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Instruments / Technical Area	Publication Details	Published
I15-1-X-ray Pair Distribution Function (XPDF)	New insights into the application of pair distribution function studies to biogenic and synthetic hydroxyapatites Emily L. Arnold , Dean S. Keeble , Charlene Greenwood , Keith Rogers Scientific Reports 10 DOI: 10.1038/s41598-020-73200-2 Diamond Proposal Number(s): [18638, 23164] Open Access Show Abstract ▼ Abstract: Biogenic and synthetic hydroxyapatites are confounding materials whose properties remain uncertain, even after years of study. Pair distribution function (PDF) analysis was applied to hydroxyapatites in the 1970’s and 1980’s, but this area of research has not taken full advantage of the relatively recent advances in synchrotron facilities. Here, synchrotron X-ray PDF analysis is compared to techniques commonly used to characterise hydroxyapatite (such as wide angle X-ray scattering, Fourier-transform infrared spectroscopy and thermogravimetric analysis) for a range of biogenic and synthetic hydroxyapatites with a wide range of carbonate substitution. Contributions to the pair distribution function from collagen, carbonate and finite crystallite size were examined through principal component analysis and comparison of PDFs. Noticeable contributions from collagen were observed in biogenic PDFs when compared to synthetic PDFs (namely r < 15 Å), consistent with simulated PDFs of collagen structures. Additionally, changes in local structure were observed for PDFs of synthetic hydroxyapatites with differing carbonate content, notably in features near 4 Å, 8 Å and 19 Å. Regression models were generated to predict carbonate substitution from peak position within the PDFs.	Nov 2020
I18-Microfocus Spectroscopy	Calcification microstructure reflects breast tissue microenvironment Sarah Gosling , Robert Scott , Charlene Greenwood , Pascaline Bouzy , Jayakrupakar Nallala , Iain D. Lyburn , Nicholas Stone , Keith Rogers Journal Of Mammary Gland Biology And Neoplasia 95 DOI: 10.1007/s10911-019-09441-3 Diamond Proposal Number(s): [12303] Open Access Show Abstract ▼ Abstract: Microcalcifications are important diagnostic indicators of disease in breast tissue. Tissue microenvironments differ in many aspects between normal and cancerous cells, notably extracellular pH and glycolytic respiration. Hydroxyapatite microcalcification microstructure is also found to differ between tissue pathologies, including differential ion substitutions and the presence of additional crystallographic phases. Distinguishing between tissue pathologies at an early stage is essential to improve patient experience and diagnostic accuracy, leading to better disease outcome. This study explores the hypothesis that microenvironment features may become immortalised within calcification crystallite characteristics thus becoming indicators of tissue pathology. In total, 55 breast calcifications incorporating 3 tissue pathologies (benign – B2, ductal carcinoma in-situ - B5a and invasive malignancy - B5b) from archive formalin-fixed paraffin-embedded core needle breast biopsies were analysed using X-ray diffraction. Crystallite size and strain were determined from 548 diffractograms using Williamson-Hall analysis. There was an increased crystallinity of hydroxyapatite with tissue malignancy compared to benign tissue. Coherence length was significantly correlated with pathology grade in all basis crystallographic directions (P < 0.01), with a greater difference between benign and in situ disease compared to in-situ disease and invasive malignancy. Crystallite size and non-uniform strain contributed to peak broadening in all three pathologies. Furthermore, crystallite size and non-uniform strain normal to the basal planes increased significantly with malignancy (P < 0.05). Our findings support the view that tissue microenvironments can influence differing formation mechanisms of hydroxyapatite through acidic precursors, leading to differential substitution of carbonate into the hydroxide and phosphate sites, causing significant changes in crystallite size and non-uniform strain.	Dec 2019
I18-Microfocus Spectroscopy	Relationships between pathology and crystal structure in breast calcifications: an in situ X-ray diffraction study in histological sections Robert Scott , Nicholas Stone , Catherine Kendall , Kalotina Geraki , Keith Rogers Npj Breast Cancer 2 DOI: 10.1038/npjbcancer.2016.29 Diamond Proposal Number(s): [12303] Open Access Show Abstract ▼ Abstract: Calcifications are not only one of the most important early diagnostic markers of breast cancer, but are also increasingly believed to aggravate the proliferation of cancer cells and invasion of surrounding tissue. Moreover, this influence appears to vary with calcification composition. Despite this, remarkably little is known about the composition and crystal structure of the most common type of breast calcifications, and how this differs between benign and malignant lesions. We sought to determine how the phase composition and crystallographic parameters within calcifications varies with pathology, using synchrotron X-ray diffraction. This is the first time crystallite size and lattice parameters have been measured in breast calcifications, and we found that these both parallel closely the changes in these parameters with age observed in fetal bone. We also discovered that these calcifications contain a small proportion of magnesium whitlockite, and that this proportion increases from benign to in situ to invasive cancer. When combined with other recent evidence on the effect of magnesium on hydroxyapatite precipitation, this suggests a mechanism explaining observations that carbonate levels within breast calcifications are lower in malignant specimens.	Sep 2016
B16-Test Beamline	High Throughput X-ray Diffraction Analysis of Combinatorial Polycrystalline Thin Film Libraries Scilla Roncallo , Omeed Karimi , Keith Rogers , John Gregoire , David Lane , Jonathan J. Scragg , Salman Ansari Analytical Chemistry 82 (11), 45644569 DOI: 10.1021/ac100572h Show Abstract ▼ Abstract: With the increasing demand for new materials, analytical techniques which are able to rapidly characterize a large number of samples are becoming indispensable. Thin film technology has the potential to improve the amount of information contained on as-deposited samples by creating compositionally graded libraries. Conventionally, raster scan methods are used to interrogate such libraries but, in this paper, a different approach is presented to provide a method of high-throughput data collection and analysis using an X-ray diffraction (XRD) probe. An extended X-ray beam was used to illuminate the libraries, and a large area detector was used to collect the data. A new algorithm "Bandit" has been employed to analyze the collected data and extract the crystallographic information. The results of the technique have been compared with the raster scans showing that the algorithm provides reliable data at a significantly increased data acquisition speed.	May 2010

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