Spouted beds provide a means of good hydrodynamic conditions and circulation of solid particles. The spouting technique has been applied in many industrial processes, such as drying of granular materials, blending of polymer chips, coating of tablets, pyrolysis, gasification, and granulation of fertilizers. The aim of the present study is to examine the performance of a batch conical air spouting vessel for conducting ion exchange reactions involving heavy metal removal. The rate of ion exchange reaction was expressed in terms of volumetric mass transfer coefficient (K). The effect of various parameters such as type of heavy metal ion (Ni2+, Pb2+), superficial air velocity, and initial heavy metal concentration has been investigated. It has been found that volumetric mass transfer coefficient increases as air superficial velocity increases. Mass transfer correlations were obtained using dimensional analysis of the present mass transfer data. The importance of these mass transfer correlations in the design and operation of air spouting vessels used for conducting diffusion-controlled reactions was highlighted.