Chitosan and Ca-alginate, derivatives of biopolymer, were separately prepared from crab chitin and algin in pellet form. for adsorption of Cu(II) and Ni(II) from aqueous solutions. The capability of these biopolymers was also investigated to remove copper and nickel from aqueous solutions in an immobilization system, along with a comparison made of these biopolymers with other adsorbents. Additionally, the feasibility of alginate/chitosan in pellets to remove nickel ion and nickel cyanide complex from polluted water was investigated. Stabilizing chitosan physically in an alginate support medium was deemed possible, by means of which both free metal and metal cyanide ions could be removed from aqueous solutions in an engineering system. However, the crosslinking reaction during immobilization would result in blocking of some adsorption sites.