AbstractIn the present study, coconut husk was employed as biomass feedstock for production of bioethanol, due to its abundance in Malaysia. Due to the complex structures of coconut husk, a pretreatment process is crucial in extracting fermentable sugars from the embedded cellulose matrix for subsequent ethanol fermentation process. The ground coconut husk was subjected to three different pretreatment processes inclusive of thermal, chemical, and microwave-assisted-alkaline techniques, prior to enzymatic hydrolysis and fermentation process. The composition profile of coconut husk was significantly altered upon the microwave-assisted-alkaline treatment as compared to the untreated sample, with the cellulose content increasing from 18-21% to 38-39% while lignin content decreased from 46-53% to 31-33%. Among the pretreatment methods applied, enzymatic hydrolysis of coconut husk pretreated by microwave-assisted-alkaline method recorded the highest yield of fermentable sugars, 0.279 g sugar/g substrate. SEM imaging showed the obvious and significant disruption of coconut husks’ structure after microwave-assisted-alkaline pretreatment. In conclusion, by employing suitable pretreatment technique in treating the lignocellulosic materials of coconut husk, the extracted fermentable sugar is a potential substrate for bioethanol production.