Nitrogen fixation using plasma electrolysis is an alternative in the production of liquid nitrate fertilizer which is safe for the environment because it does not produce emissions that pollute the environment. The effectiveness of nitrate production is shown from the position of plasma formation at cathodic and anodic levels. This study aims to analyze the comparison of cathodic and anodic plasma electrolysis levels in producing nitrate. Current-voltage characterization is carried out to determine the position of plasma formation. The glow discharge of the cathodic plasma is achieved after the critical voltage (280 V) is lower than that of the anodic plasma (650 V). Measurement of emission intensity using electron spin resonance to determine reactive species that play a role in the formation of nitrate in cathodic and anodic plasma. Nitrate formation is influenced by reactive species in the form of N, N2*, N2+, •OH, •H and •O, especially reactive species of nitrogen and •OH are needed to form nitrate both from the NO pathway (anodic plasma) and from the ammonia pathway (cathodic plasma). The results of this study showed that anodic plasma electrolysis was more effective for nitrate synthesis. Nitrate produced from anodic plasma is 1889 mg L-1, greater than cathodic plasma as much as 213 mg L-1 © 2024 Penerbit UTM Press. All rights reserved.