Desulfurant sorbents prepared by hydration, in sea or distilled water, of calcined sewage sludge (ash) and CaO at CaO/ash weight ratios of 0.2 or 3 at room temperature or at 90 °C, were characterized by X-ray diffraction in order to relate the X-ray composition of the sorbents to the preparation process and to the specific surface area of the obtained sorbents. Results show that the main compounds detected in the sludge´s ash are the same than those found in bibliography for the calcined sludge. In all the sorbents, independently of the preparation conditions, Ca(OH)2 was found instead of CaO used as raw material. New and different crystalline products were found in the sorbents depending on the preparation conditions. All the sorbents prepared in seawater contain NaCl in their composition; the specific surface area of the sorbents increased with hydration time and temperature and was lower when seawater was used for hydration.