Rietveld structure refinement of precipitated carbonate apatite using neutron diffraction data

Biomaterials. 2004 May;25(11):2205-13. doi: 10.1016/j.biomaterials.2003.08.057.

Abstract

X-ray and time of flight neutron diffraction data, FTIR and MAS-NMR spectra, and ICP-AES and carbonate analyses have been collected from a sodium-containing carbonate apatite (CO(3) content 12.5(7)wt%). A structural model based on Holly Springs hydroxyapatite without CO(3)(2-) ions showed an apparent reduction in the PO(4) tetrahedral volume which is ascribed to CO(3)(2-) replacing PO(4)(3-) ions in the lattice. Four structural models from the literature with the CO(3)(2-) ion explicitly modelled were fitted to the neutron diffraction data by the Rietveld method. The best fit was obtained with the CO(3)(2-) ion in disorder between the mirror symmetry related faces of a vacant PO(4)(3-) site and with the normal to the plane of the CO(3)(2-) ion at approximately 30 degrees to the c-axis. This angle is consistent with results from previous polarised IR measurements on single crystals of francolite (a fluorocarbonate apatite) and human dental enamel. Further refinement of the model revealed a hitherto unknown atom site close to the unit cell origin, (possibly a water molecule). The refined hexagonal unit cell parameters from the neutron diffraction data were a=9.3446(3)A and c=6.9199(4)A.

Publication types

  • Comparative Study
  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Apatites / analysis
  • Apatites / chemistry*
  • Biocompatible Materials / chemistry*
  • Carbonates / chemistry
  • Chemical Precipitation
  • Computer Simulation
  • Crystallography
  • Materials Testing / methods*
  • Models, Chemical*
  • Models, Molecular*
  • Molecular Conformation
  • Neutron Diffraction / methods*

Substances

  • Apatites
  • Biocompatible Materials
  • Carbonates
  • carboapatite