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Instruments / Technical Area	Publication Details	Published
B21-High Throughput SAXS DL-SAXS-Offline SAXS and Sample Environment Development	Sample preparation of atherosclerotic plaque for SAXS/WAXS experimentation Rebecca R. Mackley , Steven Huband , Tara L. Schiller Acs Omega DOI: 10.1021/acsomega.3c00060 Diamond Proposal Number(s): [27756, 29720] Open Access Show Abstract ▼ Abstract: Atherosclerosis is often described as a single disease entity; however, the morphology of each plaque is unique to the individual. The field currently lacks a technique that can discriminate stable from unstable plaques, to identify those at risk of a thromboembolic event. Small- and wide-angle X-ray scattering (SAXS/WAXS) holds the potential to be able to identify key materials present in a plaque, such as cholesterol species, collagen, low-density lipoproteins (LDLs), and hydroxyapatite. Protocols have been established for the preparation of excised human atherosclerotic tissue that are investigated herein. This includes the fixing, sectioning, and substrate selection of the sample. Through several sample preparation methods, vast improvements have been made to sample-to-noise ratio and background subtraction.	Apr 2023
I22-Small angle scattering & Diffraction	Exploring the nanostructures accessible to an organic surfactant atmospheric aerosol proxy Adam Milsom , Adam M. Squires , Isabel Quant , Nicholas J. Terrill , Steven Huband , Ben Woden , Edna Cabrera-Martinez , Christian Pfrang The Journal Of Physical Chemistry A 2 DOI: 10.1021/acs.jpca.2c04611 Diamond Proposal Number(s): [28020, 15121] Open Access Show Abstract ▼ Abstract: The composition of atmospheric aerosols varies with time, season, location, and environment. This affects key aerosol properties such as hygroscopicity and reactivity, influencing the aerosol’s impact on the climate and air quality. The organic fraction of atmospheric aerosol emissions often contains surfactant material, such as fatty acids. These molecules are known to form three-dimensional nanostructures in contact with water. Different nanostructures have marked differences in viscosity and diffusivity that are properties whose understanding is essential when considering an aerosol’s atmospheric impact. We have explored a range of nanostructures accessible to the organic surfactant oleic acid (commonly found in cooking emissions), simulating variation that is likely to happen in the atmosphere. This was achieved by changing the amount of water, aqueous phase salinity and by addition of other commonly coemitted compounds: sugars and stearic acid (the saturated analogue of oleic acid). The nanostructure was observed by both synchrotron and laboratory small/wide angle X-ray scattering (SAXS/WAXS) and found to be sensitive to the proxy composition. Additionally, the spacing between repeat units in these nanostructures was water content dependent (i.e., an increase from 41 to 54 Å in inverse hexagonal phase d-spacing when increasing the water content from 30 to 50 wt %), suggesting incorporation of water within the nanostructure. A significant decrease in mixture viscosity was also observed with increasing water content from ∼104 to ∼102 Pa s when increasing the water content from 30 to 60 wt %. Time-resolved SAXS experiments on levitated droplets of this proxy confirm the phase changes observed in bulk phase mixtures and demonstrate that coexistent nanostructures can form in droplets. Aerosol compositional and subsequent nanostructural changes could affect aerosol processes, leading to an impact on the climate and urban air pollution.	Sep 2022
I18-Microfocus Spectroscopy	Metallic iron in cornflakes Frederik Lermyte , Wen-Ying Zhang , Jake Brooks , Steven Huband , Joanna F. Collingwood , Martin R. Lees , Margaret P. Rayman , Peter J. Sadler Food & Function 373 DOI: 10.1039/C9FO02370D Open Access Show Abstract ▼ Abstract: Iron is an essential element, and cornflake-style cereals are typically fortified with iron to a level up to 14 mg iron per 100 g. Even single cornflakes exhibit magnetic behaviour. We extracted iron microparticles from samples of two own-brand supermarket cornflakes using a strong permanent magnet. Synchrotron iron K-edge X-ray absorption near-edge spectroscopic data were consistent with identification as metallic iron, and X-ray diffraction studies provided unequivocal identification of the extracted iron as body-centred cubic (BCC) α-iron. Magnetometry measurements were also consistent with ca. 14 mg per 100 g BCC iron. These findings emphasise that attention must be paid to the speciation of trace elements, in relation to their bioavailability. To mimic conditions in the stomach, we suspended the iron extract in dilute HCl (pH 1.0–2.0) at 310 K (body temperature) and found by ICP-MS that over a period of 5 hours, up to 13% of the iron dissolved. This implies that despite its metallic form in the cornflakes, the iron is potentially bioavailable for oxidation and absorption into the body.	Mar 2020
	Crystallographic and optical study of LiNb1 − xTaxO3 S. Huband , D. S. Keeble , N. Zhang , A. M. Glazer , A. Bartasyte , P. A. Thomas Acta Crystallographica Section B Structural Science, Crystal Engineering And Materials 73, 498 - 506 DOI: 10.1107/S2052520617004711 Show Abstract ▼ Abstract: Powders of lithium niobate-tantalate across the full compositional range have been made and crystals grown using a lithium vanadate flux growth technique. The Li-content of a lithium tantalate crystal has been determined using the zero-birefringence temperature and Curie measurements, confirming the Li content is between that of congruent and stoichiometric crystals. X-ray diffraction measurements show the Nb/Ta displacement and octahedral tilt both decrease as the Ta content is increased. This also results in a decrease in the lattice parameters from lithium niobate to lithium tantalate. Birefringence measurements on the crystals as a function of temperature have been used to determine the point that the crystals become zero-birefringent, and by comparison with the structural studies have confirmed that it is not related to a phase transition and the structures remain polar through the zero-birefringence points.	Jun 2017

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