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The paper presents a scheme of an experimental full-scale evaporation rig and a description of the tests carried out on it for the evaporation of nitric acid solutions with simultaneous denitration with formaldehyde. The results of work on a full-scale evaporator rig confirmed the possibility of using evaporation method with simultaneous denitration by formaldehyde in a natural-circulation evaporator with external heating chamber. The dependence of concentration of nitric acid to the molar ratio of formaldehyde to nitric acid was obtained.