Interest of this study is to develop classical macroscopic diffusion measurements to probe and allow distinguishing a true hierarchical material from the other material. To this aim, the AGIR methodology (Analysis by Gravimetry and IR spectroscopy) will be used Gravimetric measurements provide more classical approach to molecular uptake measurements, whereas infrared (IR) spectroscopy can provide additional data on the interaction, orientation and environment of the molecules on the solid surfaces. In this study we evaluated the mass transport properties in a mechanical mixture of hierarchical H-MFI and H-FAU zeolites. Using AGIR technique, we have been able to distinguish the diffusivity of each component present in the mechanical mixture of following pure zeolites: H-MFI and H-FAU respectively. The potential and limitations of this new methodology will be discussed.