AbstractHemicellulosic fractions were extracted from soybean hull with various concentrations of NaOH at 50 °C for 5 h. The chemical compositions and physicochemical properties were determined by high performance anion exchange chromatography (HPAEC), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analyzer (TGA), and 13C and 2D nuclear magnetic resonance (NMR) analysis. The crystallinity of soybean hulls treated and untreated by alkali liquid was examined by X-ray diffraction (XRD). The sugar analysis results indicated that all of the hemicellulosic preparations were heteropolysaccharides containing arabinose, galactose, glucose, xylose, and mannose. According to the spectral analysis, hemicelluloses from soybean hull were assumed to be L-arabino-4-O-methyl-D-glucurono-D-xylan. Xylose was the predominant monosaccharide in the hemicellulose fraction 1 (H1), and it ranged between 40.1% and 48.8% of the total neutral sugars. It was found that hemicellulose fraction 3 (H3) had the highest thermal stability and H1 had the lowest thermal stability. The crystallinity index (CrI) was found to be about 20.8%, 14.3%, 10.9%, and 4.7% for soybean hulls, untreated and treated with 1.5, 2.0, and 2.5 M NaOH, respectively.