Adouble channel hydride atomic fluoresence spectrometric method for simultaneous determination of trace arsenic and antimony in geochemical samples is described in this paper. In this procedure potassium borohydride is used as reductive agent, and the hydrides of arsenic and antimony produced are then introduced into a electrothermal silica tube "atomizer for determination. The detection limit for arsenic and antimony are 1.4 × 10^-9 g and 3.7+10^-10g. respectively.The procedure has been applied to analysis of standard-reference samples of stream sediments GSD1-8, developed by the Ministry of Geology and Mineral Resources for Geochemical survey and DSG Sreference samples for geochemical exploration GXR1-6, and a faily good agreement is bobtained bebween our determinations and the published data.The method is characterized by its simplicity, its speed of determination, as well as its high sensitivity and accuracy.