The aim of this study was to investigate the effects of different acid catalysts and pretreatment factors on the hydrolysis of biomass compounds over a range of thermochemical pretreatments; maleic, oxalic, and sulfuric acids were each used under different pretreatment conditions. The most influential factor for fermentable sugar production in the dicarboxylic acid-pretreated mixed hardwood was pH. Reaction time was the next significant factor followed by reaction temperature. However, fermentable sugar production was more dependent on reaction temperature than time during sulfuric acid pretreatment, whereas the effect of acid concentration was considerably lower. Maleic acid pretreatment was very effective for attaining high glucose yields after enzymatic hydrolysis. The highest enzymatic hydrolysis yield was found following maleic acid pretreatment, which reached 95.56%. The trend in enzymatic hydrolysis yields that were detected concomitantly with pretreatment condition or type of acid catalyst was closely related to xylose production in the hydrolysate. Crown Copyright (C) 2012 Published by Elsevier Ltd. All rights reserved.