Tin dioxide nanoparticles are prepared using a newly developed synthesis method of plasma-assisted electrolysis. A high voltage is applied to the tin metal plate to apply a high pressure and temperature to the synthesized oxide layer on the metal surface, producing nanoparticles in a low concentration of sulfuric acid. The particle size, morphology, and size distribution is controlled by the concentration of electrolytes and frequency of the power supply. The as-prepared powder of tin dioxide nanoparticles is used to fabricate a gas sensor to investigate the potential application. The particle-based gas sensor exhibits a short response and recovery time. There is sensitivity to the reduction gas for the gas flowing at rates of 50, 250, and 500 ppm of H2S gas.