Inductively coupled plasma-atomic emission spectrometry (ICP-AES) has been applied to the simultaneous determination of trace impurities in high purity iron after simultaneous separation. Sub μg·g-1 levels of Ca, Cd, Co, Cu, Mg, Mn, Ni, Pb and Zn in high purity iron which had been dissolved in hydrofluoric acid and hydrogen peroxide were separated from the iron matrix using a horizontal cation exchange resin mini-column. Flow rates and flow directions of solutions through the mini-column were controlled by a peristaltic pump. Adsorbed elements on the resin mini-column were rapidly eluted using a reverse flow of the eluant against the flow for the adsorption. The eluted elements were determined by ICP-AES using an internal standard method and good results were obtained. A 100-fold enrichment of analytes was obtained with this preconcentration system using 1 g of the sample in comparison with an ordinary sample solution in which 0.5 g of the sample was dissolved in 100 cm3 without separation.