I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[4911]
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Feb 2011
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[1125]
Abstract: Disregulation of transition metal ions is implicated in many neurodegenerative disorders,
and altered status may both affect disease progression and hold biomarker potential. The analytical
challenges in this field often lead to isolated evidence for altered concentration, distribution, chemical or
mineral state, limiting the conclusions that can be drawn. Combining methods that are highly sensitive to
a range of these properties can give new insight.
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Mar 2011
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I18-Microfocus Spectroscopy
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Mar 2011
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I18-Microfocus Spectroscopy
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Mar 2011
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I18-Microfocus Spectroscopy
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Jun 2011
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I18-Microfocus Spectroscopy
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Open Access
Abstract: The preservation of waterlogged archaeological wooden finds, such as Henry VIII's flagship the Mary Rose[1], [2] and [3], is complicated by the biological, chemical, and mechanical changes induced from prolonged exposure to a marine environment. Of particular concern are sulfur species that form acidic compounds that attack wood4. Here we show that different sulfur compounds do not form acids at the same rate or pathway and propose a preservation strategy of applying SrCO3 nanoparticles. These nanoparticles not only neutralize problematic sulfuric acid, but also reduced sulfur compounds, such as sulfur and pyrite, which pose a long term threat. This is the first treatment that eliminates acidification at the root. Although this strategy was devised for the Mary Rose, it could be employed to preserve any archaeological organic artifact rich in problematic sulfur, from sunken ships and silk tapestries to ancient texts and parchments.
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Jul 2011
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[614]
Abstract: We report R2 and R2* in human hippocampus from five unfixed post-mortem Alzheimer's disease (AD) and three age-matched control cases. Formalin-fixed tissues from opposing hemispheres in a matched AD and control were included for comparison. Imaging was performed in a 600 MHz (14 T) vertical bore magnet at MR microscopy resolution to obtain R2 and R2* (62 ?m × 62 ?m in-plane, 80 ?m slice thickness), and R1 at 250 ?m isotropic resolution. R1, R2 and R2* maps were computed for individual slices in each case, and used to compare subfields between AD and controls. The magnitudes of R2 and R2* changed very little between AD and control, but their variances in the Cornu Ammonis and dentate gyrus were significantly higher in AD compared for controls (p < 0.001). To investigate the relationship between tissue iron and MRI parameters, each tissue block was cryosectioned at 30 ?m in the imaging plane, and iron distribution was mapped using synchrotron microfocus X-ray fluorescence spectroscopy. A positive correlation of R2 and R2* with iron was demonstrated. While studies with fixed tissues are more straightforward to conduct, fixation can alter iron status in tissues, making measurement of unfixed tissue relevant. To our knowledge, these data represent an advance in quantitative imaging of hippocampal subfields in unfixed tissue, and the methods facilitate direct analysis of the relationship between MRI parameters and iron. The significantly increased variance in AD compared for controls warrants investigation at lower fields and in-vivo, to determine if this parameter is clinically relevant.
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Aug 2011
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[4861]
Abstract: The deposition of gold at the interface between immiscible electrolyte solutions has been investigated using reduction of tetrachloroaurate or tetrabromoaurate in 1,2-dichloroethane, with aqueous phase hexacyanoferrate as reducing agent. In a clean environment without defects present at the interface, the Au(III) complex was reduced to the Au(I) complex, but no solid phase formation could be observed. A deposition process could only be observed through the addition of artificial nucleation sites in the form of palladium nanoparticles at the interface. This process could be associated with the reduction of the Au(I) halide complex to metallic gold, by determining the gold reduction potentials in 1,2-dichloroethane. XANES measurements indicate that tetrachloroaurate ion transfers intact into the organic phase, with the central Au atom retaining its oxidation state of +3 and the overall anion remaining charged at −1.
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Aug 2011
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[1493]
Abstract: Highly alkaline (pH 12.2) chromate contaminated leachate (990 ?mol L?1) has been entering soils below a chromite ore processing residue disposal (COPR) site for over 100 years. The soil immediately beneath the waste has a pH of 11 ? 12.5, contains 0.3 ? 0.5% (w/w) chromium, and 45 ? 75% of the microbially available iron is Fe(II). Despite elevated pH, a viable microbial consortium of Firmicutes dominated iron reducers was isolated from this COPR affected soil. Soil pH and Cr concentration decrease with distance from the waste. XAS analysis of soil samples indicated that Cr is present as a mixed Cr(III)–Fe(III) oxy-hydroxide phase, suggesting that the elevated soil Cr content is due to reductive precipitation of Cr(VI) by Fe(II). Microcosm results demonstrate the capacity of COPR affected soil to abiotically remove all Cr(VI) from the leachate within 40 days. In air oxidation experiments less than 2% of the total Cr in the soil was remobilised despite significant Fe(II) oxidation. XAS analysis after air oxidation showed no change in Cr-speciation, indicating the Cr(III)-containing phase is a stable long term host for Cr. This work suggests that reductive precipitation of Cr(VI) is an effective method of contaminant immobilisation in soils where microbially produced Fe(II) is present.
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Aug 2011
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I18-Microfocus Spectroscopy
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Diamond Proposal Number(s):
[6769]
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Aug 2011
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