as the eluent, column temperature of 45 ℃ and a flow rate of 1.5 mL/min. The detection limits （S/N = 3） of six anions were in range of 0.02 -0.58 mg/L. The relative standard deviations （RSD） of the chromatographic peak areas for six anions were less than 0.8 % （ n = 5 ）. The method was successfully applied to determine tetrafluoroborate and other inorganic anions in ion liquids. The recoveries of six anions after spiking were from 98.2% to 102.7%.

关 键 词：离子色谱法 氟硼酸根 无机阴离子 电导检测 离子液体 

分 类 号：O657.75[理学—分析化学]