An effective removal of heavy metals from and safe deposition of spent power plant fly ashes has been an on-going problem in Korea In this study, a selective separation of Ni from the leach liquor has been attempted using chemical precipitation method.Variables considered included pH of the solution and concentrations of various ions in the solution.The effect of other ions present in the system on the separation efficiency was also investigated.The Ni species with-OH and-NH3 has been also investigated.