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In this paper, we present a comparative analysis of the physicochemical properties of magnetite nanoparticles synthesized via two primary methods: (i) co-precipitation of iron (II) and (III) chloride in an ammonia solution and (ii) thermal decomposition of Fe(acac)3in an organic solvent. In each case, variable synthesis conditions were used (mixing, temperature, inert gas presence, time of synthesis), which significantly influenced the resulting nanoparticle characteristics, including size, size distribution, shape, and magnetic properties. By utilization of such techniques as transmission electron microscopy, X-ray diffraction, infrared spectroscopy, and Mössbauer spectroscopy, we demonstrate the ability to exert control over particle growth to a considerable extent. Our findings underscore the innovative aspect of our work, revealing quantitative insights into the precise manipulation of nanoparticle properties, thus offering promising ways for tailored applications in diverse fields.