An enrichment/separation system for atomic absorption spectrometric determinations of Cu(Ⅱ), Fe(Ⅲ), Ni(Ⅱ) and Co(Ⅱ) has been established. The procedure is based on the adsorption of the analytes as calmagite chelates on Chromosorb-102. The effects of some parameters including pH, amount of ligand, salt matrix, flow rates of sample and eluent solutions were investigated. Under optimized conditions, the relative standard deviation of the combined method of sample treatment, preconcentration and determination with FAAS (N=5) is generally lower than 5%. The limit of detection (3σ) was between 6.0-112.9 ㎍/L. The results were used for preconcentration of analytes from some sodium and ammonium salt.