大体积进样-浓缩柱在线富集-离子色谱法测定水中痕量及超痕量溴酸盐

摘要

A method for the determination of trace and ultra-trace level bromate in water by ion chromatography with large volume sample injection for on-line preconcentration was estab-lished. A high capacity Dionex IonPac AG23 guard column was simply used as the enrichment column instead of the loop for the preconcentration of bromate. High purity KOH solution used as eluent for gradient elution was on-line produced by an eluent generator automatically. The results showed that a good linear relationship of bromate was exhibited in the range of 0. 05-51. 2 μg/L( r≥0. 999 5),and the method detection limit was 0. 01 μg/L. Compared with con-ventional sample injection,the injection volume was up to 5 mL,and the enrichment factor of this method was about 240 times. This method was successfully applied for several real samples of pure water which were purchased in the supermarket,and the recoveries of bromate were between 90%-100% with the RSDs( n=6)of 2. 1%-6. 4% at two spiked levels. This method without pretreatment is simple,and of high accuracy and precision. The preconcentration can be achieved by large volume sample injection. It is suitable for the analysis of trace and ultra-trace level bromate.%建立了一种测定水中痕量及超痕量溴酸盐的在线富集大体积进样离子色谱法。采用实验室常备的柱容量较高的 Dionex IonPac AG23保护柱作为浓缩柱，连接在定量环处富集溴酸盐。淋洗液自动发生装置在线生成高纯度氢氧化钾淋洗液进行梯度洗脱，抑制电导检测。实验结果表明：溴酸盐质量浓度范围在0.05~51.2μg／L 之间时线性关系良好，相关系数r≥0.9995，方法检出限为0.01μg／L。与常规进样相比，进样量可高达5 mL，浓缩因子约为240倍。本方法成功应用于市售纯净水中溴酸盐的测定，2个加标水平的回收率在90％~100％之间，RSD（ n=6）为2.1％~6.4％。该方法无需前处理，操作简单，准确度和精密度良好。通过大体积进样实现高倍富集，适用于痕量及超痕量溴酸盐的分析。