The properties of wood can be improved after heat-treatment. There have been many studies dealing with mechanical properties and chemical modifications of heat-treated wood. The purpose of this paper is to provide a new analysis method, to give better insights on the hemicelluloses, cellulose, and lignin contents of heat-treated wood by using Fourier transform infrared (FT-IR) and two-dimensional infrared (2D-IR) spectroscopies. The FT-IR spectra results showed progressive degradation in the carbonyl groups of the glucuronic acid units and degradation of the pyranose of hemicelluloses. These changes were measured as the percentage decrease of crystalline cellulose and the loss of C=O and C=C groups linking together the aromatic skeleton of lignin. The 2D-IR spectra showed the appearance of 5 × 5 peak clusters in the 1000 to 1200 cm-1 region, which could account for the hemicellulose degradation. In addition, changes in the degree of sensitivity at 1627 and 1509 cm-1 coincided with cross-linking reactions among the aromatic units in the lignin molecules.