期刊
JOURNAL OF SOLID STATE CHEMISTRY
卷 206, 期 -, 页码 192-198出版社
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jssc.2013.08.011
关键词
Crystallinity; Carbonated apatite; MAS NMR; Raman spectroscopy; Bone mineral
资金
- NIH [R01 AR052010, RR023597, R01 AR047969, T90 DK070071]
- CRIF-NSF
Solid-state (magic-angle spinning) NMR spectroscopy is a useful tool for obtaining structural information on bone organic and mineral components and synthetic model minerals at the atomic-level. Raman and P-31 NMR spectral parameters were investigated in a series of synthetic B-type carbonated apatites (CAps). Inverse P-31 NMR linewidth and inverse Raman PO43- nu(1) bandwidth were both correlated with powder XRD c-axis crystallinity over the 0.3-10.3 wt% CO32- range investigated. Comparison with bone powder crystallinities showed agreement with values predicted by NMR and Raman calibration curves. Carbonate content was divided into two domains by the P-31 NMR chemical shift frequency and the Raman phosphate nu(1) band position. These parameters remain stable except for an abrupt transition at 6.5 wt% carbonate, a composition which corresponds to an average of one carbonate per unit cell. This near-binary distribution of spectroscopic properties was also found in AFM-measured particle sizes and Ca/P molar ratios by elemental analysis. We propose that this transition differentiates between two charge-balancing ion-loss mechanisms as measured by Ca/P ratios. These results define a criterion for spectroscopic characterization of B-type carbonate substitution in apatitic minerals. (C) 2013 Elsevier Inc. All rights reserved.
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