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本文采用国产XJP—821(B)型新极谱仪,用滴汞电极2.5次微分法,测定硫酸试剂中痕量硒(Ⅳ)。通过多种底液组成的试验,提出在HCl—HClO_4—NaHSO_3—NH_3—NH_4Cl—NH_2OH·HCl—KIO_3体系中,硒的峰电位—0.57V(相对银电极)。硒浓度在0.005～0.500ng·ml~(-1)范围与峰高呈线性关系,最低检出限为0.005ng·ml~(-1)。试验选择了最佳条件,并且对硒的催化波性质作了初步探讨。对不同地区的硫酸试剂作了硒的分析。分析结果重现性好,变异系数为5.5%～19.4%,相关系数为O.9999,回收率为97%～109%。
In this paper, domestic XJP-821 (B) new polarographic apparatus was used to determine the trace amount of selenium (Ⅳ) in sulfuric acid reagent by droplet mercury electrode 2.5 times differential method. Based on the experiments of a variety of bottom solutions, the peak potential of selenium is -0.57V (relative to the silver electrode) in the system of HCl-HClO 4 -HaHSO 3 -NH 3 -NH 4 Cl-NH 2 OH · HCl-KIO 3. The concentration of selenium in the range of 0.005 ~ 0.500ng · ml ~ (-1) has a linear relationship with the peak height, with the lowest detection limit of 0.005ng · ml ~ (-1). The optimal conditions were selected and the catalytic wave properties of selenium were preliminarily discussed. Selenium analysis of sulfuric acid reagents in different regions. The results showed good reproducibility, with a coefficient of variation of 5.5% -19.4%, a correlation coefficient of 0.999, and a recovery of 97% -109%.