In this paper a sensitive and rapid method for the determination of lead in antimony and antimony compounds by HG AFS is developed. The matrix of antimony is vaporized with hydrobromic acid during sample pre treatment. The detection limit of this method for lead is less than 1×10 -6 . The precision for the samples with w (Pb)=0.045×10 -2 is better than 2.0% RSD ( n =4). The recovery of the method is 95%~105%. The method has been applied to the determination of trace lead in antimony and antimony products. The analytical results are in agreement with those from AAS analysis.