Abstract: The high content lead hosted in sulfide ore is easily formed PbSO₄ precipitation with sulfur under the strong oxidizing acids, which effected the determination of Pb. This experiment established the two methods for determination of high content Pb in sulfide ore by inductively coupled plasma-atomic emission spectrometry (ICP-AES), being dissolved by aqua regia and H₂O₂ and by aqua regia after calcination at high temperature. The aqua regia-H₂O₂ decomposition method can be used to simultaneously determine Pb, Ag and Sb in samples, but calcination at high temperature-aqua regia decomposition method only can be used to determinate Pb. The two methods are both simple and fast with high accuracy and precision. The precision and accuracy of the two methods were demonstrated by analyzing reference materials GBW 07167 and GBW 07269. The RSD (n=10) of Pb for GBW 07167 were 0.38% and 0.56%, and relative error were -0.41% and 0.14%, respectively. The analytical results of Pb for reference material GBW 07269 were determinated by the same methods, whose RSD (n=10) were 0.76% and 0.66%, and relative error were 0.82% and 0.45%, respectively.