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This article is devoted to the study of the technology of selective separation of zinc and copper compounds from metallurgical wastes formed during the production of bronze and brass by hydrometallurgical method. The relevance of the study is associated with the depletion of mineral raw materials and the increasing environmental load of metallurgical wastes on the environment. The purpose of the work is to determine the possibility of obtaining copper and zinc in an efficient and environmentally friendly way during the processing of bronze and brass slags. During the study, nitric acid, ammonia solutions and sulfuric acid were used, and their leaching efficiency was comparatively evaluated. The chemical and phase composition of the slags was determined by inductively coupled plasma optical emission spectrometry, infrared spectroscopy and X-ray phase analysis. As a new methodological approach, the “hot leaching” method using 25% sulfuric acid at a temperature of 80 °C was used. The results of the study showed that sulfuric acid is more economically and environmentally effective in the separation of copper and zinc. The process resulted in the formation of tin precipitate, chemically and electrochemically extracted high-purity metallic copper, and solid waste rich in zinc. The proposed technological scheme reduces metal consumption, increases the possibility of waste recycling, and is of practical importance for the development of low-waste, resource-saving metallurgical technologies.