The importance of uranium metal is growing day by day in light of its increasing global demand for fulfilling societal needs through atomic power programs. Considering the high demand for uranium, it is necessary to find innovative hydrometallurgical techniques to separate uranium from other associated elements, especially vanadium. This study deals with the separation of uranium(VI) and vanadium(V) from sulfuric acid solutions using commercial amine-based extractants diluted in kerosene. The concentrations of the sulfuric acid solutions ranged from 0.005 to 5.0 mol/L. The effect of extractant concentration ranging from 0.005 to 0.2 mol/L was studied. The temperature was maintained at 25°C and the experiment was performed for 30 min at an aqueous: organic phase ratio of 1 (A:O = 1:1). The calculated separation factors (SFs) are presented and comparisons are made among all the experiments.