Every year, metallurgical enterprises generate a massive amount of toxic exhausted high-concentration etching solutions. Application of the ferritization process to recycle exhausted etching solutions can help to prevent environmental pollution. It enables a cost-efficient use of water at an industrial plant and allows the plant to obtain products from toxic industrial waste and utilize it. The aim of the study was to analyze the qualitative and quantitative composition of the formed sediment and its grain size composition. Variable study parameters were the initial pH values of the solutions, the initial concentrations of total iron, and the duration of the aeration process of the reaction mixture. Thermal activation and alternating magnetic fields were used to activate the ferritization. The XRD showed that the formed sediments contained phases of γ-FeOOH, δ-FeOOH, Fe3O4, and γ-Fe2O3. Granulometry analysis showed that these sediments were highly dispersed and heterogeneous. Chemically stable phases of magnetite were obtained in the composition of sediments, with an initial concentration of iron in the reaction mixture of 16.6 g/dm3, a pH of 11.5, and a process duration of 15 min. The study results demonstrated the feasibility of further study and possible use of such sediments with a high magnetite content for the production of materials with ferromagnetic and sorption properties.