A study on superparamagnetic magnetite polymer composite development was undertaken for application to magnetically assisted chemical separation. Tetramethyl ammonium hydroxide as an alternative to ammonia was used as a precipitation agent to obtain nanoscale magnetite particles. Investigation on stoichiometry control of Fe(III) and Fe(II) ions suggested a correlation between alkalinity and initial Fe(III): Fe(II) ratio for precipitation of magnetite. Studies on polymerization conditions suggested that polymers setting at ambient conditions enable retention of superparamagnetic property of substrate magnetite. Vaporization method for impregnation of solvent extractant CMPO, yielded product that had a high sorption capability for radionuclide europium as compared to wet impregnation method.