The objective of this work was to investigate the feasibility of acid-catalyzed hydrothermal fractionation for maximum solubilization of the hemicellulosic portion of two typical agricultural residues. The fractionation conditions converted into combined reaction severity (CS) in the range of 1.2-2.9 was used to establish a simple reaction criteria at glance. The hemicellulosic sugar yield of 56.6% was shown when rice straw was fractionated at the conditions at the conditions; 160℃ of temperature 0.75% (w/v) of H2SO4, 20 min of reaction time, 1:15 solid/liquid ratio. The hemicellulosic sugar yield of 83.0%, however, was achieved when barley straw was fractionated at the conditions at the conditions; 150℃ of temperature 0.75% (w/v) of H2SO4, and 15 min of reaction time, 1:10 solid/liquid ratio. For barley straw, acid-catalyzed hydrothermal fractionation could be effectively performed. After the fractionation process, the remaining fractionated solids were 48.5% and 57.5% from raw rice and barley straws, respectively. The XMG contents in the solid residues decreased from 17.3% and 17.6% to 6.0% and 2.6%, which corresponded to 16.7% and 8.5% on the basis of the raw straws, respectively. In another way, only 5.6% of cellulose and 8.5% of XMG were lost due to excessive decomposition during the acid-catalyzed hydrothermal fractionation of barley straw, compared to cellulose and XMG losses of 6.4% and 26.6% in rice straw. Hemicellulosic sugars from the rice straw were considered more overdecomposed due to the somewhat higher reaction severity at the acid-catalyzed hydrothermal fractionation.