Abstract: A method for determination of selenium and tellurium in polymetallic minerals by hydride-generation atomic fluorescence spectrophotometry was developed. The samples were decomposed with HNO3-HF-HClO4. In 6 mol/L HCl media and using Fe3+ as relieving reagent, selenium and tellurium in the sample solutions were directly determined by double channel atomic fluorescence spectrophotometer. The detection limits of the method were 0.032 μg/g for selenium and 0.023 μg/g for tellurium. The method has been applied to the determination of selenium and tellurium in National Standard Reference materials and the results are in agreement with certified values with precision of less than 4.0%RSD for selenium and less than 7.0%RSD for tellurium (n=8). The method also provides the advantages of easy sample pretreatment, is more efficient and suitable for determination of selenium and tellurium in polymetallic minerals.