Abstract: The sample of high lead slag was dissolved with HNO3, and after filtration, the filtrate was reacted with H2SO4 to precipitate PbSO4 to separate Pb from Zn, Fe, Ca, Cu and Al. The precipitate of PbSO4 obtained was dissolved with CH3COOH and the content (w1) of Pb was determined by titration with xylenol orange as indicator and EDTA as titrant in a medium of pH 5.5-6.0. The precipitate was fused with Na2O2 and the content of Pb (w2) was determined by ICP-AES. The sum of w1 and w2 was the total content of Pb (w) in the sample.