One of the new technologies for water treatment is the pulsed discharge plasma method, which utilizes high voltage pulses with a fast rise time and a very short duration. In this study, under argon atmosphere at 313 K, the decoloration of methyl orange was conducted with copper (Cu) and stainless steel 304 (SUS-304) as electrodes in the batch reactor. The performance of pulse discharge plasma generation was observed using an intensified charge coupled device (ICCD) camera. The results show that the intermediate compounds from the degradation of methyl orange consist primarily of aromatic compounds containing nitrogen functional groups. At the same number of plasma discharge times, the percentage conversion of methyl orange with Cu as the electrode is higher than that with SUS as the electrode. However, the percentage degradation of methyl orange is over 90% in both cases when the number of plasma discharge times was 20000.