| 四氟硼酸根的离子排斥色谱-直接电导检测法分析 |
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| 基金项目:黑龙江省教育厅科学技术研究项目（11541088）;黑龙江省高校科技创新团队建设计划资助项目（2011TD010） |
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| 中文摘要:建立了离子排斥色谱-直接电导检测法分离测定四氟硼酸根的方法。以Shim-pack SCR-102H离子排斥色谱柱为分离柱,考察了淋洗液种类、浓度、色谱柱温度对四氟硼酸根测定的影响。最佳色谱条件为:以0.2 mmol/L p-甲苯磺酸溶液为流动相，流速1.0 mL/min，柱温 40 ℃，进样体积20 μL。在此条件下，四氟硼酸根的保留时间为5.95 min。该方法测定四氟硼酸根的检出限（S/N=3）为0.14 mg/L，标准曲线的线性范围为3~100 mg/L，保留时间和峰面积的相对标准偏差（n=5） 分别为0.02%和0.7%。将方法用于离子液体中四氟硼酸根的测定，加标回收率为99%~102%。 |
| 中文关键词:离子排斥色谱法 四氟硼酸根 离子液体 p-甲苯磺酸 |
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| Determination of Tetrafluoroborate by Ion-exclusion Chromatography with Direct Conductivity Detection |
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| Abstract:A method was developed for the determination of tetrafluoroborate by ion-exclusion chromatography coupled with direct conductivity detection.Chromatographic separation was performed on a Shim-pack SCR-102H column.Influences of eluent and column temperature on retention time of tetrafluoroborate were investigated.The results indicated the retention time of tetrafluoroborate was increased with the increase of column temperature,and the retention process of tetrafluoroborate was endothermic.The optimal chromatographic conditions for determination of tetrafluoroborate were using 0.2 mmol/L p-toluenesulfonic acid as eluent with a column temperature of 40 ℃ and a flow rate of 1.0 mL/min.Under the optimal conditions,a good separation of tetrafluoroborate and common organic acids（such as,citric acid,malic acid,formic acid and acetic acid） was obtained.The retention time of tetrafluoroborate was 5.95 min.The determination were not interfered by the common inorganic anions（Cl-,Br-,NO-3,SO2-4）.The calibration curve was linear in the range of 3-100 mg/L with a detection limit（S/N=3） of 0.14 mg/L.The relative standard deviations（n=5） for retention time and peak area were 0.02% and 0.7%,respectively.The method was successfully applied in the determination of tetrafluoroborate in ionic liquids with spiked recoveries of 99%-102%.With the advantages of simplicity,accuracy and good repeatability,this method could be applied in the quality control analysis of relevant ionic liquids. |
| Key Words:ion-exclusion chromatography tetrafluoroborate ionic-liquid p-toluenesulfonic acid |
| 引用本文：张欣，司明鑫，于泓，李朦.四氟硼酸根的离子排斥色谱-直接电导检测法分析[J].分析测试学报,2011,30(10):1163-1166. |
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