Abstract: A hydride generation atomic fluorescence spectrometric method was proposed for the determination of arsenic and antimony in copper concentrate.Itis selected that the optimal condition of HG-AFS for the determination of As、Sb in copper concentrate.The method is simple and easy to operate and is also good in sensitivity and selectivity.The above method can be used to determine the content of As in the range of 0.001percent~2.5percent, Sb in the range of 0.001percent~0.5percent.