Employing an advanced citrate precursor methodology, we successfully synthesized nanoscale spinel ferrites, denoted as Mg1-xZnxFe2O4 (where x ranges between 0.0 and 1.0) or MZFO. Comprehensive analysis, utilizing state-of-the-art X-ray diffraction (XRD) techniques, demonstrated the defining attributes of the crystal structure. All examined specimens consistently exhibited a singular phase, adopting a cubic crystalline architecture. XRD pattern analysis allowed us to deduce the average particle dimensions of these ferrite specimens, which span between 17.2 nm and 31.5 nm. This observed size distribution corroborates well with transmission electron microscopy (TEM) imagery estimations. Delving into the Fourier-transform infrared (FTIR) spectra, two distinctive absorption bands of ferrites emerged: the first between 540 and 570 cm−1 and the subsequent between 339 and 435 cm−1. To glean insight into the electromagnetic attributes of MZFO, we meticulously assessed the experimentally ascertained S-parameters. This scrutiny spanned a frequency spectrum of 8–18 GHz. It was inferred that electromagnetic wave energy dissipation arises chiefly from a combination of electrical and magnetic phenomena. The underlying mechanisms of electrical dissipation can be attributed to polarization processes. Concurrently, the magnetic energy losses predominantly stem from magnetization reversal dynamics. Notably, a substantial attenuation observed in the reflected wave energy, ranging between −10 and −18.5 dB, augments the potential for this material's integration into practical applications.