Two preconcentration techniques, ion exchange and fl otation, were used for the determination of zinc (Zn), nickel (Ni) and cadmium (Cd) in natural water samples. In the fi rst part of our work, the adsorption of zinc(II), nickel(II) and cadmium(II) on Lewatit TP 207 chelating resin containing iminodiacetate groups was studied at different pH values by a batch process. The effects of parameters such as amount of resin, contact time, pH and initial metal concentration on the ion exchange separation were investigated. For the determination of the adsorption behavior of the resin, the adsorption isotherms of metal ions were also studied. The concentrations of metal ions were measured by batch techniques and with atomic absorption spectrometry analysis. Adsorption analysis results obtained at various concentrations showed that the adsorption pattern on the resin followed Langmuir and Freundlich isotherms. The effi ciency of removal is higher for Ni and Zn than Cd ions. Here, we report the method that is applied for the sorption and separation of some toxic metals from the solutions. In the second part of our work, the fl otation technique was used for preconcentration. The ability of Co(III) hexamethylenedithiocarbamate, Co(HMDTC) 3 , as a fl otation collector for metals from natural waters was investigated. The fl otation method was compared with the ion exchange method. The recoveries of Zn, Cd and Ni from natural water samples were approximately 99 % . Our results showed that the two methods were very effective, but the fl otation results were higher than the ion exchange results. In the present study, a method was described for the determination of Zn, Ni and Cd by fl ame atomic absorption spectrometry (FAAS) after preconcentration and separation in water by ion exchange resin and fl otation. Results of these two methods are compared. Analytical parameters such as precision and accuracy of methods were also studied. The equilibrium experimental results of Zn, Ni and Cd ions exchanged were fi tted by Langmuir-Freundlich adsorption isotherm models.