MAS-NMR spectroscopy studies in the setting reaction of glass ionomer cements

A. Stamboulis, S. Matsuya, R. G. Hill, R. V. Law, K. Udoh, Masaharu Nakagawa, Y. Matsuya

Research output: Contribution to journalArticle

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Abstract

Objectives: The main objective is the characterisation of the setting reaction in glass ionomer cements based on experimental ionomer glasses with different fluorine content and a commercial glass ionomer cement liquid by using 13C CP/MAS-NMR, 29Si, 27Al and 31P MAS-NMR spectroscopy in order to receive information specifically about the cross-linking process. Methods: Different fluorine containing glass compositions based on 4.5SiO2-3Al2O3-1.5P2O5-(5 - z)CaO-zCaF2 where z = 0-3, were mixed with a commercially available polymer liquid to form glass ionomer cements. The cements were subjected to 27Al, 13C CP/MAS, 29Si, and 31P MAS-NMR analysis. Results: : The 27Al spectra showed clearly the formation of six-fold coordinate Al(VI), that may crosslink the carboxyl groups in the poly-acid molecules. A shift towards to more positive values of the carboxyl peak in the 13C CP/MAS-NMR spectra showed clearly the proton dissociation of the carboxyl groups. A shift towards more negative values was observed in the 29Si MAS-NMR spectra, suggesting formation of hydrated silica gel and consequently formation of additional Si-O-Si bonds. 31P MAS-NMR spectra also reflected changes in the coordination state around a PO4 3- tetrahedron. Increasing the fluorine content of the glasses resulted generally in increased reactivity during setting, due to promoting cross-linking and repolymerisation of the silicate phase, followed by clear changes in the MAS-NMR spectra. Conclusions: : The cross-linking process during the setting reaction of glass ionomer cements can be followed by MAS-NMR spectroscopy observing the conversion of Al(IV) to Al(VI). The acid base setting reaction is completed in 1 day and no further significant changes in the MAS-NMR spectra can be observed. Further study is required in order to understand the role of phosphorus.

Original languageEnglish
Pages (from-to)574-581
Number of pages8
JournalJournal of Dentistry
Volume34
Issue number8
DOIs
Publication statusPublished - Sep 1 2006
Externally publishedYes

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Glass Ionomer Cements
Fluorine
Magnetic Resonance Spectroscopy
Glass
Silicic Acid
Silicates
Acids
Phosphorus
Protons
Polymers

All Science Journal Classification (ASJC) codes

  • Dentistry(all)

Cite this

Stamboulis, A., Matsuya, S., Hill, R. G., Law, R. V., Udoh, K., Nakagawa, M., & Matsuya, Y. (2006). MAS-NMR spectroscopy studies in the setting reaction of glass ionomer cements. Journal of Dentistry, 34(8), 574-581. https://doi.org/10.1016/j.jdent.2005.08.006

MAS-NMR spectroscopy studies in the setting reaction of glass ionomer cements. / Stamboulis, A.; Matsuya, S.; Hill, R. G.; Law, R. V.; Udoh, K.; Nakagawa, Masaharu; Matsuya, Y.

In: Journal of Dentistry, Vol. 34, No. 8, 01.09.2006, p. 574-581.

Research output: Contribution to journalArticle

Stamboulis, A, Matsuya, S, Hill, RG, Law, RV, Udoh, K, Nakagawa, M & Matsuya, Y 2006, 'MAS-NMR spectroscopy studies in the setting reaction of glass ionomer cements', Journal of Dentistry, vol. 34, no. 8, pp. 574-581. https://doi.org/10.1016/j.jdent.2005.08.006
Stamboulis, A. ; Matsuya, S. ; Hill, R. G. ; Law, R. V. ; Udoh, K. ; Nakagawa, Masaharu ; Matsuya, Y. / MAS-NMR spectroscopy studies in the setting reaction of glass ionomer cements. In: Journal of Dentistry. 2006 ; Vol. 34, No. 8. pp. 574-581.
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AU - Stamboulis, A.

AU - Matsuya, S.

AU - Hill, R. G.

AU - Law, R. V.

AU - Udoh, K.

AU - Nakagawa, Masaharu

AU - Matsuya, Y.

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N2 - Objectives: The main objective is the characterisation of the setting reaction in glass ionomer cements based on experimental ionomer glasses with different fluorine content and a commercial glass ionomer cement liquid by using 13C CP/MAS-NMR, 29Si, 27Al and 31P MAS-NMR spectroscopy in order to receive information specifically about the cross-linking process. Methods: Different fluorine containing glass compositions based on 4.5SiO2-3Al2O3-1.5P2O5-(5 - z)CaO-zCaF2 where z = 0-3, were mixed with a commercially available polymer liquid to form glass ionomer cements. The cements were subjected to 27Al, 13C CP/MAS, 29Si, and 31P MAS-NMR analysis. Results: : The 27Al spectra showed clearly the formation of six-fold coordinate Al(VI), that may crosslink the carboxyl groups in the poly-acid molecules. A shift towards to more positive values of the carboxyl peak in the 13C CP/MAS-NMR spectra showed clearly the proton dissociation of the carboxyl groups. A shift towards more negative values was observed in the 29Si MAS-NMR spectra, suggesting formation of hydrated silica gel and consequently formation of additional Si-O-Si bonds. 31P MAS-NMR spectra also reflected changes in the coordination state around a PO4 3- tetrahedron. Increasing the fluorine content of the glasses resulted generally in increased reactivity during setting, due to promoting cross-linking and repolymerisation of the silicate phase, followed by clear changes in the MAS-NMR spectra. Conclusions: : The cross-linking process during the setting reaction of glass ionomer cements can be followed by MAS-NMR spectroscopy observing the conversion of Al(IV) to Al(VI). The acid base setting reaction is completed in 1 day and no further significant changes in the MAS-NMR spectra can be observed. Further study is required in order to understand the role of phosphorus.

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