The sequential co-production of bioethanol and biodiesel from spent coffee grounds was investigated. The direct conversion of bioethanol from spent coffee grounds was not found to be a desirable option because of the relatively slow enzymatic saccharification behavior in the presence of triglycerides and the free fatty acids (FFAs) found to exist in the raw materials. Similarly, the direct transformation of the spent coffee grounds into ethanol without first extracting lipids was not found to be a feasible alternative. However, the crude lipids extracted from the spent coffee grounds were themselves converted into fatty acid methyl ester (FAME) and fatty acid ethyl ester (FAEE) via the non-catalytic biodiesel transesterification reaction. The yields of bioethanol and biodiesel were 0.46 g g(-1) and 97.5 +/- 0.5%, which were calculated based on consumed sugar and lipids extracted from spent coffee grounds respectively. Thus, this study clearly validated our theory that spent coffee grounds could be a strong candidate for the production of bioethanol and biodiesel. (C) 2013 Elsevier Ltd. All rights reserved.