X-ray Micro-Diffraction Analysis Revealed the Crystallite Size Variation in the Neighboring Regions of a Small Bone Mass

Abstract

Applying a laboratory used X-ray micro-diffraction technique to analysis of human bone mineral, the variation of crystallite size in a small bone mass was clarified. The mandible cortical small masses were taken off by a bone trephine bar. The micro-XRD patterns showed the broaden peaks, but the full-width at half maximum (FWHM) of the 002 diffraction peak could be obtained. There were three characteristics on the FWHM values obtained in this study. First, the values showed a wide deviation range from 0.44 to 0.66 (2°), indicating the crystallite length of 12.4 nm to 18.5 nm. Second, such a small FWHM value, 0.44, was not reported previously. And third, the variation of FWHM value was observed in the closely neighboring regions within one small bone mass separated within 1 mm only. These results suggested that the crystallites in bone may vary in size from to parts due to bone remodeling and histological textures.

Anisotropic aspects of solubility behavior in the demineralization of cortical bone revealed by XRD analysis

“…Some authors have attempted to take into account the lattice microstrain contribution to the line broadening, while many authors (like we in this study) ignored this factor. That is why the data available from the references [7][8][9]36] have a rather wide range. Certainly, the variety of values depends also on the biological species where the bone has been collected [37].…”

“…where β is the line breadth of the pure diffraction profile resulting from small crystallite sizes, λ is the X-ray wavelength for CuKα and K is a constant roughly equal to unity and related to crystallite shape (shape factor). Although the Scherrer equation to some extent is limited by the uncertainties in K and β, the equation is widely used for the ease to calculate [9]. Powdered polycrystalline NaCl was used as the reference specimen free of size and distortion broadening.…”

“…Bone mineral has an apatite-like structure with hexagonal symmetry [1][2][3]. Crystals, as deduced by direct [4,5] and indirect methods [6][7][8][9], can be rod-shaped, prism-shaped, or elongated platelets with dimensions of 20 to 50 nm along the c-axis perpendicular to the basal plane of the hexagonal unit cell. As stated by many authors [10][11][12][13][14][15], bioapatite crystals in a bone possess not only shape anisotropy but also a natural texture.…”

Validated Approaches for Quantification of Bone Mineral Crystallinity Using Transmission Fourier Transform Infrared (FT-IR), Attenuated Total Reflection (ATR) FT-IR, and Raman Spectroscopy

“…It is also important to evaluate correlations including smaller crystals, since the majority of bone apatite crystals have been described as within 10–20 nm in length. 10,39…”

“…It is also important to evaluate correlations including smaller crystals, since the majority of bone apatite crystals have been described as within 10-20 nm in length. 10,39 Moreover, it is essential to consider that the current FT-IR approaches describing crystallinity were established using transmission modes, and it is unclear whether they are applicable to other sampling modes. In particular, the attenuated total reflection (ATR) FT-IR is a very straightforward sampling mode that has become increasingly attractive instead of transmission, including for the analysis of apatite crystals.…”