Ternary Mn-Zn ferrite (MnxZn1-xFe2O4) nanoparticles (NPs) have been prepared by the thermal decomposition of an oleate complex, sodium dodecylbenzenesulfonate (SDBS) mediated hydrazine decomposition of the chloride salts, and triethylene glycol (TREG) mediated thermal decomposition of the metal acetylacetonates. Only the first method was found to facilitate the synthesis of uniform, isolable NPs with the correct Mn : Zn ratio (0.7 : 0.3) as characterized by small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), and inductively coupled plasma-optical emission spectroscopy (ICP-OES). Scaling allowed for retention of the composition and size; however, attempts to prepare Zn-rich ferrites did not result in NP formation. Thermogravimetric analysis (TGA) indicated that the incomplete decomposition of the metal-oleate complexes prior to NP nucleation for Zn-rich compositions is the cause.