Samples of Arundo donax were subjected to isothermal autohydrolysis, defined by temperature, 150-195 degrees C; time, 0-15 h; and liquor to solid ratio, 8 g/g. The effect of the operational variables on the yield and composition of both liquid and solid phases obtained after the treatments has been studied. The oligomer concentration and composition have been determined. In the conditions leading to maximum oligomers concentration (defined by dimensionlees time theta=1) it can be produced up to 17.7 g oligomers/100 g raw material and four acetyl groups/10 xylose monomers. These oligomers are the mean of 50% of nonvolatile compounds. In these conditions, cellulose is almost quantitatively retained in the solid phase, whereas lignin is solubilized at 9%.