Due to their short wavelength, X-rays can in principle be focused down to a few nanometres and below. At the same time, it is this short wavelength that puts stringent requirements on X-ray optics and their metrology. Both are limited by today's technology. In this work, we present accurate at wavelength measurements of residual aberrations of a refractive X-ray lens using ptychography to manufacture a corrective phase plate. Together with the fitted phase plate the optics shows diffraction-limited performance, generating a nearly Gaussian beam profile with a Strehl ratio above 0.8. This scheme can be applied to any other focusing optics, thus solving the X-ray optical problem at synchrotron radiation sources and X-ray free-electron lasers.
Chelation of iron and zinc in wheat as phytates lowers their bio-accessibility. Steeping and germination (15 °C, 120 h) lowered phytate content from 0.96% to only 0.81% of initial dry matter. A multifactorial experiment in which (steeped/germinated) wheat was subjected to different time (2-24 h), temperature (20-80 °C) and pH (2.0-8.0) conditions showed that hydrothermal processing of germinated (15 °C, 120 h) wheat at 50 °C and pH 3.8 for 24 h reduced phytate content by 95%. X-ray absorption near-edge structure imaging showed that it indeed abolished chelation of iron to phytate. It also proved that iron was oxidized during steeping, germination and hydrothermal processing. It was further shown that zinc and iron bio-accessibility were respectively 3 and 5% in wheat and 27 and 37% in hydrothermally processed wheat. Thus, hydrothermal processing of (germinated) wheat paves the way for increasing elemental bio-accessibility in whole grain-based products.
A combination of X-ray ptychography and X-ray fluorescence tomography (XRF) has been used to study the fragmentation behavior of an individual Ziegler−Natta catalyst particle, ∼40 μm in diameter, in the early stages of propylene polymerization with submicron spatial resolution. The electron density signal obtained from X-ray ptychography gives the composite phases of the Ziegler−Natta catalyst particle fragments and isotactic polypropylene, while 3-D XRF visualizes multiple isolated clusters, rich in Ti, of several microns in size. The radial distribution of Ti species throughout the polymer−catalyst composite particle shows that the continuous bisection fragmentation model is the main contributor to the fragmentation pathway of the catalyst particle as a whole. Furthermore, within the largest Ti clusters the fragmentation pathway was found to occur through both the continuous bisection and layer-by-layer models. The fragmentation behavior of polyolefin catalysts was for the first time visualized in 3-D by directly imaging and correlating the distribution of the Ti species to the polymer−catalyst composite phase.
Catalyst deactivation involves a complex interplay of processes taking place at different length and time scales. Understanding this phenomenon is one of the grand challenges in solid catalyst characterization. A process contributing to deactivation is carbon deposition (i. e., coking), which reduces catalyst activity by limiting diffusion and blocking active sites. However, characterizing coke formation and its effects remains challenging as it involves both the organic and inorganic phase of the catalytic process and length scales from the atomic scale to the scale of the catalyst body. Here we present a combination of hard X-ray imaging techniques able to visualize in 3-D the distribution, effect and nature of carbon deposits in the macropore space of an entire industrially used catalyst particle. Our findings provide direct evidence for coke promoting effects of metal poisons, pore clogging by coke, and a correlation between carbon nature and its location. These results provide a better understanding of the coking process, its relation to catalyst deactivation and new insights into the efficiency of the industrial scale process of fluid catalytic cracking.
The high brilliance of third-generation synchrotron sources increases the demand for faster detectors to utilize the available flux. The Maia detector is an advanced imaging scheme for energy-dispersive detection realising dwell times per image-pixel as low as 50 µs and count rates higher than 10 × 10 s. In this article the integration of such a Maia detector in the Microprobe setup of beamline P06 at the storage ring PETRA III at the Deutsches Elektronen-Synchrotron (DESY) in Hamburg, Germany, is described. The analytical performance of the complete system in terms of rate-dependent energy resolution, scanning-speed-dependent spatial resolution and lower limits of detection is characterized. The potential of the Maia-based setup is demonstrated by key applications from materials science and chemistry, as well as environmental science with geological applications and biological questions that have been investigated at the P06 beamline.
To improve the prognosis of glioblastoma, innovative radiotherapy regimens are required to augment the effect of tolerable radiation doses while sparing surrounding tissues. In this context, nanoscintillators are emerging radiotherapeutics that down-convert X-rays into photons with energies ranging from UV to near-infrared. During radiotherapy, these scintillating properties amplify radiation-induced damage by UV-C emission or photodynamic effects. Additionally, nanoscintillators that contain high-Z elements are likely to induce another, currently unexplored effect: radiation dose-enhancement. This phenomenon stems from a higher photoelectric absorption of orthovoltage X-rays by high-Z elements compared to tissues, resulting in increased production of tissue-damaging photo-and Auger electrons. In this study, Geant4 simulations reveal that rare-earth composite LaF 3 :Ce nanoscintillators effectively generate photo-and Auger-electrons upon orthovoltage X-rays. 3D spatially resolved X-ray fluorescence microtomography shows that LaF 3 :Ce highly concentrates in microtumors and enhances radiotherapy in an X-ray energy-dependent manner. In an aggressive syngeneic model of orthotopic glioblastoma, intracerebral injection of LaF 3 :Ce is well tolerated and achieves complete tumor remission in 15% of the subjects receiving monochromatic synchrotron radiotherapy. This study provides unequivocal evidence for radiation dose-enhancement by nanoscintillators, eliciting a prominent radiotherapeutic effect. Altogether, nanoscintillators have invaluable properties for enhancing the focal damage of radiotherapy in glioblastoma and other radioresistant cancers.
Objectives: Our first objective was to review the evidence describing the appearance and microstructure of the neonatal line and to link this with known changes in neonatal physiology occurring at and around birth. A second objective was to explore ways to improve identification of the neonatal line by mapping the pre-and postnatal distribution of Ca, Sr and Zn in deciduous cuspal enamel and superimposing these maps onto transmitted light micrographs that included a clear true section of the neonatal line. Materials and Methods: We used synchrotron X-ray fluorescence to map elemental distributions in pre-and postnatal enamel and dentine. Two deciduous canines and 5 molars were scanned with an X-ray beam monochromatised to 17.0 keV at either 10.0, 2.5 or 1.0 µm resolution and 10 ms integration time. Results: Calcium maps distinguished enamel and dentine but did not clearly demarcate tissues formed pre-or postnatally. Strontium maps reflected presumed pre-and postnatal maternal serum levels and what are likely to be diet-dependent regions of Sr enrichment or depletion. Prenatal Zn maps, particularly for dentine, mirror elevated levels in the fetus and in colostrum during the first few days of life. Conclusions: The neonatal line, enamel dentine junction and surface enamel were all Zn-rich. Within the neonatal line Zn may be associated with increased crystallinity but also with caries resistance, both of which have been reported previously. Elemental mapping may improve the identification of ambiguous NNLs and so be useful in forensic and archaeological studies.
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