The diffusion and partition coefficients of polyurethane foam (PUF) are estimated using a microbalance experiment and small chamber test. The microbalance is used to measure sorption/desorption kinetics and equilibrium data. When the diffusion condition is controlled in the chamber of the sample, interactions between volatile organic compounds (VOCs) and PUF can lead to the estimation of a relatively homogenous rate of mass transfer in the interiors and surfaces of PUF. The estimates of the material/air partition coefficient (K) and the material-phase diffusion coefficient (D) are shown to be independent of the concentrations of VOCs. This approach, if applied to a diffusion-controlled or physically-based model, can facilitate more precise prediction of their source/sink behavior. Although further research and more rigorous validation is needed, an emission model applied with the diffusion and partition coefficients from this research holds promise for the improvement of reliability in predicting the behavior of VOCs emitted from porous building materials by D and K.