In this study, a new modified chemical route allowing for synthesizing carbon-supported Pt-Ti nanomaterials is presented. The effect of post-synthesis heat treatment on the physicochemical properties of the synthesized particles is described. The evolution of their size distribution, crystallographic structure, composition and electronic properties as a function of heating temperature is examined and fully described by means of scanning transmission electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy. The activity of the synthesized nanomaterials as well as their tolerance towards methanol is then investigated and fully correlated with their physicochemical properties.