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A new technique for sensing nanomolar concentrations of hydrazine in water samples is reported. A screen-printed carbon electrode (SPCE) altered using an amine-azo functional group encompassing poly(dicyandiamide) is used in this study. The modified electrode exhibits an enhanced activity toward hydrazine detection at a lower overpotential and broad linear scale between 20 nM and 1 mM, with an accurate sensitivity value of 0.1 nA μm–1 cm–2. To the best of our knowledge, poly(dicyandiamide)-modified electrodes exhibit one of the lowest limits of detection for any metal-free electrode that detects 6.7 nM (S/N = 3) of hydrazine. The method established sufficient selectivity and better recoveries. Finally, the poly(dicyandiamide)-modified SPCE* is highly suitable for electrochemical determination of hydrazine in water samples from tap and lake.