Sorbents synthesized from various types of ash (coal fly ash, coal bottom ash, oil palm ash, and incinerator ash) for flue gas desulfurization were investigated. The sorbents were prepared by mixing the ashes with calcium oxide and calcium sulfate using the water hydration method. The effects of various sorbent preparation variables, such as the hydration period, the ratio of calcium oxide to ash, and the amount of calcium sulfate, on the Brunauer-EmmettTeller (BET)-specific surface area of the resulting sorbent were studied using a two-level full factorial design. The surface area of the sorbents obtained range from 15.4 to 122.1 m 2 /g. Regression models were developed to correlate the significant variables to the surface area of the sorbents. An analysis of variance (ANOVA) showed that the model was significant at a confidence level of 95%. It was found that apart from all the individual variables studied, interactions between variables also exerted a significant influence on the surface area of the sorbent. From the activity test results, it was found that sorbents prepared from coal fly ash and oil palm ash have the highest SO 2 absorption capacity. Scanning electron microscope (SEM) analysis showed that the sorbent was composed of a compound with a high structural porosity, while an X-ray diffraction spectrum showed that calcium aluminum silicate hydrate compounds are the main products of the hydration reaction.