This work describes Fe 3 O 4 @SiO 2 core-shell nanoparticles functionalized with polyvinyl alcohol and its application for the removal of Cu(П) and Cd(П) ions by analytical methods under diverse experimental parameters. Surface chemistry and morphology during functionalization of Fe 3 O 4 @SiO 2 NPs were monitored using Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), vibration sample magnetometer (VSM), transmission electron microscope (TEM), eld emission scanning electron microscope (FE-SEM), dynamic light scattering (DLS). The performance of the polyvinyl alcohol modi ed magnetic nanoparticles for metal ions removal was evaluated by changing ve process variables: contact time of adsorbent, temperature, pH, adsorbent dosage and the selective removal. The adsorption isotherm studies of the novel adsorbent in removing heavy metals from wastewater showed that the maximum absorption amounts of Cu(П) and Cd(П) were 1.57 and 0.99 mmol/g at 35 o C. According to the results, the prepared composites possess excellent adsorption e ciency to be applied for the preconcentration of heavy metal ions in the eld of water treatment. The Fe 3 O 4 @SiO 2 -TCT-PVA adsorbent is completely separated from the aqueous solution under external magnetic eld for ve consecutive cycles without signi cant loss of activity.