The effectiveness of wet-spraying calcium acetate as an alternative to limestone and dolomite for the desulfurization of flue gases (in particular, H2S removal from coal gas) has been investigated by experimental studies using drop tube (DTR) and fixed-bed flow reactors (FBR). Calcium acetate solution was spray-calcined in the DTR at temperatures of 1073 and 1323 K. At the lower temperature, conversions approaching 80% were found at the longest residence time studied, 0.8 s. On the other hand, the higher temperature condition initially showed a much greater rate of calcination, indicated by greater conversion at shorter residence times, but was then followed by a much slower rate beyond 0.4 s. The final degree of conversion was in the region of 70%. Batches of spray-calcined calcium acetate (SCA), limestone, and dolomite, prepared in the DTR at 1323 K, to 70% conversion, were sulfided in the FBR at temperatures of 873 and 1173 K to assess their relative sulfur capture reactivities. Significantly higher conversions were achieved by the spray-calcined material, especially at the higher FBR temperature (1173 K) where a difference in conversion of more than 40% was observed. The physical structure of the particles formed from wet-spray calcination were determined by electron microscopy and showed highly porous cenospheres with large internal voids and an outside surface characterized by "blowholes" of between 1 and 10 mu m in diameter. As a consequence, the available surface area for reaction with H2S is greater than with limestone or dolomite, producing a 4-fold difference in the level of particle conversion.