AbstractHemicellulose material is an abundant and relatively under-utilized hetero-polysaccharide material present in lignocellulosic materials. In this study, an alkaline treatment was applied to sweetgum and Eucalyptus globulus chips to extract hemicelluloses prior to kraft pulping to subsequently evaluate the final product and process. An alkaline extraction (10 and 50% NaOH by weight on wood) for 60 min at 100 °C followed by precipitation in ethanol recovered 4.3% of the biomass as a predominantly xylan material (sweetgum 50% NaOH) with an average degree of polymerization around 250 and functional groups similar to a commercial xylan (sweetgum 10% NaOH). This process in comparison to autohydrolysis (water extraction at 100 °C) produced a much higher molecular weight and more pure hemicellullose. The results obtained indicate a promising combination between the effective extraction of hemicellulose from wood and a distillation process that recovers the ethanol, which may be an attractive alternative to recover liquor and ethanol after hemicellulose precipitation. Hemicellulose from sweetgum showed more thermal stability with high molecular weight compared to the hemicellulose extracted from Eucalyptus globulus. An attractive alternative looks to be to recover liquor and ethanol after hemicellulose precipitation.