The separation of copper (II) and nickel (II) was investigated by a surfactantgel extraction method. In the presence of nitrilotriacetic acid (H3NTA), by the addition of potassium ethylxanthate (KEtX) to solutions including copper (II) and nickel (II), nickel (II) remained as NTA complex in aqueous phase while copper (II) was extracted as EtX complex into a surfactant phase of sodium dodecylsulfate (SDS) . This method was applied to the separation and recovery of metals in an alloy consisting of 30 % copper, 66 % nickel, 1.9 % iron and 1.6 % manganese. Extracted copper complex was decomposed by the addition of hydrochloric acid. Copper was back-extracted from the SDS phase and was recovered in aqueous solution. The bromine water was added to the separated aqueous phase in which nickel, iron and manganese remained. Iron and manganese was excluded from the solution as precipitates by the oxidation with bromine.