Alumina nanofibers containing either platinum or rhodium crystalline nanoparticles have been successfully fabricated by electrospinning a solution of polyvinylpyrrolidone mixed with platinum or rhodium chloride and subsequent calcination and hydrogen reduction. Transmission electron microscopy images indicate that the platinum and rhodium nanoparticles are well dispersed on the electrospun alumina nanofibers. X-ray diffraction results demonstrate that the platinum and rhodium nanoparticles are crystalline, while the alumina matrix is amorphous. Furthermore, X-ray photoelectron spectroscopy was used to investigate the chemical nature of these nanofibers containing noble metals before and after calcination and hydrogen processing.