The subject of this study is chemical functionalization as means of structural modification of multiwalled carbon nanotubes. The main goal of the experiments was to create highest density of carboxyl groups on multiwalled carbon nanotubes surface, necessary for further nanocomposite application. Two different types of multiwalled carbon nanotubes (I: outer diameter d = 50 ÷ 100 nm, purity ≈84%, synthesized by pyrolysis and II: outer diameter d = 10 ÷ 40 nm, purity ≈94%, synthesized by chemical vapor deposition) were treated by concentrated nitric acid (HNO3) and by alkaline mixture (NH4OH+H2O2). The alkaline medium as "milder" and less aggressive than nitric acid, was expected to be less destructive and cause minimal structural damage on multiwalled carbon nanotubes surface. Structural changes due to oxidation were observed by the Raman analysis, while the ratio of the intensities of the D and G peak was used to estimate the concentration of defects. Pristine and functionalized multiwalled carbon nanotubes were characterized by thermogravimetric analysis, scanning electron microscopy, ultraviolet-visible spectroscopy and zeta (ζ) spectroscopy. The results showed that functionalization initiates changes in carbon nanotubes structure as well as in their density of states. It also results in carbon nanotubes shortening and exfoliation and decreases their agglomeration tendency. Carbon nanotubes functionalized by both acid and alkaline treatment can successfully replace conventional carbon fibers as fillers in polymer composites for sensing application.