This monograph is based on research work and several literature. Heavy metals, especially Nickel and Chromium can have serious effects on human and animal health and they are non-renewable resources. Therefore effective recovery of heavy metals is as important as removal of them from waste streams.The conventional methods may be ineffective or expensive, especially when the heavy metal ions are in solutions containing in the order of 1-100 mg dissolved heavy metal ions/L.The Calotropis procera and Embalica officinalis, plant biomasses were investigated as a new biosorbent for the removal of Ni(II) and Cr(VI) from aqueous solution with 90% and 100% sorption efficiency of Ni(II) and Cr(VI) from 50 mg/L solution. This study provides information on the removal of Cr(VI) and Ni(II) by using two different low cost adsorbents. Different parameters, adsorption isotherm and elution test, co-ions effects etc were studied.