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The main mineral component of bone is hydroxyapatite, a commonly nanocrystalline material which presents many challenges for those trying to characterize it. Here, local structure is analyzed using X-ray total scattering for synthetic samples, to enable a better understanding of the nanocrystalline nature of hydroxyapatite. Two samples were measured dynamically during heat treatment from 25°C to 800°C, and were analyzed using small box modelling. Analysis of sequential measurements when dwelling at key temperatures showed a significant relationship between time and temperature, indicating a process occurring more slowly than thermal expansion. This indicates a decrease in B-type CO32- substitution between 550°C and 575°C and an increase in A-type CO32- substitution above 750°C. A greater understanding of local, intermediate, and long-range order of this complex biomineral during heat treatment can be of interest in several sectors, such as in forensic, biomedical and clinical settings for the study of implant coatings and bone diseases including osteoporosis and osteoarthritis. Engineering and Physical Sciences Research Council (EPSRC): EP/T034238/1. This work was also partly supported by a Royal Society and Wolfson Foundation (RSWF/R1/180012). This work was carried out with the support of the Diamond Light Source, instrument I15-1 (proposal cy24283).

Hy­droxy­apatite (HA) is a com­plex material, which is often nanocrystalline when found within a biological setting. This work has directly com­pared the structural characteristics derived from data collected using a conventional laboratory-based X-ray diffractometer with those collected from a dedicated pair distribution function (PDF) beamline at Diamond Light Source. In particular, the application of PDF analysis methods to carbonated HA is evaluated. 20 synthetic samples were measured using both X-ray diffraction (XRD) and PDFs. Both Rietveld refinement (of laboratory XRD data) and real-space refinement (of PDF data) were used to analyse all samples. The results of Rietveld and real-space refinements were com­pared to evaluate their application to crystalline and nanocrystalline hy­droxy­apatite. Significant relationships were observed between real-space refinement parameters and increasing carbonate substitution. Understanding the local order of synthetic hy­droxy­apatite can benefit several fields, including both biomedical and clinical settings. Engineering and Physical Sciences Research Council (EPSRC): EP/T034238/1. Royal Society Wolfson Fellowship: RSWF/R1/180012. Diamond Light Source, instrument I15-1: proposal ee18638.