A multi-element preconcentration-separation technique for heavy metal ions in environmental samples has been established. The procedure is based on coprecipitation of gold(III), bismuth(III), cobalt(II), chromium(III), iron(III), manganese(II), nicke](11), lead(II), thorium(TV) and uranium(VI) ions by the aid of Cu(Il)-9-phenyl-3-fluorone precipitate. The Cu(Il)-9-phenyl-3-fluorone precipitate was dissolved by the addition 1.0 mL of concentrated HNO3 and then the solution was completed to 5 mL with distilled water. Iron, lead, cobalt, chromium, manganese and nickel levels in the final solution were determined by flame atomic absorption spectrometer, while gold, bismuth, uranium and thorium were determined by inductively coupled plasma mass spectrometer. The optimal conditions are pH 7, amounts of 9-phenyl-3-fluorone: 5 mg and amounts of Cu(11): I mg. The effects of concomitant ions as matrix were also examined. The preconcentration factor was 30. Gold(III), bismuth(III), chromium(III), iron(III), lead(II) and thorium(IV) were quantitatively recovered from the real samples. The detection limits for the analyte elements based on 3 sigma (n = 15) were in the range of 0.05-12.9 mu g L-1. The validation of the presented procedure was checked by the analysis of two certified reference materials (Montana I Soil (NIST-SRM 2710) and Lake Sediment (IAEA-SL-1)). The procedure was successfully applied to some environmental samples including water and sediments. (c) 2007 Elsevier B.V. All rights reserved.