This paper presents a simple, rapid and sensitive radiometric method for the determination of uranium in Thorex Process stream containing large amount of thorium. This method involves the extraction of uranium into 0.05M tri-n-octyl phosphine oxide (TOPO) in xylene at 2M HNO₃. The extraction of thorium is prevented by masking them with suitable quantity of fluoride ions. The optimum experimental parameters for extraction of ²³³U were evaluated and using the most suitable experimental conditions the extracted uranium is radiometrically determined by α-counting in proportional counter with a prior knowledge of specific activity of uranium. Simultaneously in the same sample uranium was determined by spectrophotometric method using 2-(5bromo-2 pyridylazo)-5-diethylaminophenol (Bromo-PADAP) as chromogenic reagents. Simulated as well as actual samples of dissolver, conditioner and raffinate tank of Thorex stream have been analyzed by both these methods. The method was tested for as low as 0.15 μg of uranium and the results of these analyses were found to be satisfactory within the experimental limits.