Fe(III)/Cr(III) hydroxide, a waste sludge from fertiliser industry has been used for adsorption of Cr(VI) and Fe(II) from aqueous solution in fixed bed method. Effects of parameters such as initial metal ion concentration and pH were studied at a flow rate of 10 ml/min of the water solution. The breakthrough curves are typical sigmoidal type ones and the results show that increase in metal ion concentration decreases the breakthrough volume. The breakthrough volume is higher at pH 5.0 (500 ml/5g) than at pH 5.7 (100 ml/5g) for Cr(VI) adsorption. The adsorption obeys the Bed Depth Service Time (BDST) model and the adsorption capacity values are presented.