VIBRATIONAL AND THERMAL STUDY OF ANTIMONY OXIDES

Antimony oxides have been characterized by combining thermogravimetric analysis and Raman spectroscopy. Residues and condensates produced from the thermogravimetric analysis of Sb2O3 (senarmontite and valentinite), Sb204 (α and β phase), Sb2O5. XH2O, and Sb6O13 were identified by X-ray diffraction and Raman and infrared spectroscopy. The formation of β -Sb2O4 was accomplished by heating α-Sb2O4 or Sb6O13 in closed quartz capillaries at 960 °C. Heating the two polymorphs of Sb2O3 in air revealed that both senarmontite and valentinite exhibited simultaneous volatilization and oxidation; however, senarmontite displayed a net weight loss of 21-26% whereas valentinite gained 0.8-2.4%. TG experiments of Sb2O5-AH2O heated in air indicated that the 650-850 °C plateau was Sb6O13 and the 890-970 °C plateau was α-Sb2O4. Infrared and Raman spectra of all the above mentioned antimony oxides were recorded, with the Raman spectra of α-Sb2O4, β -Sb2O4, and Sb6O13 being reported for the first time. © 1979, American Chemical Society. All rights reserved.