In this study, a water-soluble polymer, polyacrylamide containing R-(+)-Cysteine end groups was used for the separation and preconcentration of copper, lead and chromium prior to their analysis by graphite furnace atomic absorption spectrometry. The sample and polymer solution were mixed and metal-bound polymer was precipitated upon addition of acetone. The precipitate was separated from solution and dissolved directly with distilled water. By this way. analyte elements were again transferred into the liquid phase and analyzed by graphite furnace atomic absorption spectrometry. The advantages and disadvantages of the method compared to those of the traditional batch and column techniques using water insoluble solid materials were described in all aspects. The method is simpler and faster compared to other preconcentration and separation techniques. Recoveries from matrix free aqueous solutions are higher than 96% and relative standard deviations were lower than 3%.