Furfural, a valuable platform chemical that has the potential to replace a variety of oil/coal/gas derived materials and chemical products, is produced by the dehydration of o-xylose, which in turn is obtained from lignocellulosic biomass. Herein, the conversion of xylose in the presence of nanocrystalline zeolite beta in the H+-form, using water as solvent, was investigated. Detailed batch kinetic studies and products identifications techniques (H-1, C-13 NMR and comprehensive two-dimensional gas chromatography (GC x GC) combined with time-of-flight mass spectrometry (ToFMS)) provided mechanistic insights into the overall reaction process. The conversion of xylose to furfural is accompanied by several side reactions, forming complex reaction mixtures. A pseudo-homogeneous kinetic model was proposed that fitted quite well the experimental data. (C) 2012 Elsevier B.V. All rights reserved.