The anodic voltammetric behavior of carbaryl on a boron-doped diamond electrode in aqueous solution is reported. The results, obtained by square-wave voltammetry at 0.1 mol L À1 Na 2 SO 4 and pH 6.0, allow the development of a method to determine carbaryl, without any previous step of extraction, clean-up, preconcentration or derivatization, in the range 2.5 -30.0 Â 10 À6 mol L À1, with a detection limit of 8.2 AE 0.2 mg L À1 in pure water. The analytical sensitivity of this electrochemical method diminished slightly, from 3.07 mA mmol À1 L to 2.90 mA mmol À1 L, when the electrolyte was prepared with water samples collected from two polluted points in an urban creek. In these conditions, the recovery efficiencies obtained were around 104%. The effect of other pesticides (fenthion and 4-nitrophenol) was evaluated and found to exert a negligible influence on carbaryl determination. The square-wave voltammetric data obtained for carbaryl were typical of an irreversible electrode process with mass transport control. The combination of square-wave voltammetry and diamond electrodes is an interesting and desirable alternative for analytical determinations.