Recently, the demands for separation/recovery of valuable metals such as nickel or tin from copper based alloys has been attracting much attention from the viewpoints of environmental protection and resource utilization. In this report, experimental results on concentration increasement of nickel and tin compared to the previous report are investigated. Ni is successfully separated by a organic solvent and reduced to the metal powder whose concentration is over 98 %. Sn is separated by a selective solution method and its concentration is increased to 97.5 % by three consecutive solution and reduction process. Crystal structure, surface morphology and microstructure of the separated samples are studied.