Generally speaking, anionic metal concentrations in wastewater from industries and mineral processing plants are well above the allowed limits for effluent set by the Ministry of Environment of Japan. Nowadays, the removal of anionic ions has been considered difficult and development of new process is desperately needed. In this paper, we report the development of three hydroxide-type adsorbents, illustrating their adsorption efficiency in removing As, Se, Mo and Sb ions from aqueous solutions. The main finding of this work was that the adsorption behavior was influenced very much by both the pH and the adsorbent concentration. Nevertheless, the newly developed hydroxide-type adsorbents were very effective in reducing the concentration of those anionic ions.