Hostname: page-component-586b7cd67f-t8hqh Total loading time: 0 Render date: 2024-11-24T00:42:05.807Z Has data issue: false hasContentIssue false

Structural evolution during the dehydration of gypsum materials

Published online by Cambridge University Press:  05 July 2018

S. D. M. Jacques*
Affiliation:
Department of Chemistry, University College London, 20 Gordon Street, London WC1H OAJ, UK and School of Crystallography, Birkbeck College, Malet Street, London WC1E 7HX, UK
A. González-Saborido
Affiliation:
Department of Chemistry, University College London, 20 Gordon Street, London WC1H OAJ, UK and School of Crystallography, Birkbeck College, Malet Street, London WC1E 7HX, UK
O. Leynaud
Affiliation:
Department of Chemistry, University College London, 20 Gordon Street, London WC1H OAJ, UK and School of Crystallography, Birkbeck College, Malet Street, London WC1E 7HX, UK
J. Bensted
Affiliation:
Department of Chemistry, University College London, 20 Gordon Street, London WC1H OAJ, UK and School of Crystallography, Birkbeck College, Malet Street, London WC1E 7HX, UK
M. Tyrer
Affiliation:
Department of Materials, Imperial College, Prince Consort Road, South Kensington, London SW7 2BP, UK
R. I. W. Greaves
Affiliation:
Department of Materials, Imperial College, Prince Consort Road, South Kensington, London SW7 2BP, UK
P. Barnes
Affiliation:
Department of Chemistry, University College London, 20 Gordon Street, London WC1H OAJ, UK and School of Crystallography, Birkbeck College, Malet Street, London WC1E 7HX, UK
*

Abstract

The dehydration of pure and waste gypsums has been examined using in situ synchrotron angledispersive X-ray diffraction. Pure gypsum was studied under a number of defined environments; various industrial waste gypsums were also studied under a common standard environment. It is found that the dehydration of gypsum to anhydrite proceeds via the hemihydrate and γ-anhydrite phases and the interplay and behaviour of these phases has been determined by full structural ‘Rietveld’ refinement. In the study of the pure gypsum system, the hemihydrate structure is shown to be preserved as water is lost. A ‘zero-water hemihydrate’ is observed before refinement in the higher symmetry γ-anhydrite cell is possible. The waste gypsum materials studied showed significant differences in the temperatures at which key transformation events occurred; these observations raise implications concerning the re-use of by-product gypsum materials. Finally, high temperature data are re-examined in the search for a variation of the anhydrite structure.

Type
Research Article
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2009

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Abriel, W., Reisdorf, K. and Pannetier, J. (1988) Kinetisch stabile phasen bei der dehydratationsreak- tion von gips. Zeitschrift für Kristallographie, 182, 1-2 .Google Scholar
Abriel, W., Reisdorf, K. and Pannetier, J. (1990) Dehydration reactions of gypsum: A neutron and X-ray diffraction study. Journal of Solid State Chemistry, 85, 23-30 .CrossRefGoogle Scholar
Ballirano, P, Maras, A., Meloni, S. and Caminiti, R. (2001) The monoclinic I2 structure of bassanite, calcium sulphate hemihydrate (CaSO4-0.5H2O). European Journal of Mineralogy, 13, 985-993 .CrossRefGoogle Scholar
Bensted, J. and Varma, S.P. (1968) Investigation of the calcium sulphate-water system by infrared spectroscopy. Nature, 219, 60-61 .CrossRefGoogle Scholar
Bensted, J. and Varma, S.P. (1971) Infrared spectroscopic studies of calcium sulphate heated to high temperatures. Zeitschrift für Naturf'orschung B, 26, 690-693 .CrossRefGoogle Scholar
Berry, A., Helsby, W.I., Parker, B.T., Hall, C.J., Buksh, P.A., Hill, A., Clague, N., Hillon, M., Corbett, G., Clifford, P. Tidbury, A., Lewis, R.A., Cernik, R.J., Barnes, P. and Derbyshire, G.E. (2003) The Rapid2 X-ray detection system. Nuclear Instruments & Methods in Physics Research, 513, 260-263 .CrossRefGoogle Scholar
Bobrov, B.S., Romaschkov, A.B. and Andreeva, E.P. (1987). Zhurnal Neorganicheskoi Khimii, 23, 497.Google Scholar
Candlot, E. (1906) Ciments et Chaux hydrauliques. Fabrication, Proprietes, Emploi, Troisieme edition, (C. Beranger, editor). Libraire Polytechnique, Paris/ Liege.Google Scholar
Cernik, R.J., Barnes, P., Bushnell-Wye, G., Dent, A.J., Diakun, G.P., Flaherty, J.V., Greaves, G.N., Heeley, E.L., Helsby, W., Jacques, S.D., Kay, J., Rayment, T., Ryan, A., Tang, C.C. and Terrill, N.J. (2004) The new materials processing beamline at the SRS Daresbury, MPW6.2. Journal of Synchrotron Radiation, 11, 163-170 .CrossRefGoogle ScholarPubMed
Christensen, A.N., Olesen, M., Cerenius, Y. and Jensen, T.R. (2008) Formation and transformation of five different phases in the CaSO4-H2O system: Crystal structure of the subhydrate beta-CaSO4.0.5H2O and soluble anhydrite. Chemistry of Materials, 20, 21242132.CrossRefGoogle Scholar
Cole, W.E. and Lancucki, C.J. (1974) A refinement of the crystal structure of gypsum CaSO4-2H2O. Acta Crystallographica B, 30, 921-929 .CrossRefGoogle Scholar
Follner, S., Wolter, A., Helming, K., Silber, C., Bartels, H. and Follner, H. (2002a) On the real structure of gypsum crystals. Crystal Research and Technology, 37, 207-218 .3.0.CO;2-L>CrossRefGoogle Scholar
Follner, S., Wolter, A., Preusser, A., Indris, S., Silber, C. and Follner, H. (2002b) The setting behaviour of a- and β-CaSO4-0,5 H2O as a function of crystal structure and morphology. Crystal Research and Technology, 37, 1075 — 1087.3.0.CO;2-X>CrossRefGoogle Scholar
Gonzalez-Saborido, A. (2008) Exploitation of synchrotron techniques in cement science. PhD thesis, University of London, London.Google Scholar
Greaves, R.I. (2009) Innovative methods to increase the usability of by-product gypsum from titanium dioxide manufacture. PhD thesis, University of London, London.Google Scholar
Kirfel, A. and Will, B. (1980) Charge density in anhydrite, CaSO4, from X-ray and neutron diffraction measurements. Acta Crystallographica B, 36, 2881—2890.Google Scholar
Kuzel, H.J. and Hauner, M. (1987) Chemical and crystallographic properties of calcium sulphate hemihydrate and anhydrite III. Zement-Kalk-Gips International, 40, 628—632.Google Scholar
Lager, G.A., Ambruster, T., Rotella, F.J., Jorgensen, J.D. and Hinks, D.G. (1984) A crystallographic study of the low-temperature dehydration products of gypsum, CaSO4-2H2O; hemihydrate CaSO4-0.5H2O, and γ-CaSO4. American Mineralogist, 69, 910—919.Google Scholar
Le Bail, A. (2005) Whole powder pattern decomposition methods and applications — A retrospection. Powder Diffraction, 20, 316—326.Google Scholar
Rietveld, H.M. (1969) A profile refinement method for nuclear and magnetic structures. Journal of Applied Crystallography, 2, 65—71.CrossRefGoogle Scholar
Rodnguez-Carvajal, J. (1993) Recent advances in magnetic structure determination by neutron powder diffraction. Physica B: Condensed Matter, 192, 55—69.Google Scholar
Roisnel, T. and Rodnguez-Carvajal, J. (2000) WinPLOTR: a Windows tool for powder diffraction patterns analysis. Materials Science Forum, Proceedings of the Seventh European Powder Diffraction Conference (EPDIC 7), 118 — 123.Google Scholar
Scheidegger, F. (1990) Aus der Geschichte der Bautechnik. Birkhauser, Basel, 211 pp.Google Scholar
Stark, J. and Wicht, B. (1999) The history of gypsum and gypsum plaster. Zement-Kalk-Gips International, 52, 527—533.Google Scholar
Wooster, W.A. (1936) On the crystal structure of gypsum CaSO4(H2O)2. Zeitschrift für Kristallographie, Kristallgeometrie, Kristallphysik, Kristallchemie, 94, 375—396.Google Scholar