An adsorptive separation of rhenium and rhodium was performed by using a jacketed glass column packed with an extractant impregnated resin (EIR). The EIR bed showed a successful separation of rhenium and rhodium with about 122 BV of a breakthrough volume. The breakthrough behavior in the column was modeled to assess the mass transfer resistances in the column. The model predicted the column dynamics for rhenium quite well by assuming a homogeneous diffusion in the particle phase. The effective diffusivities of rhenium were in the order of 10.7 cm2/min. The EIR loaded beds could be eluted with a high purity of more than 99% by using a nitric acid solution.