ID23-2 is a fixed-energy (14.2 keV) microfocus beamline at the European Synchrotron Radiation Facility (ESRF) dedicated to macromolecular crystallography. The optics and sample environment have recently been redesigned and rebuilt to take full advantage of the upgrade of the ESRF to the fourth generation Extremely Brilliant Source (ESRF-EBS). The upgraded beamline now makes use of two sets of compound refractive lenses and multilayer mirrors to obtain a highly intense (>1013 photons s-1) focused microbeam (minimum size 1.5 µm × 3 µm full width at half-maximum). The sample environment now includes a FLEX-HCD sample changer/storage system, as well as a state-of-the-art MD3Up high-precision multi-axis diffractometer. Automatic data reduction and analysis are also provided for more advanced protocols such as synchrotron serial crystallographic experiments.
The generation of fully coherent and femtosecond time-scale radiation pulses in the X-ray regime is one of the most common demands of ring-based synchrotron light source users. In this paper, a method that utilizes the recent proposed angular dispersion induced microbunching technique to convert external light from high-harmonic generation (HHG) to coherent light at shorter wavelength is proposed. Numerical simulations using the practical parameters of a diffraction-limited storage ring demonstrate the generation of coherent pulse trains with photon energy as high as 2 keV, pulse duration as short as ∼10 fs and high peak brightness directly from an HHG source at 13 nm.
The solution-state interactions of plutonium and berkelium with the octadentate chelator 3,4,3-LI(1,2-HOPO) (343-HOPO) were investigated and characterized by X-ray absorption spectroscopy, which revealed in situ reductive decomposition of the tetravalent species of both actinide metals to yield Pu(III) and Bk(III) coordination complexes. X-ray absorption near-edge structure (XANES) measurements were the first indication of in situ synchrotron redox chemistry as the Pu threshold and white-line position energies for Pu-343-HOPO were in good agreement with known diagnostic Pu(III) species, whereas Bk-343-HOPO results were found to mirror the XANES behavior of Bk(III)-DTPA. Extended X-ray absorption fine structure results revealed An-OHOPO bond distances of 2.498 (5) and 2.415 (2) Å for Pu and Bk, respectively, which match well with bond distances obtained for trivalent actinides and 343-HOPO via density functional theory calculations. Pu(III)- and Bk(III)-343-HOPO data also provide initial insight into actinide periodicity as they can be compared with previous results with Am(III)-, Cm(III)-, Cf(III)-, and Es(III)-343-HOPO, which indicate there is likely an increase in 5f covalency and heterogeneity across the actinide series.
An improved theoretical model to calculate the focal spot properties of coherent synchrotron radiation (SR) soft X-ray beams by combining and aligning two microchannel plates (MCPs) is presented. The diffraction patterns of the radiation behind the MCP system are simulated in the framework of the electrodynamical model of the radiation emission from two-dimensional finite antenna arrays. Simulations show that this particular optical device focuses the soft X-ray radiation in a circular central spot with a radius of ∼4 µm. The study points out that such MCP-based devices may achieve micrometre and sub-micrometre spot sizes as required by many applications in the soft X-ray range. Finally, based on experimental and theoretical results of the radiation transmission by this MCP-based device, a new method to characterize the spatial properties of brilliant SR sources is discussed.
Although the use of fluoride for root caries control is reported to be effective, the mechanism of maintaining hydroxyapatite is still unclear. This study elucidates the roles of fluoride in the recrystallization of hydroxyapatite, and the impact of calcium to maintain the abundance of hydroxyapatite on acid-challenged root dentin with a novel approach - using synchrotron radiation. Root dentin samples obtained from 40 extracted human premolars were subjected to pH challenge in combination with fluoride treatment. The effect of fluoride on hydroxyapatite regeneration on the root was investigated by using a range of fluoride concentrations (1000-5000 p.p.m.) and the EDTA-chelation technique in vitro. Synchrotron radiation X-ray micro-computed tomography and X-ray absorption spectroscopy were utilized to characterize the chemical composition of calcium species on the surface of prepared samples. The percentage of hydroxyapatite and the relative abundance of calcium species were subsequently compared between groups. The absence of calcium or fluoride prevented the complete remineralization of hydroxyapatite on the surface of early root caries. Different concentrations of fluoride exposure did not affect the relative abundance of hydroxyapatite. Sufficient potency of 1000 p.p.m. fluoride solution in promoting hydroxyapatite structural recrystallization on the root was demonstrated. Both calcium and fluoride ions are prerequisites in a caries-prone environment. Orchestration of F- and Ca2+ is required for structural homeostasis of root dentin during acid attack. Sustainable levels of F- and Ca2+ might thus be a strict requirement in the saliva of the population prone to root caries. Fluoride and calcium contribute to structural homeostasis of tooth root, highlighting that routine fluoride use in combination with calcium replenishment is recommended for maintaining dental health. This study also demonstrates that utilization of synchrotron radiation could provide a promising experimental platform for laboratory investigation especially in the dental material research field.