Zinc ferrite Polyurethane foam composite materials were formed by adding 0.33wt% ZnFe₂O₄ nanoparticles into polyurethane foam (PUF) during the preparation process. ZnFe₂O₄/PUF composite materials have successfully been utilized as a new solid phase extraction (SPE) sorbent for the separation of cadmium and copper ions in various water samples. The XRD results revealed that only the spinel structure of ZnFe₂O₄ was formed, with an average crystallite size of 24nm. The ferromagnetic behaviour of ZnFe₂O₄ nanoparticles was observed, with magnetization of 4.179emu/g and coercivity of 267.11G. The microstructure of the prepared composite materials observed the spongy structure and higher porosity. The aqueous solution and real water (from Fayoum city, Egypt) were used for studying the effects of pH, sorbent dose, and shaking time of the composite materials on the Cd²⁺ and Cu²⁺ ions removal. The batch procedure shows the maximum extraction percentage of Cd²⁺ and Cu²⁺ ions were 95.8% and 96.5% at the optimal conditions.