I18-Microfocus Spectroscopy
Detectors
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Abstract: The long-wavelength MX beamline I23 currently under design at Diamond Light Source will be optimized in the X-ray energy range between 3 and 5 keV. At the moment no commercial off-the-shelf detector with high quantum efficiency and dynamic range is available to cover the large area required for diffraction experiments in this energy range. The hybrid pixel detector technology used in PILATUS detectors could overcome these limitations as the modular design could allow a large coverage in reciprocal space and high detection efficiency. Experiments were carried out on the Microfocus Spectroscopy beamline I18 at Diamond Light Source to test the performance of a 100K PILATUS module in the low-energy range from 2.3 to 3.7 keV.
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Jun 2010
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I18-Microfocus Spectroscopy
Detectors
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Diamond Proposal Number(s):
[6841]
Abstract: Changes in the chemical conditions of sediment following a resuspension event might lead to release of sequestered pollutants. In the present study, arsenic (As) and iron (Fe) speciation were investigated before and after such an event, in sediment from L'Estaque marina (France). This marina is located near an industrial plant which processed As-bearing ores for several decades.
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Jan 2014
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I02-Macromolecular Crystallography
I13-1-Coherence
I13-2-Diamond Manchester Imaging
I18-Microfocus Spectroscopy
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Abstract: Background: Skogsbergia lerneri (Kornicker, 1958) is a species of ostracod which, like all crustaceans, has a protective exoskeleton (or carapace). As well as being used for a protective function, the S. lerneri carapace is also transparent. Understanding how the carapace is transparent while retaining its protective function was the primary aim of this thesis.
Results: Ultrastructural analysis showed that the carapace consisted of an epicuticle, exocuticle and an endocuticle split into a calcified, crystalline endocuticle and a laminated endocuticle. Numerous structural adaptations were seen to minimise refractive index changes at the layer intersections. These layers developed along with growth of the ostracod, maintaining similar proportions throughout. Microstructural analysis identified a chitin based second harmonic generated signal from the carapace. Pixel analysis of this signal showed a consistent level of chitin expression (~60-80% of the total carapace) throughout all the developmental stages except instar 4, which showed a lower level of expression. Elemental analysis showed that the calcified, crystalline layer comprised mainly calcium, oxygen and magnesium, leading to the assumption that the structures were calcium carbonate. X-ray absorption near edge structure analysis revealed that the calcium carbonate consisted of entirely amorphous calcium carbonate in the early to middle stages of development and a mix of amorphous and aragonite in the later stages. Unlike most crustaceans, calcite was not seen in any carapaces. Optical testing showed a consistent refractive index across all stages (1.401-1.406) leading to a mean 99.94% transmission of light at the carapace surface in seawater. Spectrophotometric results showed that light transmission increased at longer wavelengths in the younger samples but maintained a consistent level by the adult stage.
Conclusions: Through the various structural adaptations of the carapace, in combination with the rare calcium carbonate polymorph distribution and its overall thinness, the S. lerneri is able to maintain its transparency without sacrificing many of its physical properties.
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Sep 2020
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I02-Macromolecular Crystallography
I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[7670, 8731, 388, 612]
Open Access
Abstract: There is evidence for iron dysregulation in many forms of disease, including a broad spectrum of neurodegenerative disorders. In order to advance our understanding of the pathophysiological role of iron, it is helpful to be able to determine in detail the distribution of iron as it relates to metabolites, proteins, cells, and tissues, the chemical state and local environment of iron, and its relationship with other metal elements. Synchrotron light sources, providing primarily X-ray beams accompanied by access to longer wavelengths such as infra-red, are an outstanding tool for multi-modal non-destructive analysis of iron in these systems. The micro- and nano-focused X-ray beams that are generated at synchrotron facilities enable measurement of iron and other transition metal elements to be performed with outstanding analytic sensitivity and specificity. Recent developments have increased the scope for methods such as X-ray fluorescence mapping to be used quantitatively rather than semi-quantitatively. Burgeoning interest, coupled with technical advances and beamline development at synchrotron facilities, has led to substantial improvements in resources and methodologies in the field over the past decade. In this paper we will consider how the field has evolved with regard to the study of iron in proteins, cells, and brain tissue, and identify challenges in sample preparation and analysis. Selected examples will be used to illustrate the contribution, and future potential, of synchrotron X-ray analysis for the characterization of iron in model systems exhibiting iron dysregulation, and for human cases of neurodegenerative disorders including Alzheimer’s disease, Parkinson’s disease, Friedreich’s ataxia, and amyotrophic lateral sclerosis.
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Aug 2014
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I12-JEEP: Joint Engineering, Environmental and Processing
I13-2-Diamond Manchester Imaging
I18-Microfocus Spectroscopy
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Open Access
Abstract: Tomographic datasets collected at synchrotrons are becoming very large and complex, and, therefore, need to be managed efficiently. Raw images may have high pixel counts, and each pixel can be multidimensional and associated with additional data such as those derived from spectroscopy. In time-resolved studies, hundreds of tomographic datasets can be collected in sequence, yielding terabytes of data. Users of tomographic beamlines are drawn from various scientific disciplines, and many are keen to use tomographic reconstruction software that does not require a deep understanding of reconstruction principles. We have developed Savu, a reconstruction pipeline that enables users to rapidly reconstruct data to consistently create high-quality results. Savu is designed to work in an 'orthogonal' fashion, meaning that data can be converted between projection and sinogram space throughout the processing workflow as required. The Savu pipeline is modular and allows processing strategies to be optimized for users' purposes. In addition to the reconstruction algorithms themselves, it can include modules for identification of experimental problems, artefact correction, general image processing and data quality assessment. Savu is open source, open licensed and 'facility-independent': it can run on standard cluster infrastructure at any institution.
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May 2015
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I12-JEEP: Joint Engineering, Environmental and Processing
I18-Microfocus Spectroscopy
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Abstract: Atmospheric pitting corrosion of stainless steel was studied to determine pit growth mechanisms and kinetics. Inkjet printing of chloride was used to investigate the growth of atmospheric corrosion pits. It has been shown that the pit size increases with increasing chloride deposition density, as well as increases with increasing deposit diameter.
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Aug 2013
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I12-JEEP: Joint Engineering, Environmental and Processing
I18-Microfocus Spectroscopy
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Abstract: In the Belgian supercontainer concept, a carbon steel overpack will surround high-level waste and spent fuel containers and be encased in a cementitious buffer material. A programme of research has been carried out to investigate and measure the rate of anaerobic corrosion of carbon steel in an artificial alkaline porewater that simulates the aqueous phase in the cementitious buffer material and also in solid cement matrices. This paper highlights the main features of the programme and presents some recent results from the analysis of several samples, including two 20-year-old steel in cement samples, which showed that under anoxic conditions there is no localised corrosion or incorporation of iron into the surrounding cement, even in the presence of 20 000 ppm chloride in the porewater.
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Aug 2017
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I13-1-Coherence
I18-Microfocus Spectroscopy
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Peter G.
Martin
,
Marion
Louvel
,
Silvia
Cipiccia
,
Christopher P.
Jones
,
Darren J.
Batey
,
Keith R.
Hallam
,
Ian A. X.
Yang
,
Yukihiko
Satou
,
Christoph
Rau
,
J. Fred W.
Mosselmans
,
David
Richards
,
Thomas B.
Scott
Diamond Proposal Number(s):
[16701, 16702, 18186]
Open Access
Abstract: Here we report the results of multiple analytical techniques on sub-mm particulate material derived from Unit 1 of the Fukushima Daiichi Nuclear Power Plant to provide a better understanding of the events that occurred and the environmental legacy. Through combined x-ray fluorescence and absorption contrast micro-focused x-ray tomography, entrapped U particulate are observed to exist around the exterior circumference of the highly porous Si-based particle. Further synchrotron radiation analysis of a number of these entrapped particles shows them to exist as UO2—identical to reactor fuel, with confirmation of their nuclear origin shown via mass spectrometry analysis. While unlikely to represent an environmental or health hazard, such assertions would likely change should break-up of the Si-containing bulk particle occur. However, more important to the long-term decommissioning of the reactors at the FDNPP (and environmental clean-upon), is the knowledge that core integrity of reactor Unit 1 was compromised with nuclear material existing outside of the reactors primary containment.
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Jun 2019
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I13-1-Coherence
I18-Microfocus Spectroscopy
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Abstract: The results of Chap. 9 identified the existence of a number of micron-scale particles of considerable density contained within the CF-01 (Unit 1) ejecta particulate. In addition to these surface and sub-surface fragments, Cs (as well as other elements, including Pb, Sr and Zr) were observed to be strongly-heterogeneous—located as spatially discontinuous regions at elevated concentrations. Despite exhibiting a spatially heterogeneous occurrence of these elements (within the Si-based particle)—the location of such constituents was shown to be concentrated greatest around the exterior circumference of the sub-mm sample.
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Apr 2019
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I13-1-Coherence
I18-Microfocus Spectroscopy
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Abstract: In addition to the micron and sub-micron scale atmospheric particulate identified through combined electron microscopy and characteristic x-ray (EDS) analysis (as described formerly within Chap. 8), a suite of considerably larger particles were also released into the environment—the analysis of which is herein described.
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Apr 2019
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