Abstract:The sample was dissolved with ammonium fluoride-hydrochloric acid-nitric acid-perchloric acid. The coexisting elements such as arsenic, antimony and tin were separated by acid-hydrobromic acid. Then, the sulphuric acid was added to promote the formation of lead sulfate precipitation, which was separated with the other elements by filtration. Before titration, mercaptoacetic acid was added into solution to eliminate the influence of bismuth. In acetic acid-sodium acetate buffer solution, the determination method of lead content in silver separating residue by EDTA titration was established by using xylenol orange as an indicator. The proposed method was used to determination of lead content in silver separating residue. The results showed that the relative standard deviations (RSD, n=11) was between 0.32% and 0.90%. The recovery rate of the determination method was between 99.98% and 101.91%. The optimized operation process is simple and satisfies the production requirements.