Journal of Thermal Analysis and Calorimetry
Volume/Issue:
Volume 82: Issue 2
Thermal decomposition of liebigite
A high resolution thermogravimetric and hot-stage Raman spectroscopic study
Authors:
R. L. Frost Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology GPO Box 2434, Brisbane Queensland 4001, Australia GPO Box 2434, Brisbane Queensland 4001, Australia

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M. L. Weier Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology GPO Box 2434, Brisbane Queensland 4001, Australia GPO Box 2434, Brisbane Queensland 4001, Australia

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W. Martens Inorganic Materials Research Program, School of Physical and Chemical Sciences, Queensland University of Technology GPO Box 2434, Brisbane Queensland 4001, Australia GPO Box 2434, Brisbane Queensland 4001, Australia

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Pages:
373–381
Online Publication Date:
04 Nov 2005
Publication Date:
04 Nov 2005
Article Category:
Research Article
DOI:
https://doi.org/10.1007/s10973-005-0905-1
Keywords:
dehydration; dehydroxylation; high-resolution thermogravimetric analysis; Raman spectroscopy; andersonite; liebigite; rutherfordine
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A combination of high resolution thermogravimetric analysis coupled to a gas evolution mass spectrometer has been used to study the thermal decomposition of liebigite. Water is lost in two steps at 44 and 302°C. Two mass loss steps are observed for carbon dioxide evolution at 456 and 686°C. The product of the thermal decomposition was found to be a mixture of CaUO4 and Ca3UO6. The thermal decomposition of liebigite was followed by hot-stage Raman spectroscopy. Two Raman bands are observed in the 50°C spectrum at 3504 and 3318 cm-1 and shift to higher wavenumbers upon thermal treatment; no intensity remains in the bands above 300°C. Three bands assigned to the υ1 symmetric stretching modes of the (CO3)2- units are observed at 1094, 1087 and 1075 cm-1 in agreement with three structurally distinct (CO3)2- units. At 100°C, two bands are found at 1089 and 1078 cm-1. Thermogravimetric analysis is undertaken as dynamic experiment with a constant heating rate whereas the hot-stage Raman spectroscopic experiment occurs as a staged experiment. Hot stage Raman spectroscopy supports the changes in molecular structure of liebigite during the proposed stages of thermal decomposition as observed in the TG-MS experiment.

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Cover Journal of Thermal Analysis and Calorimetry
Journal of Thermal Analysis and Calorimetry
Print ISSN:
1388-6150
Online ISSN:
1572-8943

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation		 1969
Volumes
per Year		 1
Issues
per Year		 24
Founder Akadémiai Kiadó
Founder's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher		 Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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