In this study, the goal was to find lower temperature for separating the Zn and Fe content of ZnFe2O4 by sulfation reaction than previously achieved, and to study the various reactions steps of sulfation. Hence, the reaction of ZnFe2O4 with Mohr's salt containing iron(II), i.e. (NH4)2Fe(SO4)2•6H2O, and ammonium iron alum containing Fe(III), i.e. NH4Fe(SO4)2•12H2O was studied. At first the thermal decomposition of precursor salts in air was studied by TG/DTA-MS to find the proper temperature for sulfation. Then ZnFe2SO4:precursor salt mixtures with ratios 1:2 and 1:5 were prepared and annealed at 400, 425, 450 °C. The solubility of the products obtained at different annealing temperatures in water (e.g. ZnSO4, FeSO4, Fe2(SO4)3) and in HCl (Fe2O3, ZnO, Fex(OH)ySO4, Znv(OH)wSO4 basic sulfates) was studied. The morphology and structure of the starting materials was investigated by SEM, XRD and FTIR, the crystalline phases after each annealing and washing steps were studied by XRD. The Fe in the starting materials and the products obtained at 425 °C was measured by Mössbauer. Based on the obtained results,