In continuation of our research on carbon nanotube/P(VDF-TrFE) nano-composites [1], total x-ray fluorescence (TXRF) is engaged in a novel characterization of these materials regarding their compositions, purities, and structural analysis. Samples such as single-walled carbon nanotubes (SWCNT), multi-walled carbon nanotubes (MWCNT), P(VDF-TrFE) copolymer, SWCNT/P(VDF-TrFE), and MWCNT/P(VDF-TrFE) were analyzed by TXRF. The synthetic quartz used as a substrate was analyzed as reference material for the TXRF measurements. The ethanol and the dimethylformamide (DMF) used as solvents for carbon nanotubes and copolymers respectively were also analyzed by TXRF to determine whether they have an influence or not on the TXRF of the previous material. The preliminary results showed that single-walled and multi-walled carbon nanotubes prepared by the arc-discharge method contain catalytic particles such as Fe, Co, and Ni used to obtain SWCNT while there were no metal or impurities in MWCNT. The TXRF spectrum of CNT/P(VDFTrFE) showed the same results as we found previously with background due to the P(VDF-TrFE) copolymer scattered signal.