A coprecipitation procedure for the separation and preconcentratiom of trace amounts of Fe(III), Mn(II), Cu(II), Pb(II), Cot(II), and Ni(II) is described. The analytical parameters including pH, ytterbium amount, centrifugation rate and time for the quantitative recovery of the analyte elements were optimized. The effect of matrix components of highly saline samples was also investigated. The limit of detection of the procedure was in the range of 2.1 mu g/L for copper, 8.2 mu g/L for nickel, and the preconcentration factor was 80. The accuracy of the method was checked by the addition recovery tests to real samples and by the analysis of the certified reference materials NIST SRM1570a Trace Elements in Spinach Leaves and SPS-WW2 Wastewater Level 2. The application of the method was performed for the determination of analyte elements in food and water samples.