Water-soluble hemicelluloses were extracted from spruce chips by heat-fractionation using microwave treatment. A screening of conditions (pH, temperature and residence time) was performed for the extraction of O-acetyl-galactoglucomannan (AcGGM). The yield and the average molecular weight of the extracted mannan were analysed using HPLC, size-exclusion chromatography (SEC) and mass-spectrometry. The pH during heat fractionation influenced the yield and the structure of AcGGM. The highest yield (78%) of AcGGM (average molecular weight 3800) was achieved with heat-fractionation in water at 190degrees C for 5 minutes. With 0.025% NaOH, an average molecular weight of 9500 was obtained at a yield of 30%. AcGGM molecular weight standard molecules were prepared using SEC. The structure of the AcGGM was determined using H-1-NMR. The enzymatic hydrolysis of AcGGM was studied using beta-mannanase and alpha-galactosidase.