The separation of cobalt and nickel with liquid surfactant membranes (LSMs) was carried out in a stirred cell using a newly synthesized extractant. The effect of a surfactant on the kinetics of cobalt and nickel extraction was investigated to elucidate the role of a surfactant used in LSMs. The extraction equilibrium of these metals was also examined. Further, the interfacial tension between the organic and aqueous phases was measured to elucidate the adsorption equilibrium of a surfactant. It was found that the interfacial activity of the extractant is as high as that of a surfactant. In the extraction equilibrium study of these metals, extraction equilibrium constants were obtained for cobalt and nickel for the following equations : Co2+ + 2(HR)(2) = CoR(2)(HR)(2) + 2H(+) Ni2+ + 3(HR)(2) = NiR(2)2(HR)(2) + 2H(+) The effects of the extractant and surfactant on the extraction rate of cobalt and nickel in LSMs were studied. The results were analyzed by a proposed model with an interfacial reaction, and rate constants were obtained for each metal. It was found that the new extractant has a very strong extractability for each metal compared with a conventional commercial extractant such as 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (commercial name, PC-88A) or di(2-ethylhexyl)phosphoric acid (D2EHPA). Further, a surfactant strongly affected the extraction rate and the separation of these metals, and a cationic surfactant was selected.