Abstract: Aiming at solving problems encountered in commercial hydrometailur-gical applications, a systematical process analysis was conducted on leaching solutions from a high grade nickel matte. Two extraction purifying processes of nickel and cobalt were experimented with Extractants 5709 and P507 and their performances were analysed, both technically and economically. Process simulation and design were based on models of extraction and stripping developed experimentally. It was concluded that the process flowsheet using Extractant 5709 appeared to be optimal. Optimal operational parameters and cost of individual unit operation were further obtained.