Hydrogen fuel can contribute as a masterpiece in conceiving a robust carbon-free economic puzzle if cleaner methods to produce hydrogen become technically efficient and economically viable. Organic photocatalytic materials such as conjugated microporous materials (CMPs) are potential attractive candidates for water splitting as their energy levels and optical bandgap as well as porosity are tunable through chemical synthesis. The performances of CMPs depend also on the mass transfer of reactants, intermediates and products. Here, we study the mass transfer of water (H2O and D2O), and of triethylamine used as a hole scavenger for hydrogen evolution, by means of neutron spectroscopy. We find that the stiffness of the nodes of the CMPs is correlated with an increase in trapped water, reflected by motions too slow to be quantified by quasi-elastic neutron scattering (QENS). Our study highlights that the addition of the polar sulfone group results in additional interactions between water and the CMP, as evidenced by inelastic neutron scattering (INS), leading to changes in the translational diffusion of water, as determined from the QENS measurements. No changes in triethylamine motions could be observed within CMPs from the present investigations.