样品(2.00 mL)用盐酸10 mL、硝酸3 mL溶解后,蒸馏至2~3 mL,加入100 g·L-1酒石酸溶液2 mL,用盐酸(5+95)溶液稀释定容至100 mL。采用电感耦合等离子体原子发射光谱法测定样品溶液中锑、铋、钴、镍和砷的含量。选择锑、铋、钴、镍、砷元素的分析谱线分别为206.836,223.061,228.615,231.604,193.696 nm。5种元素在一定的质量浓度范围内与其发射强度呈线性关系,方法的检出限(3s)在0.005~0.130 mg·L-1之间。方法用于铜电积液分析,所得测定值与火焰原子吸收光谱法测定结果相符。加标回收率在95.8%~108%之间,测定值的相对标准偏差(n=11)在0.70%~6.4%之间。

The sample (2.00 mL) was decomposed with 10 mL of hydrochloric acid, and nitric acid 3 mL, evaporeted to 2-3 mL. Then 2 mL of 100 g·L-1 tartaric acid solution were added and the solution was diluted to 100 mL with HCl(5+95) solution, and ICP-AES was applied to the determination of stibium, bismuth, cobalt, nickel and arsenic in the sample solution. Analytical spectral lines of 206.836, 223.061, 228.615, 231.604, 193.696 nm were chosen for the determination of Sb, Bi, Co, Ni and As respectively. Linear relationships between values of emission intensity and mass concentration of the 5 elements were kept in definite ranges, with detection limits (3s) in the range of 0.005-0.130 mg·L-1. The proposed method was applied to the analysis of copper electrowinning solution, giving results in consistency with those given by FAAS. Values of recovery found by standard addition method were in the range of 95.8%-108%, and values of RSD′s (n=11) in the range of 0.70%-6.4%.