A novel column solid phase extraction method was developed for the determination of Cu(II) and Fe(III) in various samples by flame atomic absorption spectrometry (FAAS) after preconcentration as their N-benzoyl-N-phenylhydroxylamine complexes on Amberlite XAD-1180 resin. Elution was performed with 1 mol L(-1) HCl in acetone. The effects of some analytical parameters such as pH, amount of reagent, eluent type, concentration and volume, flow rate of sample and elution solutions, volume of the sample solution and matrix interference were investigated. The recoveries of Cu(II) and Fe(III) under optimum conditions were a parts per thousand yen95%. A good relative standard deviation (a parts per thousand currency sign2.0%), a good preconcentration factor (50) and low detection limits (0.82 mu g L(-1) for Cu and 1.05 mu g L(-1) for Fe) were obtained. The accuracy of the procedure developed was confirmed by determining the analytes in three certified reference materials (TMDA-54.4 fortified lake water, SRM 1643e trace elements in water, SRM 1568a rice flour) and the analysis of spiked water samples. The results showed a good agreement with the certified values. The method was applied to the determination of the analytes in water (sea water, dam water, lake water and waste water), vegetable, rice and spices samples.