Abstract: HG-AFS was applied to the determination of bismuth and antimony in molybdenum powder and products made of molybdenum. Sample was dissolved with mixture of HCl and HNO3, and hydrides of Bi and Sb were generated from HCl (10+90) solution by reacting with 15 g·L-1 and 20 g·L-1 NaBH4 solution respectively. No pre-reduction was necessary for the sample solution. Linear relationships between values of fluorescence intensity and mass concentration of Bi and Sb were found in the same range within 100 μg L-1, with detection limits (3s/k) of 0.13 and 0.03 μg·L-1 respectively. Standard samples of molybdenum oxide (YSS 003-96) were analyzed by the proposed method, results of Bi and Sb found were in consistency with the standard values. Samples of molybdenum powder and products of molybdenum were also analyzed, and tests for recovery were made on the base of these samples as matrixes, values of recovery found were in the ranges of 91.3%-95.7% for Bi and 94.0%-105.5% for Sb respectively.