Accurate calculation of conversion yields during biomass processing requires precise compositional information on the native and/or pretreated biomass feedstock. A two-stage acid hydrolysis step is used as part of the standard compositional analysis procedure to determine carbohydrate content of these materials. In the first stage, the samples are suspended in 72% (w/w) sulfuric acid and held at 30^oC for one hour. Then the samples are diluted to 4% acid (w/w) and autoclaved at 121^oC for an hour. This procedure is both time-intensive and results in degradation of some of the sugars solubilized during hydrolysis. Microwave digestion was investigated as an alternative to the conventional autoclave method for its potential to decrease sample preparation time and reduce the degradation of free monosaccharides. The latter outcome is expected to improve the accuracy of carbohydrate analysis in biomass samples.