Abstract:A determination method of arsenic and mercury in imported copper matte by hydride generation- atomic fluorescence spectrometry (AFS) was established. The copper matte samples were digested in aqua regia and hydrofluoric acid by microwave. Then, the solution was diluted. The thiourea and ascorbic acid were added into digestion solution for prereduction Arsenic and mercury were made to form hydride by adding potassium borohydride. The contents of arsenic and mercury were determined by AFS. The results indicated that the matrix effect of Cu, Fe and S on the determination of elements was not obvious. Under the selected conditions, the detection limits were for arsenic and mercury were 0.003 9 μg/L and 0.060 8 μg/L, respectively. The recoveries of standard addition were 95 %-123 %, and the relative standard deviations (RSD, n=10) were 0.56 % and 2.0 % for arsenic and mercury, respectively. The proposed method could be used for the determination of arsenic and mercury in large quantities of copper matte samples.