Abstract: For high radioactivity level of dissolved solution of spent fuel and the solution of uranium product, radioactive hazard must be considered and reduced as low as possible during accurate determination of uranium. In this work automatic potentiometric titration was applied and the sample only 10 mg of uranium contained was taken in order to reduce the harm of analyzer suffered from the radioactivity. RSD<0.06%, at the same time the result can be corrected for more reliable and accurate measurement. The determination method can effectively reduce the harm of analyzer suffered from the radioactivity, and meets the requirement of reliable accurate measurement of uranium.