海贝样品经硝酸和过氧化氢微波加热消解,用氢化物发生-原子荧光光谱法测定其中硒的含量。使用溶于5 g·L-1氢氧化钾溶液中的10 g·L-1硼氢化钾溶液与溶液中硒离子反应生成氢化物。试样溶液中加入抗坏血酸消除硝酸的干扰。在优化的试验条件下,硒的质量浓度在600 μg·L-1以内与其荧光强度呈线性关系;方法检出限(3s/k)为0.076 μg·L-1。对2 μg·L-1硒标准溶液进行11次测定,相对标准偏差为1.6%。方法用于4种的海贝样品分析,加标回收率在86.0%~116.0%之间。

The sample of sea shellfish was digested with HNO3 and H2O2 with microwave assisted heating, and the content of Se in sample solution was determined by HG-AFS. Hydride of Se ion was generated by reacting with 10 g·L-1 KBH4 solution (dissolved in 5 g·L-1 KOH solution). The interference of HNO3 was eliminated by adding ascorbic acid. Under the optimized experimental conditions, linear relationship between the fluorescence intensity and mass concentration of Se was kept in the range within 600 μg·L-1, with detection limit (3s/k) of 0.076 μg·L-1. Test for precision was performed with 2 μg·L-1 Se standard solution, the value of RSD (n=11) found was 1.6%. The proposed method was applied to the analysis of 4 substantial samples, giving values of recovery found by standard addition method in the range of 86.0%-116.0%.