Use of Solid Insertion Probe Mass Spectrometry and Constant Rate Thermal Analysis in the Study of Materials: Determination of Apparent Activation Energies and Mechanisms of Solid-State Decomposition Reactions

M. J. Tiernan, P. A. Barnes, G. M B Parkes

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15 Citations (Scopus)

Abstract

Thermally induced reactions are of great importance in the manufacture and characterization of a very wide range of increasingly complex materials covering areas as diverse as ceramics and heterogeneous catalysts. Subsequently, there is a need for improved thermoanalytical methods that can provide enhanced resolution and a greater understanding of the energetics and mechanisms involved. This paper describes a new solid insertion probe mass spectrometer (SIP-MS) system that is designed to meet these needs by operating high vacuum with small sample masses. The SIP-MS system supports both conventional linear heating and a range of sample-controlled thermal analysis (SCTA) techniques including constant rate thermal analysis (CRTA). Its ability, in conjunction with the latter technique, to obtain reliable apparent activation energy measurements throughout a process under near-ideal experimental conditions is demonstrated. In addition, the system can discriminate between different reaction mechanisms and provide information on the often complex solid-state reactions found in calcination processes.

LanguageEnglish
Pages6944-6949
Number of pages6
JournalJournal of Physical Chemistry B
Volume103
Issue number33
DOIs
Publication statusPublished - 19 Aug 1999

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Mass spectrometers
Thermoanalysis
Mass spectrometry
insertion
thermal analysis
mass spectroscopy
Activation energy
activation energy
solid state
Decomposition
decomposition
Electric power measurement
mass spectrometers
probes
Solid state reactions
Calcination
support systems
Vacuum
high vacuum
Heating

Cite this

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