A simple flame atomic absorption spectrometric (FAAS) procedure for the determination of lead, bismuth, gold, palladium and cadmium as impurities in Raney nickel and nickel oxide was developed using a preconcentration step on an Amberlite XAD-16 resin packed column. Lead, bismuth, gold, palladium and cadmium were quantitatively recovered and separated from a solution containing 1 M HCl and 0.3 M NaI by the column system. Effects of the various parameters such as reagent concentrations, sample volume, matrix effects, etc, have been investigated. Under optimized conditions, the relative standard deviation of the combined method of sample treatment. preconcentration and determination with FAAS (n = 7) is generally lower than 12%. The limit of detection (3s, n = 20) was between 10-270 ng/g. The results were used for separation and preconcentration of five trace elements from nickel matrices.