In general, separating osmium and ruthenium metals via hydrometallurgical methods poses significant challenges. This study presents a novel approach to separate osmium from a metallic mixture with ruthenium through selective dissolution using a two phase system. The system comprises an aqueous phase containing sulfuric acid solution with sodium chlorate and an organic phase consisting of pure tributyl phosphate. Among the several variables investigated in this work, sulfuric acid concentration and stirring speed showed most significant effect on the dissolution of osmium metal. Based on the potential pH diagram of osmium metal, an oxidation reaction of osmium metal by the sulfuric acid and sodium chlorate mixture was proposed. The role of tributyl phosphate was to prevent the evaporation of the dissolved osmium tetroxide species by extracting into organic phase. The separation of the two metals was accomplished by selective dissolution of osmium at the following conditions: 3 M sulfuric acid, 0.7 M sodium chlorate, pure tributyl phosphate, pulp density of 2 g/L, 20°C, 60minutes and stirring speed of 200 rpm. Use of a mixture of thiourea and hydrochloric acid solution containing ascorbic acid completely stripped the osmium fromtheloadedtributyl phosphate. Comparison of dissolution efficiency of osmium metal between two phase system and one phasesystem ofsulfuric acid-sodium chlorate-water indicated that the employment of tributyl phosphate in two phase system was of importance in the recovery of the dissolved osmium species. Our results demonstrated that osmium can be separated from ruthenium by selective dissolution with the two phase system.