An ion exchange method has been developed to separate no-carrier-added Cu-64 from irradiated Ni target. The target is first dissolved in nitric acid and the solution is evaporated to dryness and the residue is dissolved in an ethanol-HCl solution. Cu, Co and Ni in ethanol-HCl solution are then absorbed on an anion exchange column. Co and Ni are removed from the column by eluting with 72% ethanol-0.3mol/l HCl. Finally, the Cu-64 is eluted with water. For separating Ni from Co isotopes and recovering the Ni-64 target, the eluate of 72% ethanol-0.3 mol/l HCl is evaporated to dryness, the residue is dissolved in a concentrated HCl solution, and loaded to an another column, Ni is eluted by 9 mol/l HCl, while Co remains on the column. The procedure developed has been successfully applied for the production of no-carrier-added Cu-64 from enriched Ni-64 generated by the reaction Ni-64(p, n)Cu-64 using a cyclotron. The decontamination of Co in Cu fraction is higher than 99% and recoveries of Cu-64 and Ni-64 are higher than 95%. (C) 2002 Elsevier Science Ltd. All rights reserved.