A sorbent extraction method for the separation/preconcentration of Fe, Co, Ph, Cd, and Cr was developed. The analyte metal ions were retained on a column of Ambersorb 563 from a buffered sample solution. The flow rates of the sample and eluent solution were controlled by a peristaltic pump. The analyte ions were quantitatively retained at pH 9 by using an ammonia/ammonium chloride buffer solution, and were then eluted with 5 mL of 0.25 M HNO3 at 5 mL/min flow rate. The detection limits were in the range of 0.33 and 72 mug/L for Cd and Ph, respectively. The relative standard deviations were less than 10%. Recoveries of spike addition to drinking water and seawater were quantitative. The method presented was applied for the determination of Fe, Co, Ph, Cd, and Cr ions in drinking and seawater samples with satisfactory results (recoveries >95%).