The level of scientific and technical progress is determined in many respects by inorganic materials – phosphors, sorbents, catalysts, aluminates, chromates, ferrite. The luminescing materials are widely used in medicine, criminalistics, agriculture, in various industries. It creates prerequisites for improvement of methods of receiving phosphors and further research of influence of features of structure of firm phases of materials on their spectral properties. Initial substances for synthesis, the leading role belongs to oxides, hydroxides and systems on their basis. Red phosphors which part compounds of europium are of particular interest. The systems of in the common besieged hydroxides (CBH) received continuous sedimentation of water solutions of nitrates of Eu (III) and AI(III), Fe(III), Cr(III) alkali. The SOG systems were studied by methods of the physical and chemical analysis: differential and thermal, IR-spectroscopic, X-ray phase, X-ray fluorescent, power dispersive. Registration, the emitted luminescent radiation of Eu3+ in a system, in the field of 741.4-746.9 nanometers were carried out at a stage of crystallization of amorphous products. The dependence of intensity of a luminescence of systems on synthesis conditions was established.