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In this study, xCaO‧5Fe₂O₃‧(95−x)Pb glasses and vitroceramics containing various concentrations of calcium ions (from 0 to 50 mol% CaO) were prepared using the spent anodic plate of a car battery. X-ray diffraction analysis revealed changes in the network structure as a function of CaO content. The intensities of the IR bands due to the sulfate and sulfite units were lowered, indicating a decrease in the sulfurization degree within the lead network. In the UV–vis spectra, the presence of electronic transitions of the Fe³⁺, Pb²⁺, and Fe²⁺ ions were identified. The EPR spectra were characterized by resonance signals centered at about g ~ 2 and 4.3, corresponding to the trivalent iron ions. For the samples with 5 ≤ x ≤ 12, the signals decreased abruptly, suggesting a Fe³⁺→Fe²⁺ interconversion and the formation of the Fe₃O₄ crystalline phase. A considerable increase in the intensity of the signal centered around g ~ 2 was observed as the CaO concentration increased to 30% in the host matrix. Our results confirm that the higher CaO levels of 3 mol% are responsible for the increase in the radius of curvature of the semicircle arcs in the EIS plots and the decrease in their conductivity.