ABSTRACT. A new sorbent was prepared using alumina and 5-Br-PADAP, and its adsorption ability for the removal of Ni(II) and Pd(II) from different waters was investigated. The procedure is based on retention of the analytes on the alumina load with 5-Br-PADAP at pH ~ 6. The separation/preconcentration conditions for the quantitative recoveries were investigated. The limit of detections (LOD) based on three times the standard deviations of the blank, were 0.187 and 0.253 ng mL -1 for Ni(II) and Pd(II), respectively. Obtained sorption capacities for 1 g sorbent were 6.0 mg Ni(II) and 11.0 mg Pd(II). The linearity was maintained in the concentration range of 0.625 to 6.0 ng mL -1 for Ni(II) and 0.416 to 7.0 ng mL -1 for Pd(II) in the original solution. Eight replicate determinations of a mixture containing 2.0 µg mL -1 each of the elements in the final solution gave relative standard deviation of ±0.82 and ±1.12% for Ni(II) and Pd(II), respectively. The proposed method was successfully applied to the determination trace amounts of Ni(II) and Pd(II) in the surface water samples.