贵铅中铅和金的连续测定

Continuous determination of lead and gold in precious lead

摘要: 研究建立了贵铅中铅和金的连续测定方法。样品使用硝酸、溴溶解，加入硫酸形成硫酸铅沉淀，与金及杂质元素分离，乙酸-乙酸铵溶解硫酸铅，Na2EDTA滴定铅量；金和不溶渣灰化-碱溶或灰化-王水溶解后火焰原子吸收光谱法测定金量。本方法测定铅的相对标准偏差为0.12 %，加标回收率为92.10 %～96.42 %；测定金的相对标准偏差为0.20 %～0.52 %，加标回收率为90.20 %～97.20 %，准确度和精密度良好，符合分析测定要求。

Abstract: The research established the continuous determination method for lead and gold in precious lead.The samples are dissolved with nitric acid and bromine.Lead sulfate precipitation is generated by adding sulfuric acid,sepa-rating lead from gold and impurities.Acetic acid-ammonium acetate dissolves lead sulfate.And lead content is determined by Na2EDTA titration;gold content is determined by flame atomic absorption spectrometry after ashing-alkali dissolution or ashing-aqua regia dissolution.When lead content is determined,the method has a RSD of 0.12 %,the recovery rate of reference materials 92.10 %-96.42 %;when gold content is determined,the RSD is 0.20 %-0.52 %,the recovery rate of reference materials is 90.20 %-97.20 %.The method has good accuracy and precision and is consistent with the requirement of analysis and determination.