Pristine and fluorinated multi-walled carbon nanotubes (MWCNTs) and single-walled carbon nanotubes (SWCNTs) were characterized using energy dispersive X-ray spectra (EDX) and X-ray photoelectron spectroscopy (XPS), respectively. The fluorine percentages of fluorinated multi-walled carbon nanotubes (F-MWCNTs) and fluorinated single-walled carbon nanotubes (F-SWCNTs) were 10.42% and 9.67% respectively by EDX. The absorption and de-absorption of fluorine properties were studied using high resolution C 1s and F 1s core level XPS and valence band spectra. The fluorine can be completely dissociated from F-MWCNTs, but partially dissociated from SWCNTs. There was 5.79% fluorine in atomic percent remaining associated with the F-SWCNTs when annealing the nanotubes to 500 °C measured by EDX. The results of F 1s core level XPS indicated that the binding energy of fluorine associated on SWCNTs was shifted from 687.0 eV to 688.3 eV after annealing the nanotubes to 500 °C. The results of valence band spectra showed that the binding energy of F 2p and F 2s shifted from 7.5 eV and 31.0 eV to 8.8 eV and 32.5 eV respectively in SWCNTS. However, the two peaks disappeared in annealed MWCNTs.