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This study presents findings from experiments on the preparation and characterization of locally available fly ash, quicklime and the CaO/fly ash sorbent, synthesized using the atmospheric hydration process. The CaO was obtained from calcination of limestone in a laboratory kiln at a temperature of 900°C. The sorbents were prepared under different hydration conditions: CaO/fly ash weight ratio (1∶1 to 1∶3), hydration temperature (55°C-75ºC) and hydration period (4-8 h). Results show that the specific surface area of CaO/ fly ash sorbents (8.8-23.6 m 2 /g) was higher than that of the CaO (4.78 m 2 /g) at all preparation conditions. The SEM micrographs show that the prepared sorbent had a more porous structure than either the fly ash or the CaO. The X-ray diffraction (XRD) analysis shows the presence of complex compounds containing calcium silicate hydrate in the synthesized sorbents. This contributed to the high BET specific surface area. The Brunauer-Emmett-Teller (BET) specific surface area was found to decrease with increase in the amount of fly ash with the ratio of 1∶1 (CaO/Fly ash) giving the highest value. It was also found that an increase in the hydration time resulted in an increased BET specific surface area, although there was only a slight effect on the same by an increase in temperature.