Abstract:A determination method of inorganic arsenic in coal was established by sequence injection hydride generation-atomic fluorescence spectrometry (HG-AFS), after the ultrasonic extraction with 6 mol/L HCl as extraction reagent. The ultrasonic extraction conditions were optimized, including extraction reagent, time and temperature. Under the optimized experimental condition, arsenic in concentration range of 0.20-100 μg/L showed linearity to the fluorescence intensity with correlation coefficient of 0.999 7. The detection limit of arsenic was 0.025 μg/L. The relative standard deviation (RSD) for 10 μg/L As was 0.9 % (n=11). The proposed method has been applied to the analysis of coal fly ash component analysis certified reference material (GBW08401) and coal samples with recoveries of 95%-102 %, and the result of GBW08401 was consist with the certified value.