Multi-walled carbon nanotubes (MWCNTs) were functionalized by different oxidative treatments to insert polar groups on their surface. The treatments included sulfuric/nitric acid mixture, 6 M nitric acid solution, concentrated hydrochloric acid, sulfuric/potassium permanganate solution, and alkaline solution. The procedures succeeded in eliminating catalyst residues remaining from the MWCNT synthesis. Physical treatment by sonication was used to modify the intertubular distances and to reduce the average particle size. The materials obtained were characterized by X-ray diffraction and their morphology was studied by TEM. Particle size was analyzed by dynamic light scattering. FTIR spectroscopy was used to confirm the presence of functional groups and thermogravimetry (TGA) was employed to estimate the oxidation degree attained. The results confirmed polar group insertion on the surface of treated carbon nanotubes. Oxidation with 6 M nitric acid followed by sonication in xylene was found to be the most effective treatment.