AbstractThe effects of thermal-alkaline pretreatment on dewatered activated sludge (DAS) solubilisation and subsequent high-solid anaerobic digestion were studied by response surface methodology (RSM) from 105 to 135 °C and between 5 and 35 mg alkaline/g total solid (TS) DAS. Soluble chemical oxygen demand (SCOD), soluble carbohydrates, and protein concentrations were significantly enhanced in thermal-alkaline pretreated DAS samples. Daily methane yield increased at the middle of digestion, and cumulative methane yield (CMY) significantly increased after thermal-alkaline pretreatment. A first-order linear model of temperature and alkaline was significant for SCOD by RSM, and the determination coefficient (R2) was 94.62%. The quadratic model of temperature and alkaline was also significant for methane yield. R2 of 99.80% confirmed that the model used in this study fit the experimental variables very well. Using the model, the optimum pretreatment condition of methane yield was obtained at 134.95 °C and 23.77 mg alkali. Therefore, RSM was an effective tool in predicting the DAS pretreatment condition for optimum methane yield.