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建立了离子液体阴离子p-甲苯磺酸根的离子色谱-直接电导检测分析方法。采用Shim-pack IC-A3季铵型阴离子交换色谱柱,考察了流动相种类和色谱柱温度对分离测定p-甲苯磺酸根的影响。确定最佳色谱条件为:以1.2 mmol/L柠檬酸-15%乙腈混合水溶液(pH 5.0)为流动相,流速1.0 mL/min,柱温45℃。在此条件下,p-甲苯磺酸根与常见无机阴离子(氟离子、氯离子、溴离子和硝酸根)可以获得很好的分离。该方法测定p-甲苯磺酸根的线性范围为4～100 mg/L,检出限(S/N=3)为1.22 mg/L,保留时间和峰面积的相对标准偏差(n=5)分别为0.42%和1.8%。将方法用于离子液体中p-甲苯磺酸根的测定,加标回收率为99.6%。
An ion chromatography-direct conductivity detection and analysis method for the anion p-toluenesulfonate anion was established. Shim-pack IC-A3 quaternary ammonium anion exchange columns were used to investigate the effect of mobile phase species and column temperature on the separation and determination of p-toluenesulfonate. The best chromatographic conditions were as follows: the flow rate was 1.0 mL / min with 1.2 mmol / L citric acid-15% acetonitrile mixed aqueous solution (pH 5.0) and the column temperature was 45 ℃. Under these conditions, p-toluenesulfonate can be well separated from common inorganic anions (fluoride, chloride, bromide and nitrate). The linear range of p-toluenesulfonate was 4-100 mg / L and the limit of detection (S / N = 3) was 1.22 mg / L. The relative standard deviations of retention time and peak area (n = 5) 0.42% and 1.8%. The method was applied to the determination of p-toluenesulfonate in ionic liquid with the recovery of 99.6%.