Abstract: Samples of sheepskin shoes were treated by extraction with artificial sweat (method 1#) and microwave digestion with HNO3 (method 1#) separately, and the contents of Hg and As in the sample solutions were determined by HG-AFS with 20 g·L-1 KBH4 as reducing reagent and HCl (5+95) solution as carrying solution. It was found that precision and recovery of the method obtained by the two pretreatment methods were all satisfactory. Linear relationships between values of absorbance and mass concentration of Hg and As were kept in definite ranges, with detection limits (3S/N) of 0.001 0 and 0.005 7 μg·L-1 (method 1#) and 0.000 8 and 0.005 3 μg·L-1 (method 2#)) respectively. The proposed method was applied to the analysis of sample of sheepskin shoes and recovery was tested by standard addition method values of recovery found were in ranges of 93.5%-99.2% for Hg and 91.9%-102% for As. Values of RSD′s (n=5) were found in ranges of 1.1%-4.3% for Hg and 1.0%-4.5% for As.