The application of cupferron as a complexing agent for a simultaneous voltammetric determination of U(VI) and Cd(II) in a single scan in environmental water samples has been developed. Optimal conditions were found to be: 0.05 mol L−1 acetate buffer (pH 5.3) as a supporting electrolyte, 1×10−3 mol L−1 cupferron, the accumulation potential −0.25 V, the accumulation time 30 s. The linear range of uranium(VI) and cadmium(II) were observed over the concentration range from 1×10−8 mol L−1 to 5×10−7 mol L−1 and from 2.5×10−9 mol L−1 to 2×10−7 mol L−1, respectively. The procedure was applied to the determination in natural water samples.