Abstract：The determination method of lead in lead concentrate with high content bismuth by national standard method has some problems such as difficulty in interference elimination and complicated operation steps. The sample was dissolved with hydrochloric acid, nitric acid and sulfuric acid. Then arsenic,antimony and tin were removed by hydrobromic acid treatment. Most of bismuth was complexed with tartaric acid. The lead sulfate was filtrated followed by washing with sulfuric acid solution. The lead sulfate precipitate together with filter paper was boiled in 45 mL of acetic acid-sodium acetate solution for 5 min. After dilution to 150 mL with water, 5 mL of sodium citrate solution, 4 drops of xylenol orange solution and 2 mL of mercaptoacetic acid (1+99) were added to eliminate the interference of bismuth. The content of lead was finally determined by EDTA titration. The systematic deviation of lead content in filtrate was modified by procedure optimization. The lead sulfate precipitate together with filter paper was dissolved and titrated,so the single determination of filtrate and residue was not required. Moreover, the placing period of lead sulfate precipitate was shortened to 1 h. The proposed method was verified using national certified reference material GBW07167 and standard sample BY0111-1. The found results were consistent with the certified values and those obtained by national standard method. The relative standard deviation (RSD, n=12) was 0.15% and 0.09%, respectively.
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