Development of a high-pressure thermobalance working under constant rate thermal analysis

• Published in: Journal of thermal analysis and calorimetry Vol. 142; no. 3; pp. 1329 - 1334
• Main Authors: Perejón, Antonio, Sánchez-Jiménez, Pedro E., Criado, José Manuel, Pérez-Maqueda, Luis A.
• Format: Journal Article
• Language: English
• Published: Cham Springer International Publishing 01.11.2020; Springer; Springer Nature B.V
• Subjects: Analytical Chemistry; Chemistry; Chemistry and Materials Science; Heat transfer; Heating rate; Inorganic Chemistry; Mass transfer; Measurement Science and Instrumentation; Oxidation; Physical Chemistry; Polymer Sciences; Room temperature; Thermal analysis; Constant rate thermal analysis; Nickel; Thermogravimetry; Thermal oxidation; High pressure
• ISSN: 1388-6150; 1588-2926
• DOI: 10.1007/s10973-020-09644-5

A thermogravimetric instrument that works at high pressure of different gases has been designed and assembled. The instrument has been devised to work in a temperature range from room temperature to 1000 °C in various controlled pressures of selected gas up to 15 bar, and under conventional rising temperature and constant rate thermal analysis (CRTA) modes. CRTA method allows an intelligent control of the reaction temperature using a feedback system that monitors the mass gain or mass loss of the sample in such a way that the reaction rate is maintained constant all over the process at a preselected value. CRTA method provides a significant advantage for studying processes under high pressure as it reduces heat and mass transfer phenomena that are very relevant under these high-pressure experimental conditions. The thermal oxidation of Ni at 8 bar of pure oxygen has been used for testing the performance of the instrument under both linear heating rate and CRTA conditions.