The determinations of cadmium(H), silver(I), gold(II) and lead(II) in metallic zinc samples were performed using separation-preconcentration procedure on an Amberlite XAD-16 adsorption resin column. Cadmium, silver, gold and lead were quantitatively recovered and separated from a solution containing 1 M HCl and 0.3 M NaI. Effects of the matrix have been investigated. The recoveries of interesting elements wre found to be in the range of 95-103% through the use of proposed method. The procedure was successfully applied to the determination of trace impurities in four metallic zinc samples (recoveries > 95%, relative standard deviations < 10).