The objective of this work was the development of reliable methods to determine 2,4-dinitrotoluene, a precursor to explosives. A complex between Fe(II) ion and 2,4-dinitrotoluene was formed in solution and characterized by ultraviolet-visible absorption spectroscopy using Job’s plots and attenuated total reflection-Fourier transform infrared spectroscopy. Surface modification of glassy carbon electrodes were performed with iron nanoparticles via electrochemical reduction of iron(II). The modified electrode was employed for the determination of 2,4-dinitrotoluene. Scanning electron micrographs showed that the iron nanoparticles were incorporated on the surface of glassy carbon electrode. The electrochemical determination of 2,4-dinitrotoluene was performed by cyclic voltammetry using the modified electrode. The iron modified electrode produced larger reduction currents than the unmodified electrode for the same concentration of 2,4-dinitrotoluene. Concentrations of 2,4-dinitrotoluene as low as 10 parts per billion were determined using the modified electrode.