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Local production of agricultural waste is increasing. It is not fully utilized and can cause an environmental issue if it is not handle wisely. Thus, it is important to increase utilization of lignocellulosic biomass by improving their added value and subsequently decrease the agriculture waste. In this study, rice straw and Leucaena leucocephala were subjected to alkali treatment (4% sodium hydroxide) such with different concentration ratio of sampel to sodium hydroxide (1:10 to 1:50). The physical and chemical properties of extracted hemicelluloses were studied. The yield of hemicellulose was higher from rice straw compared to Leucaena l.. The chemical functional groups present in hemicellulose were confirmed by Fourier tranform infrared spectroscopy (FTIR). The surface morphology and roughnesses of xylan were examined by scanning electron microscopy (SEM).