火焰原子吸收光谱法测定粗硒中的银

Determination of silver in crude selenium by flame atomic absorption spectrometry

当粗硒中的银量在5~500 g/t时,采用硝酸、盐酸溶解试样,加入硫酸挥发去除硒,在10%的盐酸介质中采用火焰原子吸收光谱仪测定银;当粗硒中的银量在300~10 000 g/t时,采用硝酸溶解,在25%的盐酸介质中采用火焰原子吸收光谱仪测定银。通过测定介质、基体和共存元素对粗硒中银测定的影响进行研究,其实验结果表明,共存元素对银的测定没有干扰,测定试液中硒质量浓度小于4 mg/m L时不干扰银的测定。该方法检出限低,测定结果准确、稳定,相对标准偏差为0.39%~8.62%,加入标准物质回收率为99.0%~102.4%,可用于粗硒中银量为5~10 000 g/t的测定。

Crude selenium was dissolved in nitric and hydrochloric acid when silver content is between 5 g / t and500 g / t,sulfuric acid was used to volatilize the selenium and then silver in solution was determined in 10 % hydrochloric acid by flame atomic absorption spectrometry; Crude selenium was dissolved in nitric acid when silver content is between 300 g / t and 10 000 g / t,and silver in solution was determined in 25 % hydrochloric acid by flame atomic absorption spectrometry. An investigation was made by examining the effects the determination medium and matrix and coexisting elements have on the determination of silver in crude selenium. The results showed that coexisting elements didn＇t make any difference to the determination of silver and so did the selenium when the content is under 4 mg / m L.This method has low detection limit and the stability and accuracy are high,the RSD is 0. 39 % to 8. 62 % and the recovery rate is 99. 0 % to 102. 4 % with addition of standard substance. The method can be easily applied to the determination of crude selenium containing silver at about 5 g / t to 10 000 g / t.