In order to design reactors for heterogeneous catalytic reactions, the aspect of intraparticle moss transport resistances is of considerable relevance. An improved technique fur following the pressure change in the Wicke-Kallenbach cell was developed with the ai m of characterizing the structure of porous solids for gas transport. The experimental set-up was proposed on the basis of sensitivity analysis of the initial-boundary-value problem describing multicomponent mass transport inside porous catalyst pellets. The system parameter with the greatest influence on the sensitivity functions was the total pressure in the upper chamber of the Wicke-Kallenbach cell. A proper adjustment of experimental conditions admitted of reliable parameter estimation of the transport parameters of two porous catalysts with very different properties. The ability of the mean transport-pore model. the dusty-gas model, and the binary friction model to describe experimental responses was discussed.