AbstractTwo hemicellulose fractions were obtained by extraction of one-month- old young bamboo (Phyllostachys pubescens Mazel). The fractionation procedure employed 2% NaOH as extractant, followed by filtration, acidification, precipitation, and washing with 70% ethanol solution. The total yield was 26.2%, based on the pentosan content in bamboo. The physicochemical properties were determined and sugar composition analysis showed that the hemicelluloses consisted mainly of xylose, arabinose, galactose, and a small amount of uronic acid. Furthermore, based on FT-IR and NMR spectra analyses, the structure of hemicelluloses was determined to be mainly arabinoxylans linked via (1→4)-β-glycosidic bonds with branches of arabinose and 4-O-methyl-D-glucuronic acid. The molecular weights were 6387 Da and 4076 Da, corresponding to the hemicelluloses HA and HB. Finally, the thermal stability was elucidated using the TG-DTG method. The obtained results can provide important information for understanding young bamboo and the hemicelluloses in it.