离子色谱法同时测定硫酸钯溶液中的氯离子和硝酸根

摘要

建立了离子色谱法同时测定贵金属化合物硫酸钯溶液中的氯离子和硝酸根离子含量的方法.使用IC-H型阳离子交换前处理柱除去样品中的钯(II)阳离子;采用梯度淋洗程恅,以KOH溶液(1.0 mL/min)淋洗液,用抑制性电导检测,外标法定量测定氯离子和硝酸根离子.测定线性范围为0.04~1.2μg/mL,检出限为0.006~0.015μg/mL,相对标准偏差(RSD)为2.5%~4.9%,样品加标回收率94.2%~112.9%,可满足硫酸钯溶液产品中氯离子和硝酸根离子杂质测定要求.%An ion chromatographic method has been established for measuring the concentrations of chloride and nitrate ions in the palladium(II) sulfate solution. The samples were pretreated with IC-H cation exchange resin to eliminate the interference from Pd(II) cations. Following the gradient elution with KOH solution at a speed of 1.0 mL/min), the two anions were detected simultaneously by the suppressed conductivity detector and their concentrations were calculated by external standard method. Under the optimum conditions, the linear range of the method was 0.04~1.2 μg/mL, and the limit of detection was 0.006~0.015 μg/mL. The recoveries were found to be in the range of 94.2%~112.9% with the relative standard deviation of 2.5%~4.9%. The method could be applied to the determination of Cl- and NO3-in the product of palladium(II) sulfate solution.