Pt-TiO2 systems are the most widely used photocatalysts in the production of green hydrogen from glycerol photoreforming. To incorporate metals on the surface of materials, photodeposition is the most used method because it employs mild conditions. However, despite its use, there are some parameters that have not been deeply studied, such as the appropriate metal loading and the method itself, to obtain a better dispersion of Pt. In this work, six Pt-TiO2 catalysts were synthesized by a classical photodeposition method employing UV radiation. The studied Pt wt.% range was 0.15–0.60 wt.%, being incorporated in one step or in subsequent ones. HRTEM analyses showed that both methods allowed a homogeneous distribution of Pt, and in both, the particle size was around 2.3–3.6 nm, increasing with metal loading. The photocatalytic activity of materials was tested in glycerol photoreforming under UV radiation, and the 0.45 wt.% Pt-containing solid that had been synthesized in one step was the one that allowed the highest hydrogen production. This might suggest that around 0.40% is the appropriate metal loading for hydrogen production under these conditions and that incorporating the desired metal percentage in one step is the most efficient method in terms of energy and time savings.
