In this study, Pt (of 0.3, 0.6 and 0.9 wt % loadings) was supported on mesoporous silica surface via microwave-assisted solution (MAS) method or rotary chemical evaporation (RCE) method in the in situ reduction step. The as-synthesized Pt nanocatalysts were characterized through XRD, XRF, TGA/ DSC, TEM, N 2 -adsorption-desorption, H 2 -pulse titration and electrical conductivity techniques. The samples prepared by MAS method exhibited higher surface area and a better dispersion profile of Pt NPs, of average sizes not exceeding 10 nm with increasing the Pt loading. In contrast, although RCE method showed higher efficacy in decomposing the used precursor, uneven distribution of larger Pt nanoparticles (≥ 33 nm) was displayed. Electrical properties in terms of AC conductivity and dielectric constant confirmed the enhancement of even distribution of smaller Pt NPs with higher concentration of grain boundaries affected by microwave electromagnetic radiations. Highly mobile electrons and lattice vibrations (phonons) were favored, as compared with aggregated NPs produced during RCE method. The TOF values calculated for reactions to selectively produce ethylene (from ethanol) or benzene (from cyclohexane) decreased with Pt loadings on catalyst samples synthesized by MAS method. The highly dispersed NPs (of 3-7 nm) seemed to be responsible of the activity in both reactions, tending probably to be structure insensitive. However, samples reduced by RCE method, with enlarged average sizes of surface Pt NPs (approaching 15.5 nm), exhibited increasing TOF values with Pt loading, i.e., turning the reactions most probably to be structure sensitive.