Thermal analysis of synthesis of wulfenite

Abstract

A derivatograph was used in a thermal analysis study of the synthesis of wulfenite (lead molybdate) by the sintering of cerussite or lead oxide with molybdite. The reaction products were identified microscopically and by using a Siemens crystalloflex diffractometer. The DTA curves of mixtures of cerussite with molybdite show first the characteristic peaks of cerussite. The sharp endothermic peak at 300°C reflects the dehydration of hydrocerussite associated with cerussite. The endothermic peak at 350°C indicates the first step of cerussite decomposition, into PbO·PbCO₃, and that at 400°C indicates the second step of its decomposition, into lead oxide. The formation of wulfenite takes place at 520°C in an exothermic reaction. The medium endothermic peaks at 880 and 955°C reflect the melting and volatilization of unreacted lead and molybdenum oxides. The DTA curve of sintering of molybdite with lead oxide reveals the formation of wulfenite at 500°C. The melting and volatilization of unreacted lead and molybdenum oxides appear in only one large and sharp endothermic peak at 980°C.

The resulting wulfenite is pale-yellow in thin section, and crystallizes in the tetragonal system, in the form of square tabular crystals, with distinct (011) cleavage.