Abstract: The contrast of the roasting methods of stibnite ore samples showed that the use of low-temperature calcination of the sample to remove sulfur, with high-temperature roasting of the sample, afterwards can dissolve gold completely by aqua regia，without the lump of the ore sample. The method has been applied to the determination of Au in the National Standard Reference materials and the results are in agreement with certified values with precision of 1.44%~4.79% (RSD,n=5) .The recovery of the method was 95.5%~104.3%. The method is rapid and accurate,and is applicable to the bulk sample analysis of gold in stibnite.