I18-Microfocus Spectroscopy
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Abstract: The salt films formed on metal surfaces dissolving inside artificial corrosion pits formed in 1 M HCl have been probed with synchrotron X-ray diffraction. NiCl2 · 6H2O is the main phase in the salt film on nickel, whereas salt films on both iron and 316 L stainless steel are predominantly FeCl2 · 4H2O. However, the salt film on iron has a very fine homogeneous crystallite size whereas that on stainless steel is much coarser. The potential-dependence of the film formed on iron has been determined.
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Feb 2008
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I18-Microfocus Spectroscopy
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J. Frederick W.
Mosselmans
,
Paul
Quinn
,
Andy
Dent
,
Stuart
Cavill
,
Sofia
Diaz-moreno
,
Andy
Peach
,
Pete
Leicester
,
Stephen
Keylock
,
Simon
Gregory
,
Kirk
Atkinson
,
Josep
Roque Rosell
Abstract: The design and performance of the microfocus spectroscopy beamline at the Diamond Light Source are described. The beamline is based on a 27 mm-period undulator to give an operable energy range between 2 and 20.7 keV, enabling it to cover the K-edges of the elements from P to Mo and the L(3)-edges from Sr to Pu. Micro-X-ray fluorescence, micro-EXAFS and micro-X-ray diffraction have all been achieved on the beamline with a spot size of similar to 3 mu m. The principal optical elements of the beamline consist of a toroid mirror, a liquid-nitrogen-cooled double-crystal monochromator and a pair of bimorph Kirkpatrick-Baez mirrors. The performance of the optics is compared with theoretical values and a few of the early experimental results are summarized.
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Nov 2009
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I18-Microfocus Spectroscopy
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Jan 2011
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I18-Microfocus Spectroscopy
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Abstract: The structure and the electrical and magnetic properties of Mn-implanted Si, which exhibits ferromagnetic ordering at room temperature, are studied. Single-crystal n- and p-type Si wafers with high and low electrical resistivities are implanted by manganese ions to a dose of 5 × 1016 cm?2. After implantation and subsequent vacuum annealing at 850°C, the implanted samples are examined by various methods. The Mn impurity that exhibits an electric activity and is incorporated into the Si lattice in interstitial sites is found to account for only a few percent of the total Mn content. The main part of Mn is fixed in Mn15Si26 nanoprecipitates in the Si matrix. The magnetization of implanted Si is found to be independent of the electrical resistivity and the conductivity type of silicon and the type of implanted impurity. The magnetization of implanted Si increases slightly upon short-term postimplantation annealing and disappears completely upon vacuum annealing at 1000°C for 5 h. The Mn impurity in Si is shown to have no significant magnetic moment at room temperature. These results indicate that the room temperature ferromagnetism in Mn-implanted Si is likely to be caused by implantation-induced defects in the silicon lattice rather than by a Mn impurity.
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Oct 2009
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I18-Microfocus Spectroscopy
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Abstract: The Moa Bay NiCo laterite deposits, placed in the so-called MayariBaracoa ophiolitic belt (eastern Cuba), are oxide type. Despite its geological relevance and economical impact no detailed studies exist with regards to cristallochemical characterization of Ni incorporated in (or attached to) the main Ni-containing minerals forming the lateritic profile. A sample corresponding to the ore limonite horizon has been studied by microfocus Raman, micro X-ray diffraction (μXRD), electron probe micro analysis (EPMA) and synchrotron radiation microfocus X-ray absorption spectroscopy (XAS) to gain structural and chemical information on Ni. The data obtained has revealed that Ni is preferably accumulated in quantities up to 21 wt.% in lithiophoriteasbolane intermediates. The local environment of Ni shows NiMn distances ∼3.5 Å suggesting that Ni is sorbed mostly in inner-sphere complexes sitting on Mn vacancies and at the edge of the Mn layers. However it is shown that in the presence of Al the Ni is incorporated within the lithiophoriteasbolane intermediate by developing brucite-like interlayers. The understanding of Ni sorption mechanisms within the limonite horizon suggests that combined physicochemical factors such as soil porosity and pH regime have important implications for Ni mobility across the profile.
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Jun 2010
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I18-Microfocus Spectroscopy
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Abstract: Shales play an important role in many earth system processes including coastal erosion, and they form the foundations of many engineering structures. The geobiology of the interior of pyrite-containing receding shale cliffs on the coast of northeast England was examined. The surface of the weathered shales was characterised by a thin layer of disordered authigenic iron oxyhydroxides and localised acicular, platy and aggregated gypsum, which was characterised by Raman spectroscopy, XAS and SEM. These chemical changes are likely to play an important role in causing rock weakening along fractures at the micron scale, which ultimately lead to coastal retreat at the larger scale. The surface of the shale hosts a novel, low-diversity microbial community. The bacterial community was dominated by Proteobacteria, with phylotypes closely associating with Methylocella and other members of the γ-subdivision. The second largest phylogenetic group corresponded to Nitrospira. The archaeal 16S rRNA phylotypes were dominated by a single group of sequences that matched phylotypes reported from South African gold mines and possessed ammonia monooxygenase (amoA) genes. Both the phylogenetic and the mineral data show that acidic microenvironments play an important role in shale weathering, but the shale has a higher microbial diversity than previously described pyritic acid mine drainage sites. The presence of a potentially biogeochemically active microbial population on the rock surface suggests that microorganisms may contribute to early events of shale degradation and coastal erosion.
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Aug 2010
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I18-Microfocus Spectroscopy
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Abstract: We have used synchrotron Fe-XANES, XRS, microRaman, and SEM-TEM analyses of Stardust track 41 slice and track 121 terminal area slices to identify Fe oxide (magnetite-hematite and amorphous oxide), Fe-Ti oxide, and V-rich chromite (Fe-Cr-V-Ti-Mn oxide) grains ranging in size from 200 nm to ∼10 μm. They co-exist with relict FeNi metal. Both Fe-XANES and microRaman analyses suggest that the FeNi metal and magnetite (Fe2O3FeO) also contain some hematite (Fe2O3). The FeNi has been partially oxidized (probably during capture), but on the basis of our experimental work with a light-gas gun and microRaman analyses, we believe that some of the magnetite-hematite mixtures may have originated on Wild 2. The terminal samples from track 121 also contain traces of sulfide and Mg-rich silicate minerals. Our results show an unequilibrated mixture of reduced and oxidized Fe-bearing minerals in the Wild 2 samples in an analogous way to mineral assemblages seen in carbonaceous chondrites and interplanetary dust particles. The samples contain some evidence for terrestrial contamination, for example, occasional Zn-bearing grains and amorphous Fe oxide in track 121 for which evidence of a cometary origin is lacking.
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Feb 2010
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[879]
Abstract: To have any hope of affecting the course of Parkinson's disease, early diagnosis is essential. Rachel Jones assesses progress so far.
When a patient is diagnosed with Parkinson's disease, they usually have two or three of the cardinal symptoms: resting tremor, rigidity and bradykinesia (slowed movement). By this stage, however, they have probably had the disease for years and up to four-fifths of the dopamine-producing neurons in the substantia nigra have been lost. There is currently no way to reverse this damage, but what if doctors could diagnose Parkinson's disease earlier, before so much harm has been done?
The search is on for a biomarker for early Parkinson's disease — a test that can reliably and specifically predict which patients are going to develop the disease while they are still in the early stages (Box 1). Such a biomarker would have several benefits: patients could be warned that they are likely to develop Parkinson's disease; longitudinal studies of these patients could help researchers develop treatments to slow or even halt the progression of the disease; and, if such treatments were to be developed, a reliable biomarker could allow treatment to begin earlier.
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Aug 2010
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[684]
Abstract: X-ray absorption near-edge structure (XANES) spectroscopy was used to examine the oxidation state of Zn, Fe and Cu in 22 normal and 23 tumour regions spread over 30 formalin-fixed, paraffin-embedded tissue samples of human primary invasive breast cancer. A micro-mapping analysis of the metal distribution in the tissue was performed prior to the XANES analysis to identify and localise the metals in the tumour and normal tissue regions. The aim of this study was to identify the oxidation state of Zn, Fe and Cu in normal and tumour tissues of the breast, in order to correlate the oxidation state of these elements with the carcinogenesis process. The position of the Zn K-edge in normal and tumour tissues suggests that Zn exists in a bounded form. The shape of the Cu K-edge XANES spectra and the first derivative spectra of normal and tumour tissues shows that a significant portion of the total copper is present as Cu (I). Nevertheless, the position of the edges in the normal and tumour tissue spectra does not exclude the presence of Cu (II). The shape and position of both normal and tumour regions of the tissue suggest that they contain mixtures of Fe (II) and Fe (III) ions with a significant fraction being Fe (III). However, normal tissue regions were found to have a higher fraction of Fe (II) compared to the tumour tissues. In order to estimate the best target for therapy, more information is required about the relative abundance of Zn, Fe and Cu binding proteins, their oxidation state and their localisation at the subcellular level. Copyright © 2010 John Wiley & Sons, Ltd.
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Aug 2010
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I18-Microfocus Spectroscopy
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Mary
Finnegan
,
Joanna
Collingwood
,
Jon
Dobson
,
Vijay
Antharam
,
Albina
Mikhailova
,
Mark
Davidson
,
JP
Bullivant
,
John
Forder
,
Chris
Batich
,
Naomi
Visanji
,
Fred
Mosselmans
,
Paul
Quinn
Diamond Proposal Number(s):
[4911]
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Jun 2010
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