Hard X-ray techniques suitable for polymer experiments

Polymers have been studied since 1979 with 8-12 keV synchrotron radiation X-ray scattering methods and the number and sophistication of the experiments have rapidly grown ever since. More recently, new experimental techniques have been developed that use softer or harder X rays in less conventional ways. This article provides a brief overview of the possibilities of hard X-ray techniques and indicates some areas that might gain from further developments

Recent experiments on a small-angle/wide-angle X-ray scattering beam line at the ESRF

Recent results using a new combined small-angle/wide-angle X-ray scattering (SAXS/WAXS) beam line at the European Synchrotron Radiation Source (ESRF) will be presented. This beam line is specifically designed to be able to handle complicated sample environments required to perform time-resolved experiments mimicking processing conditions used in material science. Besides the attention that has been given to the interfacing of these sample environments to the beam line data acquisition system also the developments in detector technology will be discussed. The influence that a high count rate and low noise WAXS detector can have on the accuracy of experimental results in polymer crystallisation will be shown. It is shown that it is feasible to detect crystalline volume fractions as low as 10(-3)-10(-4) in polymeric systems

Investigating the interstellar dust through the Fe K-edge

The chemical and physical properties of interstellar dust in the densest regions of the Galaxy are still not well understood. X-rays provide a powerful probe since they can penetrate gas and dust over a wide range of column densities (up to $10^{24}\ \rm{cm}^{-2}$). The interaction (scattering and absorption) with the medium imprints spectral signatures that reflect the individual atoms which constitute the gas, molecule, or solid. In this work we investigate the ability of high resolution X-ray spectroscopy to probe the properties of cosmic grains containing iron. Although iron is heavily depleted into interstellar dust, the nature of the Fe-bearing grains is still largely uncertain. In our analysis we use iron K-edge synchrotron data of minerals likely present in the ISM dust taken at the European Synchrotron Radiation Facility. We explore the prospects of determining the chemical composition and the size of astrophysical dust in the Galactic centre and in molecular clouds with future X-ray missions. The energy resolution and the effective area of the present X-ray telescopes are not sufficient to detect and study the Fe K-edge, even for bright X-ray sources. From the analysis of the extinction cross sections of our dust models implemented in the spectral fitting program SPEX, the Fe K-edge is promising for investigating both the chemistry and the size distribution of the interstellar dust. We find that the chemical composition regulates the X-ray absorption fine structures in the post edge region, whereas the scattering feature in the pre-edge is sensitive to the mean grain size. Finally, we note that the Fe K-edge is insensitive to other dust properties, such as the porosity and the geometry of the dust.Comment: 11 pages, 10 figures. Accepted for publication in Astronomy and Astrophysic

Direct observation of the high magnetic field effect on the Jahn-Teller state in TbVO4

We report the first direct observation of the influence of high magnetic fields on the Jahn-Teller (JT) transition in TbVO4. Contrary to spectroscopic and magnetic methods, X-ray diffraction directly measures the JT distortion; the splitting between the (311)/(131) and (202)/(022) pairs of Bragg reflections is proportional to the order parameter. Our experimental results are compared to mean field calculations, taking into account all possible orientations of the grains relative to the applied field, and qualitative agreement is obtained.Comment: 11 pages, 4 figures, submitted to Phys. Rev. Let

Self-Assembly of Supramolecules Consisting of Octyl Gallate Hydrogen Bonded to Polyisoprene-block-poly(vinylpyridine) Diblock Copolymers

Synchrotron radiation was used to investigate the self-assembly in two comb-shaped supramolecules systems consisting of octyl gallate (OG), i.e., 1-octyl-3,4,5-trihydroxybenzoate, hydrogen bonded to the pyridine groups of polyisoprene-block-poly(vinylpyridine) diblock copolymers. In the case of the 1,2-polyisoprene-block-poly(4-vinylpyridine)(OG)x system, self-assembly was only observed for x ≥0.5, where x denotes the number of OG molecules per pyridine group. For x = 0.5, 0.75, 1.0, and 1.2 the system self-assembled in the form of hexagonally ordered cylinders of P4VP(OG) throughout the entire temperature range of 25-200 °C investigated. For the 1,4-polyisoprene-block-poly(2-vinylpyridine)(OG)x system, on the other hand, a considerably more complex phase behavior was found, including the formation of cubic, hexagonally ordered cylinders and lamellar morphologies. In this case several order-order transitions were observed as a function of temperature, including a lamellar to lamellar transition involving a collapse of the layer thickness. The absence of hydrogen bonding between the octyl gallate molecules and the pyridine groups at elevated temperatures is argued to be a key factor for many of the phenomena observed.

How does iron interact with sporopollenin exine capsules? An X-ray absorption study including microfocus XANES and XRF imaging

Sporopollenin exine capsules (SECs) derived from plant spores and pollen grains have been proposed as adsorption, remediation and drug delivery agents. Despite many studies there is scant structural data available. This X-ray absorption investigation represents the first direct structural data on the interaction of metals with SECs and allows elucidation of their structure–property relationships. Fe K-edge XANES and EXAFS data have shown that the iron local environment in SECs (derived from Lycopodium clavatum) reacted with aqueous ferric chloride solutions is similar to that of ferrihydrite (FeOOH) and by implication ferritin. Fe Kα XRF micro-focus experiments show that there is a poor correlation between the iron distribution and the underlying SEC structure indicating that the SEC is coated in the FeOOH material. In contrast, the Fe Kα XRF micro-focus experiments on SECs reacted with aqueous ferrous chloride solutions show that there is a very high correlation between the iron distribution and the SEC structure, indicating a much more specific form of interaction of the iron with the SEC surface functional groups. Fe K-edge XANES and EXAFS data show that the FeII can be easily oxidised to give a structure similar to, but not identical to that in the FeIII case, and that even if anaerobic conditions are used there is still partial oxidation to FeIII

Past, present and future—sample environments for materials research studies in scattering and spectroscopy; a UK perspective

Small angle x-ray scattering and x-ray absorption fine structure are two techniques that have been employed at synchrotron sources ever since their inception. Over the course of the development of the techniques, the introduction of sample environments for added value experiments has grown dramatically. This article reviews past successes, current developments and an exploration of future possibilities for these two x-ray techniques with an emphasis on the developments in the United Kingdom between 1980–2020

Arrival of new great salinity anomaly weakens convection in the Irminger Sea

© The Author(s), 2022. This article is distributed under the terms of the Creative Commons Attribution License. The definitive version was published in Biló, T., Straneo, F., Holte, J., & Le Bras, I. Arrival of new great salinity anomaly weakens convection in the Irminger Sea. Geophysical Research Letters, 49(11), (2022): e2022GL098857, https://doi.org/10.1029/2022gl098857.The Subpolar North Atlantic is prone to recurrent extreme freshening events called Great Salinity Anomalies (GSAs). Here, we combine hydrographic ocean analyses and moored observations to document the arrival, spreading, and impacts of the most recent GSA in the Irminger Sea. This GSA is associated with a rapid freshening of the upper Irminger Sea between 2015 and 2020, culminating in annually averaged salinities as low as the freshest years of the 1990s and possibly since 1960. Upon the GSA propagation into the Irminger Sea over the Reykjanes Ridge, the boundary currents rapidly advected its signal around the basin within months while fresher waters slowly spread and accumulated into the interior. The anomalies in the interior freshened waters produced by deep convection during the 2017–2018 winter and actively contributed to the suppression of deep convection in the following two winters.We gratefully acknowledge the US National Science Foundation for funding this work under grants OCE-1258823, OCE-1756272, OCE-1948335, and OCE-2038481

The Chihuahua dog: A new animal model for neuronal ceroid lipofuscinosis CLN7 disease?

Neuronal ceroid lipofuscinoses (NCLs) are a group of incurable lysosomal storage disorders characterized by neurodegeneration and accumulation of lipopigments mainly within the neurons. We studied two littermate Chihuahua dogs presenting with progressive signs of blindness, ataxia, pacing, and cognitive impairment from 1 year of age. Because of worsening of clinical signs, both dogs were euthanized at about 2 years of age. Postmortem examination revealed marked accumulation of autofluorescent intracellular inclusions within the brain, characteristic of NCL. Whole-genome sequencing was performed on one of the affected dogs. After sequence alignment and variant calling against the canine reference genome, variants were identified in the coding region or splicing regions of four previously known NCL genes (CLN6, ARSG, CLN2 [=TPP1], and CLN7 [=MFSD8]). Subsequent segregation analysis within the family (two affected dogs, both parents, and three relatives) identified MFSD8:p.Phe282Leufs13*, which had previously been identified in one Chinese crested dog with no available ancestries, as the causal mutation. Because of the similarities of the clinical signs and histopathological changes with the human form of the disease, we propose that the Chihuahua dog could be a good animal model of CLN7 disease