The demand for cobalt has increased significantly in recent years due to its use in a wide variety of products and processes. Cobalt and nickel often accompany each other in nature and close physicochemical properties of both metals make their separation a complicated practical problem. Organophosphorous extractants have been widely used to separate cobalt from nickel. This paper presents the preliminary results obtained for separation of cobalt from nickel using Cyanex 272 containing supported liquid membranes prepared by a novel ultrasound-assisted method. The results show that this novel supported liquid membrane preparation method leads to higher separation factors than those described in the literature under similar separation conditions.