Abstract: Hydride generation-atomic fluorescence spectrometry was applied to the determination of arsenic in yellow phosphorus. Optimum condition of sample digestion,working condition of the instrument and suitable concentration of reductant were studied. Under the tested conditions of analysis,linear relationship between the fluorescence intensity and concentration of arsenic was found in the range from 0.06 to 10.0 μg·L-1 (r=0.999 4),with a detection limit of 0.03 μg·L-1. Five samples of yellow phosphorus were analyzed by the proposed method,giving values of RSD less than 3.5%. Recovery was tested and the results obtained were in the range of 93.8%-103.6%.