The physical and chemical characteristics of silica based materials and doped with different metals (Ni, Co and Ru) synthesized by the sol–gel method were investigated. The used techniques were: temperature programmed reduction, thermogravimetric analysis, specific surface area measurements, X-ray diffraction and Photoacoustic Spectroscopy. After calcination, higher surface areas were obtained, with the larger value for Ru–SiO2 (550m2/g), followed by Ni–SiO2 (337m2/g) and Co–SiO2 (298m2/g). For Ni–SiO2, the nickel oxide is present at the surface in two different forms. This also happens for the Co–SiO2 material, which showed two reduction peaks, probably attributed to the CoIII⇒CoII and CoII⇒Co0 reaction. However, for Ru–SiO2 only one peak reduction was observed. The X-ray diffraction data revealed the existence of an amorphous structure, while thermogravimetric analysis showed that the calcination procedure decomposes the organic residues adsorbed at the material surface.