Abstract：The quantitative analysis conditions of uranium content were investigated by X-ray fluorescence spectrometry combined with solution method, which provided timely and reliable data for the on-line monitoring of nuclear critical safety and guaranteed the safe production of fuel elements. The optimal current and voltage for the quantitative analysis of uranium content was 40 mA and 40 kV, respectively. The optimal measuring angle was 26.119 6°, and the PHD range was 20-70. The results indicated that the gravity of solution led to hook face at bottom of solution in liquid sample cup, which could cause the change of action scope of X-ray. As a result, some X-rays could not enter into the detector, leading to the decrease of counting. By comprehensive consideration of low limit of determination and the change of counting rate, the holding time of solution should be less than 730 s, and the sampling amount of uranium solution was 5 mL. The solution samples from six different monitoring sites were determined. The relative standard deviations (RSD, n=6) were all not more than 1.2%. The determination results of uranium content were consistent with those obtained by ferrous sulfate oxidization-potassium dichromate reduction titration method.
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