An experimental set-up was developed to measure the mass diffusion kinetics in adsorbents. The mass and the temperature of a sample are measured simultaneously during a pressure step. The temperature is measured by an IR detector which yields very precise and very fast measurements without perturbation of the system. The kinetics parameters are identified by a numerical model. A qualitative approach permits mass diffusion effects to be separated from thermal relaxation, and a typical result obtained for NaX zeolite pellets in the presence of water vapour is presented.