Cobalt and nickel are among the most important nonferrous metals. The using of flat sheet supported liquid membranes (FSSLMs) to remove metals from wastewaters has been used actively by the scientific and industrial communities. In this study, the selective separation of cobalt from thiocyanate solutions containing cobalt and nickel by FSSLM was examined using tri-n-octylamine (Alamine 300) as carrier. The FSSLM was consisted of extractant, flat sheet support and organic solvent. The various parameters were studied to determine the optimum extraction and striping conditions of cobalt and nickel. These parameters were stirring speeds of phases, NH4SCN concentration, pH, diluent type, extractant concentration, stripping reagent concentration and modifier concentration. Concentration of cobalt and nickel were determined by Shimadzu AA-6701GF spectrophotometer. In the optimum conditions, selective separation of cobalt was achieved with an efficiency of 98.4% within 8 h, for equimolar feed mixtures, 400 mg/L Co + 400 mg/L Ni, and the separation factor of Co(II) over Ni(II) was 234.4. In addition, for nonequimolar feed mixtures, 500 mg/L Co + 1000 mg/L Ni, Ni in excess, selective separation of cobalt was 99.9%, and the separation factor of Co was 506 in the same time.