In the last few years functionalised carbon nanotubes and carbon nanofibers have shown promising results in the area of heterogeneous catalysis due to the ability to tune the electronic, mechanical, thermal and adsorption properties and therefore affect surface area, porosity, conductivity, acidic/basic properties and metal-support interactions.The objective of this proposal is to spectroscopically identify the nature of surface functional groups formed before and after the oxidative treatment followed or not by NH3 at high temperature of the carbon nanofibers and their interaction with metal nanoparticles deposited onto the carbon materials. The synthesised metal supported nanoparticles showed significant differences in catalytic performance in terms of activity and selectivity in the liquid phase oxidation of polyols (e.g. glycerol).