Abstract: An energy dispersive X-ray fluorescence spectrometry with ~(109)Cd isotopic exciting source and S (Li) detector are used to analyse uranium in the high-level liquid waste. Film technique is used for preparation of the measured source. For the elimination of effect of radiation on Si (Li) detector, the dead time must be corrected in measurement. After the initial sample is dilluted to measurable range, uranium is analysed by external standard method. The precision of the method is better than 3％. The recovery of U is (101—107)％ with 10 μg uranium added to the sample.