Biosorption of nickel (II) and copper (II) ions from aqueous solution by dead sphaeroplea algae in natural and acid treated forms were studied as a function of concentration, pH, and adsorbent dose. The optimum pH for nickel (II) and copper (II) biosorption was found to be 6.0 and 4.0 respectively. The metal ion uptake increased with initial metal ion concentration studied up to 500 mg/L. Both the Freundlich and Langmuir adsorption models could fit the equilibrium data. The adsorption reasonably fitted the Lagergren kinetic model. Further the biomass was characterized by FTIR spectra. Surface area values are measured to be 0.9 and 2.1 m(2) /g for natural and acid treated forms respectively. The maximum adsorption capacity was found to be 3.40, 4.15 mmol/g for nickel (II) and 2.21, 3.41 mmol/g for copper (II) in natural and acid treated forms respectively.