The paper describes an analytical method whereby the chemical composition of the polysaccharide fraction of woody materials, including the uronic acids and carbohydrate acid degradation products, can be completely determined. Sealed vessels, termed bombs, are used during the high temperature acid hydrolysis of the materials to retain volatile constituents that would otherwise be lost. High-Performance Liquid Chromatography (HPLC) is used for all of the analyses. The sample preparation procedures are simple and easily adopted into a routine. To demonstrate the reproducibility of the method, triplicate samples of Quaking aspen (Populus tremuloides) and White fir (Abies concolor) were analyzed. No significant peaks in the chromatograms were left unidentified.