AbstractNowadays agricultural wastes represent an alternative source of renewable raw materials. Different processes can be applied to these alternative materials to separate their components and obtain chemical products with high added value, such as bioethanol, organic acids, monomers, and biopolymers. The main objective of this work is to study the extraction of hemicelluloses from corn stalks using different reagents [H2SO4, HNO3, HCL, CH3COOH, CF3COOH, Ca(OH)2, NaOH]. The raw material was characterized and fractionated with autoclave hydrolysis processes (121 ºC, 1:20 solid/liquid ratio, 60 min, pH = 4 or 8). Monomeric sugars concentration, TDS, MO, MI, density, and final pH of the hydrolysate were determined. Hemicelluloses were precipitated and analyzed by different techniques (FTIR, TGA and GPC). The highest yield of hemicelluloses extraction was achieved by sulphuric acid (0.98 g/L total sugar content) and the less effective reagent was Ca(OH)2 (0.52 g/L total sugar content).