Abstract: The trace fluoride and chloride were separated from uranyl nitrate solution by steam distillation, determined by ion chromatography, and the separation conditions and measurement conditions were discussed in this paper. The linear range of the method is between 0.04 mg/L and 0.3 mg/L, the linear correlation coefficient is more than 0.999, the relative standard deviation is less than 10%, and the sample added recovery is between 94% and 97%.