The prolysis of cellulose, hemicelluloses, lignin preparations, and wood was studied by differential calorimetric analysis (DCA) for the range of 25° to 800° C. The test samples included powdered and filter paper celluloses; hardwood xylan; softwood galactoglucomannans, compression wood galactan, and arabinogalactan; a synthetic (DHP), sulfuric acid, Bjorkman, Brownell, and cellulase lignins; and unextracted and extracted hardwoods and softwoods. Heats of reaction were determined from the DCA thermal transition areas. Distinct differences were found between the thermograms of each hemicellulose and lignin sample. Although wood species could not be separated thermally, hardwood and softwood thermograms differed because of the hemicellulose degradation pattern.