Carboxylic exchange membranes were prepared from poly(vinyl chloride)/poly(methyl methacrylate-co-divinylbenzene) (PVC) [poly(MMA-co-DVB]. Transport of nickel and copper against a concentration gradient through the membrane was investigated by using a system containing NiCl2 or CuCl2 aqueous solution on the left side (L) and mixed solution of NiCl2 (or CuCl2) and HCl on the right side (R) of the membrane. It was found that nickel and copper were actively transported through the membrane from the L to the R side during the first 5 h of the experiments. The rate of transport of the ions increased with increasing H+ ion concentration on the R side and the initial concentration of the metals ions on both sides. The highest rate of transport was observed when 0.1 mol/L MeCl(2) on the L side and 0.1 mol/L MeCl(2)-0.5 mol/L HCl on the R side were used. The nickel and copper transport fractions were 34 and 24%, respectively.