A sulfuric acid-free ethanol cooking (SFEC) treatment was developed to achieve complete saccharification of the Cellulosic component of eucalyptus and baggase flour, thereby avoiding the problems associated with the use of strong acid Catalysts. Cutter-milled flours were exposed to an ethanol (EtOH)/water/acetic acid mixture in an autoclave. Enzymatic hydrolysis experiments of the pretreated samples demonstrated that almost complete conversion of the cellulosic components to glucose was achieved under optimal conditions. A large-scale trial revealed that there was little consumption of in-feed EtOH during SFEC: therefore, it is considered that most part EtOH used can be essentially recovered and reused. Field emission scanning electron microscopy showed that SFEC induced the formation of pores ranging in size from approximately 10 to several 100 nm. It can be assumed that the porous surface was due to the partial removals of lignin and hemicellulose. which improved the accessibility of the enzyme onto the substrate. (C) 2008 Elsevier Ltd. All rights reserved.