The aim of this study was to optimize the production of furfural by hydrolysis with dilute acid of Eucalyptus globulus wood in two stages, using a factorial experimental design and multiple regression models to maximize furfural yields. The two-stage process could provide a solid phase with less degraded cellulose and older applications that the solid phase of a conventional acid hydrolysis. The selectivity for furfural of the process was increased by effect of the glucan and lignin fractions being efficiently removed after the first acid hydrolysis stage. The operational ranges are especially suitable for the extraction of xylose, which was virtually quantitative at 170 C and virtually independent of the operation time. It is therefore advisable to use non-isothermal conditions or short times. This is quite important if one considers the low acid concentration used. The liquid phase obtained after autohydrolysis of the raw material under the optimum conditions contained 2.3% glucose, 9.8% xylose, 2.5% xylo-oligomers, 0.6% arabinose, 1.1% furfural and 0.1% 5-OH methyl furfural. After the residual solid from the first hydrolysis stage is removed, the acid concentration is the most influential variable on the conversion of xylo-oligomers or xylose into furfural. Conversions to furfural were quite substantial (greater than 10 g/L). Hemicelluloses in the raw material were extracted by 32-57.7% and xylan by 40.5-84%. The highest conversions to furfural were obtained by using a medium operation time (15 min) and low temperature (170 degrees C) and pH = 2. The process additionally provides hemicellulose derivatives that are scarcely contaminated with cellulose derivatives. The concentrations of gluco-oligomers were very low and those of glucose in the region of 3% of the raw material. (C) 2013 Elsevier B.V. All rights reserved.