离子色谱法测定硫酸氧钒中氯含量

Method for Determination of Chlorine in Sulphuric Acid Vanadium by Ion Chromatography

采用超纯水溶解试样,用水合肼在酸性条件下将高价钒还原,高速离心分离沉淀除去大量高价钒,再用阳离子交换柱进一步去除残余钒;选用IC S-5000+离子色谱系统,在氢氧化钾溶液梯度淋洗条件下,可较好完成硫酸氧钒样品中氯含量的分析。在系列浓度围内,色谱峰与浓度之间具有良好的线性关系(≥0.9995),加标回收率为95.6%-1 07.0%,相对标准偏差为0.5%-2.5%。结果表明,该方法简便、快速、灵敏、准确、精密度好、检出限低,适于硫酸氧钒中氯含量的测定。

The samples are dissolved using ultra pure water and high vanadium are reduced in acidic conditions by using hydrazine hydrate. A large number of high vanadium are precipitation removed at high-speed centrifugal separation. Further,residual vanadium are removed by cation exchange column. In hydroxide gradient elution conditions,selecting ICS-5000＋ion chromatography system,the content of chlorine are better analyzed in vanadyl sulfate sample. In the series of concentration range between the peaks and concentration has a good linear relationship（≥0.9995）,and the recovery rate was 95.6%-107% and relative standard deviation was 0.5%-2.5%. The results show that the method is simple,rapid,sensitive,accurate,good precision and low detection limit. It is suitable for the determination of chlorine content in vanadium sulfate.