Abstract:A method was established for the determination of lead in copper flash smelting dust by EDTA complexometric titration after the precipitation of lead sulfate formed by sulfuric acid was separated. The sample was dissolved with hydrochloric acid, nitric acid, sulfuric acid, ammonium bifluoride and perchloric acid, lead precipitated with sulfuric acid was separated from other interfering elements, the precipitate was dissolved in acetic acid-sodium acetate buffer solution, bismuth was masked with mercaptoacetic acid, iron was masked with ascorbic acid, xylenol orange was used as indicator, lead content in the solution was titrated with Na2EDTA standard titration solution, and lead content in the filtrate was determined by flame atomic absorption spectrometry to correct it. The experimental results showed that the addition of sulfuric acid (1+24) was 50mL, anhydrous ethanol was 10mL, and acetic acid-sodium acetate buffer solution was 30mL. The relative standard deviation (RSD) of this method is between 0.35 and 1.52, and the recovery rate of standard addition is between 99.0% ~ 101.3%. It fully meets the requirements of production control analysis and can also be used as a reference method for lead analysis in similar materials.