Cu²⁺ and Ni²⁺ complexes of chitosan/poly(vinyl amine) (CS/PVAm) composites were prepared. The metal-CS/PVAm complexes were characterized by FT-IR spectroscopy, SEM-EDX, X-ray diffraction (XRD), and magnetic moment determination. FT-IR spectra of the metal-CS/PVAm complexes showed the characteristic bands of anhidroglucose unit were affected by the metal complexation, and new bands assigned to Me–N and Me-O bonds were observed. SEM images of the surface of metal-composite complexes show the influence of metal ion on the morphology of the complexes, the strong binding of Cu²⁺ and Ni²⁺, involving most of the amino groups, leading to a dense surface structure. The chemical composition on the surface of metal-CS/PVAm complexes was determined from EDX measurements. XRD provided information about the amorphous or crystalline nature of the composite and metal-composite complexes. Using magnetic susceptibility method, the oxidation degree of metal ions from the polymer phase, the homogeneous distribution of the ligand groups from the volume of the CS/PVAm beads, and the existence of the antiferromagnetic interactions between the metal ions were determined.