To certify the oxidation reaction process (Scheme 1A), the FT-IR spectra of the hemicelluloses before and after oxidation were investigated (Figure 1). From the spectrum of DHC, the new band at 1723 cm–1, which was assigned to the C═O vibration in the aldehyde groups appeared.(38) Meanwhile, the peak at 3406 cm–1 associated with the hydroxyl group became broader, and the intensity of this peak was decreased, which was probably due to change in space steric and a decrease in hydroxyl group after the oxidation reaction. The hydroxyl groups of hemicelluloses were oxidized by periodate, and the C═O were produced during the process. The space structure of the xylose unit was changed when the hydroxyl group converted into aldehyde group. These results implied that the oxidation of hemicelluloses was prepared successfully. The reaction position of hemicelluloses was still uncertain by FT-IR analysis; therefore, the NMR spectrum was required.