Abstract：The coal fly ash was a kind of valuable uranium resource. The comprehensive recovery and use of uranium in coal fly ash must be strengthened in order to meet the increasing demands of uranium in nuclear power industry. Therefore, the accurate determination of uranium content in coal fly ash was of great significance. The sample was treated by microwave digestion in nitric acid-hydrofluoric acid-perchloric acid system. An accurate and rapid determination method of uranium in coal fly ash by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion was established with 187Re as the internal standard element and 238U as the determination isotope. The sample dissolution conditions were optimized. The acid dosage was selected as follows: 5.0mL of nitric acid, 3.0mL of hydrofluoric acid and 0.50mL of perchloric acid. The digestion procedures were listed as follows: the digestion power was 800W; the temperature was increased from room temperature to 150℃ in 15min and kept for 10min; then the temperature was increased from 150℃ to 200℃ in 15min and kept for 30min. The experimental results showed that the mass concentration of uranium in range of 0.5-20ng/mL was linear to its corresponding signal intensity with linear correlation coefficient of 0.9999. The detection limit of method was 0.05μg/g. The proposed method was applied for the analysis of coal fly ash actual sample. The relative standard deviation (RSD, n=6) of the results was 3.2%. The spiked recoveries were between 95% and 104%. Various coal fly ash samples from different coal-fired power plants were determined according to the experimental method. The found results were basically consistent with those obtained by laser fluorescence method
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