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In this article process mineralogy research on the sorting flotation tailings of zinc and sulfur has been carried out at first.X-ray diffraction analysis and chemical multi-element analysis results show that in the tailings the main metal sulphide minerals are pyrite, the main gangue constituents are quartz, chlorite-serpentine and muscovite.the main valuable metals in the tailings are copper、 zinc and silver.Basic mineral composition of copper and zinc have been identified through chemical phase analysis,and the feasibility for extracting the main valuable metals were discussed accordingly.In order to identify the loss form of copper and zinc in the tailings, first of all the basic chemical composition of samples were determined through X-ray photoelectron spectroscopy(xps) analysis, then the mode of occurrence of copper and zinc minerals are identified under microscopic study.