Jordanian corn leaf waste was characterized by ultimate and proximate analysis, TGA, FTIR and solid state 13C NMR. The waste showed high volatile matter, high atomic H/C ratio and high O content. The corn leaf waste contained 32.1 wt% cellulose, 18.1 wt% hemicelluloses and 11.9 wt% lignin.. Higher oil yield was obtained at pyrolysis temperature of 450 °C. The gas yield and higher heating value of the product increased as the temperature increased, whereas the water content decreased. The biofuels were rich in carbon and had a high oxygen content, which decreased as the temperature increased. The 1H NMR confirmed the markedly aliphatic character of the biofuel. The GC-MS for the biofuel indicated the presence of hydrocarbon series, large amounts of oxygenated compounds and a few nitrogen and sulfur compounds. The simulated distillation showed a high proportion of diesel fraction (57–73%).