An effective process for the chemical-biotechnological utilization of Eucalyptus globulus wood is reported. In a first stage, a treatment with catalysed acetic acid solutions allowed the solubilization of both lignin and hemicelluloses, leaving cellulose as solid residue. A subsequent swelling treatment with NH4OH solutions caused structural modifications to the cellulosic fraction, giving a substrate highly susceptible to the enzymic hydrolysis. A centered, incomplete, factorial design of experiments was carried out in order to establish the inter-relationships between three selected operational variables (NH4OH concentration used in the chemical treatment and both liquid/solid and enzyme/substrate ratios employed in the hydrolysis step) on the kinetics and yields of enzymatic hydrolysis. From experimental data, generalized kinetic models giving the influence of the operational variables on the hydrolysis stage were developed. Further discussion on relevant aspects involved in the process is provided.