This paper describes the development of a simple voltammetric method for the measurement of 2,4-dinitrotoluene (24DNT) at glassy carbon electrode (GCE). Initial investigations were undertaken using cyclic voltammetry to characterise the redox behaviour of 24DNT. Over the pH range 2 to 10 two pH dependent reduction peaks were recorded on the initial negative going scan, concluded to result from the reduction of the two nitro groups to the corresponding hydroxylamines. On the return positive going scan two oxidation peaks were recorded, resulting from the oxidation of the hydroxylamine (O1) formed on the initial negative scan. At pH 6, the peak potential of the oxidation process O1 occurred at a potential close to 0 V and was chosen for investigation. The optimum voltammetric conditions required were identified to be supporting electrolyte of 0.1 M pH 6.0 phosphate buffer containing 10 % acetonitrile. Using differential pulse voltammetry, the calibration plot was found to be linear from 5.0 µM to 500 µM (R2= 0.9979), with a detection limit of 11.0 µM (based on a signal-to-noise ratio of 3).