Journal
CALCIFIED TISSUE INTERNATIONAL
Volume 90, Issue 1, Pages 60-67Publisher
SPRINGER
DOI: 10.1007/s00223-011-9542-9
Keywords
Bone structure; Carbonated apatite; Solid state deuterium NMR spectroscopy; Structural water
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Funding
- Division Of Earth Sciences
- Directorate For Geosciences [0923224] Funding Source: National Science Foundation
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Water is well recognized as an important component in bone, typically regarded as a constituent of collagen, a pore-filling fluid in bone, and an adsorbed species on the surface of bone crystallites. The possible siting and role of water within the structure of the apatite crystallites have not been fully explored. In our experiments, carbonated hydroxyl- and fluorapatites were prepared in D2O and characterized by elemental analysis, thermal gravimetric analysis, powder X-ray diffraction, and infrared and Raman spectroscopy. Two hydroxylapatites and two fluorapatites, with widely different amounts of carbonate were analyzed by solid state H-2 NMR spectroscopy using the quadrupole echo pulse sequence, and each spectrum showed one single line as well as a low-intensity powder pattern. The relaxation time of 7.1 ms for 5.9 wt% carbonated hydroxylapatite indicates that the single line is likely due to rapid, high-symmetry jumps in translationally rigid D2O molecules, indicative of structural incorporation within the lattice. Discrimination between structurally incorporated and adsorbed water is enhanced by the rapid exchange of surface D2O with atmospheric H2O. Moreover, a H-2 resonance was observed for samples dried under a variety of conditions, including in vacuo heating to 150A degrees C. In contrast, a sample heated to 500A degrees C produced no deuterium resonance, indicating that structural water had been released by that temperature. We propose that water is located in the c-axis channels. Because structural water is observed even for apatites with very low carbonate content, some of the water molecules must lie between the monovalent ions.
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