Separation of nickel from copper in ammoniacal/ammonium carbonate solution using ACORGA M5640 by selective stripping was carried out. The influence of equilibration time, equilibrium pH and extractant concentration on the extraction of both the metals was studied. It was found that the copper extraction equilibrium was reached in a shorter time than the nickel extraction equilibrium. Nickel extraction decreases above an equilibrium pH of 9.0, while the extraction of copper remains unaffected by the changes in the equilibrium pH range of 7-10. Co-extraction, ammonia scrubbing and the selective stripping of copper and nickel were performed for a solution containing 3 g/l each of copper and nickel and 60 g/l ammonium carbonate. The extraction and the percentage stripping of copper and nickel were almost quantitative.