Measurements of diffusion and partitioning of nearly monodisperse polystyrene, having molecular weights of from 600 to 670,000, in chloro‐form and dichloroethane and of two proteins in aqueous solution were made with leached borosilicate glass cubes having a narrow pore size distribution and pore radi of from 2.5 to 47.6 nm. With increasing ratio of molecular to pore size, the partition coefficient for all solutes decreased; the ratio of effective to bulk diffusivity decreased for the proteins but remained constant for polystyrene. This suggests that polystyrene behaved like a free‐draining macromolecule under the conditions of this study.