This paper proposes an alternative analytical method using energy dispersive X-ray fluorescence (EDXRF) to determine Fe and Cu in gasoline samples. In the proposed procedure, samples were distilled and the distillation residues were spotted on cellulose paper disk to form a uniform thin film and to produce a homogeneous and reproducible interface to the XRF instrument. The disks were dried at 60 degrees C for 20min and copper and iron were determined directly in the solid phase at 6.40 and 8.04keV, respectively. The calibration curves showed linear response in the 20-800mugL(-1) concentration range of each metal. The precisions (repeatability) calculated from 15 consecutive measurements and defined as the coefficient of variation of solutions containing 100mugL(-1) of Fe and Cu were 7.8 and 8.1%, respectively. The limits of detection (LOD), defined as the analyte concentration that gives a response equivalent to three times the standard deviation of the blank (n=10), were found to be 10 and 15mugL(-1) for Fe and Cu, respectively. The proposed method was applied to copper and iron determination in gasoline samples collected from different gas stations.