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样品(2.00mL)用盐酸10mL、硝酸3mL溶解后,蒸馏至2~3mL,加入100g·L-1酒石酸溶液2mL,用盐酸(5+95)溶液稀释定容至100mL。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206.836,223.061,228.615,231.604,193.696nm。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0.005~0.130mg·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 dissolved in 10 mL of hydrochloric acid and 3 mL of nitric acid and then distilled to 2 to 3 mL. 2 mL of a 100 g · L-1 tartaric acid solution was added and the volume was diluted to 100 mL with a solution of (5 + 95) hydrochloric acid. Determination of antimony, bismuth, cobalt, nickel and arsenic in sample solution by inductively coupled plasma atomic emission spectrometry. The analytical spectra of antimony, bismuth, cobalt, nickel and arsenic are 206.836, 223.061, 228.615, 231.604 and 193.696 nm, respectively. The five elements have a linear relationship with the emission intensity within a certain mass concentration range. The detection limit (3s) of the five methods is between 0.005 and 0.130 mg · L -1. The method was applied to the analysis of copper electrowinning. The obtained results were in good agreement with the results of flame atomic absorption spectrometry. The spiked recoveries ranged from 95.8% to 108%, and the relative standard deviations (n = 11) of the measured values ranged from 0.70% to 6.4%.