An application of solid-phase extraction procedure of chromium, cadmium and cobalt in urine was performed in the present study. Diaion HP-20 adsorption resin was used as solid phase. The analyte ions were complexed with 8-hydroxiquinoline, then metal complexes were adsorbed on the resin. After adsorption, the analytes were eluted by using 1M HNO3 in acetone. The metal determinations were performed by atomic absorption spectrometry. The influences of some analytical parameters such as pH, amounts of oxine. type of eluent etc, on the recoveries of chromium, cadmium and cobalt were discussed.