Solid-state NMR spectroscopy of Pb-rich apatite
Copyright 2009 John Wiley & Sons, Ltd.
| Veröffentlicht in: | Magnetic resonance in chemistry : MRC. - 1985. - 47(2009), 12 vom: 16. Dez., Seite 1062-70 |
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| 1. Verfasser: | |
| Weitere Verfasser: | , , , |
| Format: | Online-Aufsatz |
| Sprache: | English |
| Veröffentlicht: |
2009
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| Zugriff auf das übergeordnete Werk: | Magnetic resonance in chemistry : MRC |
| Schlagworte: | Journal Article |
| Zusammenfassung: | Copyright 2009 John Wiley & Sons, Ltd. Pb-containing hydroxylapatite phases synthesized under aqueous conditions were investigated by X-ray diffraction and solid-state nuclear magnetic resonance (NMR) techniques to determine the Pb, Ca distribution. 31P and 1H magic-angle spinning (MAS) NMR results indicate slight shifts of the isotropic chemical shift with increased Ca content and complex lineshapes at compositions with near equal amounts of Ca and Pb. 31P{207Pb} and 1H{207Pb} rotational-echo double resonance (REDOR) results for intermediate compositions show that resolved spectral features cannot be assigned simply in terms of local Ca, Pb configurations or coexisting phases. 207Pb MAS NMR spectra are easily obtained for these materials and contain well-resolved resonances for crystallographically unique A1 and A2 Pb sites. Splitting of the A1 and A2 207Pb resonances for pure hydroxyl-pyromorphite (Pb10(PO4)6(OH)2) compared to natural pyromorphite (Pb5(PO4)3Cl) suggests symmetry reduced from hexagonal. We find that 207Pb{1H} CP/MAS NMR is impractical in Pb-rich hydroxylapatites due to fast 207Pb relaxation |
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| Beschreibung: | Date Completed 23.02.2010 Date Revised 12.11.2009 published: Print Citation Status PubMed-not-MEDLINE |
| ISSN: | 1097-458X |
| DOI: | 10.1002/mrc.2514 |