A separation and preconcentration method is described for the determination of copper, nickel, cobalt, lead, iron and cadmium in natural water and some salt samples by flame AAS. The analyte trace metal ions in the samples were sorbed as xylenol orange complexes on Amberlite XAD-16 column at the pH range of 7-9, and then eluted with 1M HNO3 in acetone. The effect of pH, reagent amount, sample volume, and matrix of the sample on the sorption of metal ions has also been investigated. The concentration of analyte ions detected after separation/and preconcentration was in agreement with the added amount of ions. The present method was found to be applicable to the preconcentration of analyte ions in natural water and some salt samples with good results such as relative standard deviations from 3 to 10% (N = 10).