Characterisation of commercial ionomer glasses using magic angle nuclear magnetic resonance (MAS-NMR)

Abstract

Five commercial ionomer glasses (Fuji IX, Ketac Molar, G338, G2, and G2SR) used to produce glass (ionomer) polyalkenoate dental cements were studied. 29Si, 27Al, 31P and 19F magic angle spinning nuclear magnetic resonance (MAS-NMR) Spectroscopy was used to characterise the glasses and the resulting spectra compared with previous studies of model glasses. The 29Si NMR spectra were consistent with Q 4(3Al) and Q 4(4Al) units being present and agreed with the low non-bridging oxygen contents calculated from the elemental composition. The 27Al NMR spectra typically exhibited three distinct sites at 45–60, 20 and 0 ppm which have been attributed to Al(IV), Al(V) and Al(VI) coordinate aluminium. The presence of Al(V) and Al(VI) are consistent with previous studies of model ionomer glasses. The 31P spectra all exhibited a chemical shift between −8 and −23 ppm with the exception of the Ketac Molar glass, which exhibited a peak at 2–3 ppm consistent with orthophosphate. The chemical shift of 31P in the range −8 to −23 ppm indicates a PO 4 tetrahedra surrounded by 1–4 Al moieties. The 19F NMR spectra indicated the presence of Al–F–Ca( n) in the G2 and G338 glasses, Al–F–Sr( n) in the G2SR and Fuji IX glasses and crystalline CaF 2, LaF 3, Al–F–Ca( n) in the Ketac Molar glass. The G338 glass with a high non-bridging oxygen content showed the presence of a F–Ca( n) species. There was also present in all the glasses a peak corresponding to Al–F–Na( n). The intensity of this peak was approximately proportional to the sodium content.