Conditions have been developed for the simultaneous determination of copper(II) and nickel(II) in mixtures using ammoniacal dimethylglyoxime solution as a reagent. The Beer's law ranges for copper(II) and nickel(II) are 5.1-91.6 and 0.2-2.5 μg/mL at 590 nm and 440 nm respectively. The molar absorptivity is 2.42 × 102 1. mol-1 cm-1for copper(II) at 590 nm and 1.44 × 104 1. mol-1 cm-1 for nickel(II) at 440 nm. Effect of diverse ions has been studied. The method is applied successfully in some alloys as well as in synthetic mixtures.