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A sensitive voltammetric method is developed for the determination of diazinon, an organophosphorus pesticide, using a Nafion®-coated glassy carbon electrode as an enrichment film. The analysis of diazinon in aqueous solutions using sensitive instrumental methods has gained importance. Investigation of the electrochemical behavior of diazinon on a Nafion®-coated glassy carbon electrode reveals the presence of a specific oxidation peak of analytical significance. The experimental parameters, such as pH, film thickness, preconcentration potential, preconcentration time, and square-wave voltammetric parameters were optimized. Using this method, a linear calibration curve for diazinon was obtained up to 5 μM range in pH 1 citrate buffer solution with a detection limit (S/N = 3) of 75 nM.