The effect of the oxidant-to-monomer (O/M) molar ratio on the morphological, magnetic, optical, and surface potential performance of polypyrrole nanofibers (PPy NFs) has been studied. The PPy NFs were prepared by chemical polymerization of pyrrole at 5°C, then the structure of nanofibers with various diameters was determined by field-emission scanning electron microscopy (FESEM). X-ray diffraction analysis and energy-dispersive x-ray spectroscopy were used to determine the composition of the PPy NFs in the prepared nanostructures. The magnetic hysteresis loop of PPy NFs showed soft ferromagnetic behavior. The surface potential of the PPy NFs was measured by Kelvin probe force microscopy, revealing that the sample with a MO:Py:FeCl 3 molar ratio equal to 1: 5.6: 4 showed excellent surface potential behavior. The H 2 S gas sensing performance of the PPy NFs thin films with each molar ratio was also tested, revealing an enhancement with increasing oxidant concentration.