The adsorption and separation of palladium and platinum from an acidic aqueous solution were conducted using microcapsules containing a metal extractant, tri-n-octylamine hydrochloride. The spherical microcapsules with an average diameter of 208μm were prepared through encapsulation of the extractant by in situ radical polymerization of divinylbenzene. Results for the adsorption equilibrium of each metal were applied to the Langmuir adsorption isotherm model to explain the experimental results. The adsorption rate of the metals was also measured using a shallow bed reactor, and indicated that diffusion of the metal-chloro complexes through the pores in the microcapsules contributed to the overall adsorption process of the metals. Separation of the metals was conducted using a glass column packed with the microcapsules. The separation efficiency increased when the flow rate of a feed solution containing both metals was 3mL/min. Separation of the metals was almost achieved under appropriate experimental conditions during the adsorption step.