Some vic-dioximcs of imidazoline and piperazine derivatives were used in order to establish whether the determination of nickel and copper ions via potentiometric titration is possible. Additionally, the determination of Ni2+ and Cu2+ using the well known ligand dimethglglyoxime in aqueous and non-aqueous solution was carried out by titration. Some of the dioximes studied were found to be efficient. Metal solutions of 2.50 x 10(-2), 1.67 X 10(-2), 1.00 X 10(-2) and 0.50 X 10(-2) mol l(-1) were used in the experiments. The errors varied with the type of metal, ligands and concentration of the metal. Neglecting high errors, the relative error interval varied between +2.04 and -1.13.