Polyacrylonitrile (PAN), cellulose acetate (CA), PAN-TiO2, and CA-TiO(2)nanofibers were prepared using the electrospinning technique under varying the loading of the TiO(2)nanoparticles. The latter TiO(2)nanoparticles were prepared using the sol-gel method by varying the calcination temperatures. The absorption and emission spectra illustrated the formation of TiO(2)nanoparticles with an increase in absorption band edges with smaller particles. The TEM results showed the spherical morphology of the nanoparticles calcined at 500 degrees C with an average diameter of12.2 +/- 3.3 nm. XRD analysis revealed anatase phase as the dominant crystalline phase of the nanoparticles. TiO(2)nanoparticle loadings of 0.2 and 0.4 wt% were incorporated into 16 wt% CA solutions while 1, 2, and 3 wt% of TiO(2)nanoparticles were incorporated into 10 wt% PAN solutions. The SEM results illustrated the lowering in diameter and morphology of the nanofibers upon incorporation of nanoparticles. Their respective average diameters are 220, 338, 181, and 250 nm for PAN, CA, PAN-TiO2, and CA-TiO(2)polymer fibers, respectively. The morphology of the nanofibers improved while the diameter increased with an increase in polymer concentration. Different loadings of TiO(2)nanoparticles improved the electrospinnability and morphology and further decreased the size of the nanofibers. FTIR spectroscopy signifies the formation of nanocomposites and the presence of TiO(2)nanoparticles which corresponded to the Ti-O stretching and Ti-O-Ti bands on the FTIR spectra.