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In this work, a mineralogical study and thermal decomposition analysis of jarosite residue sample from a zinc plant were carried out. The mineralogical analysis showed that the jarosite residue is mainly composed of four components, including jarosites, sulfates–hydroxides, sulfides and spinel. The distribution of relevant metallic elements in these components was characterized using a sequential extraction process. The X-ray diffraction results showed that AFe3(OH)6(SO4)2 and ZnFe2O4 are the main components of the jarosite residue sample. The thermal decomposition mechanisms of ammoniojarosite and sodium jarosite were studied by TG-DSC (Thermogravimetric analysis–differential scanning calorimetry). The thermal decomposition process and the corresponding mechanism of the jarosite residue were analyzed. The jarosite thermal decomposition process includes the removal of crystal water, dihydroxylation and deammoniation, desulfonation of component jarosite and desulfonation of component zinc sulfate.