Manganese ferrite nanoparticles (MnFe2O4) were synthesized via surfactant-assisted co-precipitation, where sodium dodecyl sulfate (SDS) was used as the template to control particle size at various SDS concentrations. The substitutions of iron (II) (Fe2+) into the MnFe2O4 ferrite nanoparticles were carried out to obtain Fe(1–x)MnxFe2O4, with various Mn2+: Fe2+ molar ratios. The synthesized ferrite nanoparticles were characterized by the Fourier-transform infrared spectroscopy (FT-IR), thermogravimetric analyzer (TGA), X-ray diffractometer (XRD), energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), transmission electron microscope (TEM), two-point probe, and vibrating sample magnetometer (VSM) techniques. The experimental Mn:Fe mole ratios of the Fe(1−x)MnxFe2O4 ferrite nanoparticles were verified to be in agreement with the theoretical values. The synthesized MnFe2O4 and Fe(1−x)MnxFe2O4 ferrite nanoparticles were of mixed spinel structures, with average spherical particle sizes between 17–22 nm, whereas the magnetite ferrite nanoparticles (Fe3O4) were of the inverse spinel structure. They showed soft ferromagnetic behavior. The synthesized Fe0.8Mn0.2Fe2O4 ferrite nanoparticle possessed the highest saturation magnetization of 88 emu/g relative to previously reported work to date.