A method for the determination of trace arsenic and mercury in antimony concentrates by hydride generation atomic fluorescence spectrometry was investigated. The method of dissolving sample and the effect of concomitant ion were studied. It was found that aqua regia can be used to dissolve the sample completely, with maximum quantities of dissolved arsenic and mercury. The interference of chemical elements in antimony concentrates was avoided by adding thiourea-Vc. The matrix of antimony was vaporized with tartaric acid during sample pre-treatment. Trace arsenic and mercury were determined in real samples. The detection limits of 0.220 ng x mL(-1) and 0.002 ng x mL(-1) were obtained, the relative standard deviations(RSD% = 11) are 1.47% and 0.52%, and the recoveries are 94.0%-103.0% and 98.7%-102.8% for As and Hg respectively. This method has proved rapid, accurate and highly sensitive.