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Serial and time-resolved macromolecular crystallography are on the rise. However, beam time at X-ray free-electron lasers is limited and most third-generation synchrotron-based macromolecular crystallography beamlines do not offer the necessary infrastructure yet. Here, a new setup is demonstrated, based on the JUNGFRAU detector and Jungfraujoch data-acquisition system, that enables collection of kilohertz serial crystallography data at fourth-generation synchrotrons. More importantly, it is shown that this setup is capable of collecting multiple-time-point time-resolved protein dynamics at kilohertz rates, allowing the probing of microsecond to second dynamics at synchrotrons in a fraction of the time needed previously. A high-quality complete X-ray dataset was obtained within 1â min from lysozyme microcrystals, and the dynamics of the light-driven sodium-pump membrane protein KR2 with a time resolution of 1â ms could be demonstrated. To make the setup more accessible for researchers, downstream data handling and analysis will be automated to allow on-the-fly spot finding and indexing, as well as data processing.
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During production of radiopharmaceuticals, the radiation situation in cyclotron pit is an important parameter, which is being monitored to ensure fulfilment of the limits and conditions of safe operation. The neutron flux in the structural components of the accelerator is also an important parameter, because the secondary neutrons are responsible for activation of cyclotron structural components and may even affect structural changes in it. This paper aims to characterize the neutron field in inner positions of medical accelerator IBA 18/9 by activation detectors and by means of scintillation spectrometry. The backward angle measurement was realized also in special liquid water target (H218O) at U120M cyclotron to confirm the data obtained in IBA 18/9 cyclotron.
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The JUNGFRAU 4-megapixel (4M) charge-integrating pixel-array detector, when operated at a full 2â kHz frame rate, streams data at a rate of 17â GBâ s-1. To operate this detector for macromolecular crystallography beamlines, a data-acquisition system called Jungfraujoch was developed. The system, running on a single server with field-programmable gate arrays and general-purpose graphics processing units, is capable of handling data produced by the JUNGFRAU 4M detector, including conversion of raw pixel readout to photon counts, compression and on-the-fly spot finding. It was also demonstrated that 30â GBâ s-1 can be handled in performance tests, indicating that the operation of even larger and faster detectors will be achievable in the future. The source code is available from a public repository.
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Programas Informáticos , Sincrotrones , Rayos X , Radiografía , Cristalografía por Rayos XRESUMEN
The inelastic neutron scattering is often followed by the emission of gamma photon. As the prompt gammas have a discrete level character they can be used for the identification of nuclides. Because of this fact, a good knowledge of photon production from inelastic scattering is important. Described research deals with the measurement of gamma originated from inelastic scattering of neutrons on 16O. The 241Am-Be was used as a neutron source because of its high average neutron energy. The oxygen in form of heavy water was used for maximization of neutron flux on oxygen and minimization of background gammas' production, namely 2223 keV gammas accompanying capture on hydrogen 1H. The gamma spectrum was measured by HPGe and the stilbene detector. The HPGe measured quantities are comparted with calculation and discrepancies between measured and calculated gamma fluxes are reported. Stilbene measurement shows indistinguishability of gamma peaks above 6 MeV.
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The diffraction endstation of the NanoMAX beamline is designed to provide high-flux coherent X-ray nano-beams for experiments requiring many degrees of freedom for sample and detector. The endstation is equipped with high-efficiency Kirkpatrick-Baez mirror focusing optics and a two-circle goniometer supporting a positioning and scanning device, designed to carry a compact sample environment. A robot is used as a detector arm. The endstation, in continued development, has been in user operation since summer 2017.
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NanoMAX is the first hard X-ray nanoprobe beamline at the MAX IV laboratory. It utilizes the unique properties of the world's first operational multi-bend achromat storage ring to provide an intense and coherent focused beam for experiments with several methods. In this paper we present the beamline optics design in detail, show the performance figures, and give an overview of the surrounding infrastructure and the operational diffraction endstation.
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Over the last decade, serial crystallography, a method to collect complete diffraction datasets from a large number of microcrystals delivered and exposed to an X-ray beam in random orientations at room temperature, has been successfully implemented at X-ray free-electron lasers and synchrotron radiation facility beamlines. This development relies on a growing variety of sample presentation methods, including different fixed target supports, injection methods using gas-dynamic virtual-nozzle injectors and high-viscosity extrusion injectors, and acoustic levitation of droplets, each with unique requirements. In comparison with X-ray free-electron lasers, increased beam time availability makes synchrotron facilities very attractive to perform serial synchrotron X-ray crystallography (SSX) experiments. Within this work, the possibilities to perform SSX at BioMAX, the first macromolecular crystallography beamline at MAX IV Laboratory in Lund, Sweden, are described, together with case studies from the SSX user program: an implementation of a high-viscosity extrusion injector to perform room temperature serial crystallography at BioMAX using two solid supports - silicon nitride membranes (Silson, UK) and XtalTool (Jena Bioscience, Germany). Future perspectives for the dedicated serial crystallography beamline MicroMAX at MAX IV Laboratory, which will provide parallel and intense micrometre-sized X-ray beams, are discussed.
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Cristalografía por Rayos X/instrumentación , Sincrotrones , Diseño de Equipo , Laboratorios , Compuestos de Silicona , Suecia , TemperaturaRESUMEN
The correct description of neutron transport in lead is an essential task for correct description of tritium production in the DEMO (DEMOnstration Power Station) breeding blanket because some concepts deal with lead as a major component: namely the WCLL (water cooled lithium lead blanket), HCLL (helium cooled lithium lead blanket), and DCLL (dual cooled lithium lead blanket). Concerning the improvement of the knowledge about the transport of fast neutrons in lead, a set of experiments and calculations was carried out to study this problem with a well-defined neutron beam. The neutron flux behind various lead arrangements positioned along the beam axis was measured using a stilbene scintillation crystal (10â¯mmâ¯×â¯10â¯mm) with neutron and gamma pulse shape discrimination. The measurement was performed along the beam axis and in the case of the thick target also above the axis, to estimate the neutron angular scatter in lead. The calculations were realized using MCNP6 with various nuclear data libraries. Discrepancies in the angular distribution description in the energy region of about 1â¯MeV were discovered by these experiments.
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The neutron flux distribution behind a reactor pressure vessel (RPV) is an important parameter that is monitored to determine neutron fluence in the RPV. Together with mechanical testing of surveillance specimens, these are the most important parts of in-service inspection programs that are essential for a realistic and reliable assessment of the RPV residual lifetime. The fast neutron fluence values are determined by a calculation. These calculation results are accompanied by measurements of induced activities of the activation foils placed in the capsules behind the RPV at selected locations, namely in azimuthal profile. In case of discrepancies between the measured and calculated activities of the activation foils placed behind the pressure vessel, it is difficult to determine the source of the deviation. During such analysis, there arises a question on the influence of power peaking near core boundary on neutron profile behind the RPV. This paper compares the calculated and measured increase of the neutron flux density distribution behind the reactor pressure vessel in the azimuthal profile that has arisen from the replacement of 164 fuel pins located close to reactor internals by pins with the higher enrichment. This work can be understood as the first step in the characterization of the effect of incorrectly calculated pin power or burn-up in the fuel assembly at the core boundary relative to the neutron flux distribution behind reactor pressure vessel. Based on a good agreement between the calculated and experimental values, it can be concluded that the mathematical model used to evaluate the power increase is correct.
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TiO2 as nanostructured powders were prepared by (1) sol-gel process and (2) hydrothermal method in combination with (A) the processing by pressurized hot water and methanol or (B) calcination. The subsequent synthesis step was the modification of prepared nanostructured TiO2 with nitrogen using commercial urea. Textural, structural, surface and optical properties of prepared TiO2 and N/TiO2 were characterized by nitrogen physisorption, powder X-ray diffraction, X-ray photoelectron spectroscopy and DR UV-vis spectroscopy. It was revealed that TiO2 and N/TiO2 processed by pressurized fluids showed the highest surface areas. Furthermore, all prepared materials were the mixtures of major anatase phase and minor brookite phase, which was in nanocrystalline or amorphous (as nuclei) form depending on the applied preparation method. All the N/TiO2 materials exhibited enhanced crystallinity with a larger anatase crystallite-size than undoped parent TiO2. The photocatalytic activity of the prepared TiO2 and N/TiO2 was tested in the photocatalytic reduction of CO2 and the photocatalytic decomposition of N2O. The key parameters influencing the photocatalytic activity was the ratio of anatase-to-brookite and character of brookite. The optimum ratio of anatase-to-brookite for the CO2 photocatalytic reduction was determined to be about 83 wt.% of anatase and 17 wt.% of brookite (amorphous-like) (TiO2-SG-C). The presence of nitrogen decreased a bit the photocatalytic activity of tested materials. On the other hand, TiO2-SG-C was the least active in the N2O photocatalytic decomposition. In the case of N2O photocatalytic decomposition, the modification of TiO2 crystallites surface by nitrogen increased the photocatalytic activity of all investigated materials. The maximum N2O conversion (about 63 % after 18 h of illumination) in inert gas was reached over all N/TiO2.
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A well-defined neutron spectrum is an essential tool not only for calibration and testing of neutron detectors used in dosimetry and spectroscopy but also for validation and verification of evaluated cross sections. A new evaluation of thermal-neutron induced 235U PFNS was performed by the International Atomic Energy Agency (IAEA) in the CIELO (Collaborative International Evaluated Library Organisation Project) project; new measurements of Spectral Averaged Cross sections averaged in the evaluated spectrum are to be obtained. In general, a neutron spectrum in the core is not identical to the pure fission one because fission neutrons undergo many scattering reactions, but it can be shown that PFNS and reactor spectra become undistinguishable from a certain energy boundary. This limit is important for experiments, because when the studied reaction threshold is over this limit, the spectral averaged cross sections in PFNS can be derived from the measured reactions in the reactor core. The evaluation of the neutron spectrum measurements in three different thermal-reactor cores shows that this lower limit is around the energy of 5.5 - 6â¯MeV. Above this energy the reactor spectra becomes identical with the 235U PFNS. IAEA CIELO PFNS is within 5% of the measured PFNS from 10 to 14â¯MeV in a LR-0 reactor, while ENDF/B-VII evaluated PFNS underestimated measured neutron spectra.
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A well-defined neutron spectrum is an essential tool for calibration and tests of spectrometry and dosimetry detectors, and evaluation methods for spectra processing. Many of the nowadays used neutron standards are calibrated against a fission spectrum which has a rather smooth energy dependence. In recent time, at the LVR-15 research reactor in Rez, an alternative approach was tested for the needs of fast neutron spectrometry detector calibration. This process comprises detector tests in a neutron beam, filtered by one meter of single-crystalline silicon, which contains several significant peaks in the fast neutron energy range. Tests in such neutron field can possibly reveal specific problems in the deconvolution matrix of the detection system, which may stay hidden in fields with a smooth structure and can provide a tool for a proper energy calibration. Test with several stilbene scintillator crystals in two different beam configurations supplemented by Monte-Carlo transport calculations have been carried out. The results have shown a high level of agreement between the experimental data and simulation, proving thus the accuracy of used deconvolution matrix. The chosen approach can, thus, provide a well-defined neutron reference field with a peaked structure for further tests of spectra evaluation methods and scintillation detector energy calibration.
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A well-defined neutron spectrum is essential for many types of experimental topics and is also important for both calibration and testing of spectrometric and dosimetric detectors. Provided it is well described, such a spectrum can also be employed as a reference neutron field that is suitable for validating selected cross sections. The present paper aims to compare calculations and measurements of such a well-defined spectra in geometrically similar cores of the LR-0 reactor with fuel containing slightly different enrichments (2%, 3.3% and 3.6%). The common feature to all cores is a centrally located dry channel which can be used for the insertion of studied materials. The calculation of neutron and gamma spectra was realized with the MCNP6 code using ENDF/B-VII.0, JEFF-3.1, JENDL-3.3, ROSFOND-2010 and CENDL-3.1 nuclear data libraries. Only minor differences in neutron and gamma spectra were found in the comparison of the presented reactor cores with different fuel enrichments. One exception is the gamma spectrum in the higher energy region (above 8MeV), where more pronounced variations could be observed.
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The MAX IV Laboratory is currently the synchrotron X-ray source with the beam of highest brilliance. Four imaging beamlines are in construction or in the project phase. Their common characteristic will be the high acquisition rates of phase-enhanced images. This high data flow will be managed at the local computing cluster jointly with the Swedish National Computing Infrastructure. A common image reconstruction and analysis platform is being designed to offer reliable quantification of the multidimensional images acquired at all the imaging beamlines at MAX IV.
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Lead(II) acetate [Pb(Ac)2, where Ac = acetate group (CH3-COO(-))2] is a very common salt with many and varied uses throughout history. However, only lead(II) acetate trihydrate [Pb(Ac)2·3H2O] has been characterized to date. In this paper, two enantiotropic polymorphs of the anhydrous salt, a novel hydrate [lead(II) acetate hemihydrate: Pb(Ac)2·(1)/2H2O], and two decomposition products [corresponding to two different basic lead(II) acetates: Pb4O(Ac)6 and Pb2O(Ac)2] are reported, with their structures being solved for the first time. The compounds present a variety of molecular arrangements, being 2D or 1D coordination polymers. A thorough thermal analysis, by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), was also carried out to study the behavior and thermal data of the salt and its decomposition process, in inert and oxygenated atmospheres, identifying the phases and byproducts that appear. The complex thermal behavior of lead(II) acetate is now solved, finding the existence of another hydrate, two anhydrous enantiotropic polymorphs, and some byproducts. Moreover, some of them are phosphorescent at room temperature. The compounds were studied by TGA, DSC, X-ray diffraction, and UV-vis spectroscopy.
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Single and multilayer TiO2 thin films coated on two types of soda-lime glass substrates (microscope slides and cylinders) were prepared by a chelating agent-assisted sol-gel method, using ethyl acetoacetate as a chelating agent, dip-coating and calcination at 500 °C for 2 h in air. Phase composition, microstructural, morphological and optical properties of thin films were comprehensively investigated by using XRF, advanced XRD analysis, Raman and UV-vis spectroscopy and AFM. It was found out that the thickness of thin films increases linearly with increasing number of deposited layers, indicating a good adhesion of the titania solution to a glass substrate as well as to a previously calcined layer. 1 layer film crystallized to anatase-TiO2(B) mixture with minor/negligible amount of nanosized brookite, 2-4 layers films crystallized to anatase-brookite-TiO2(B) mixture. In contrast to other multilayers films, 4 layers film was highly inhomogeneous. The different phase composition of thin films was clarified based on the crystallization via titanate/s and metastable monoclinic TiO2(B) as a consequence of several phenomena; the diffusion of Na⺠ions from a soda-lime glass substrate, acidic conditions and repeated thermal treatment. The multilayer films were in average highly transparent (80-95%) in the visible light region with the sharp absorption edge in the UV light region. Additionally, the photocatalytic properties of selected multilayer films were compared in AO7 photodegradation. Photocatalytic experiments showed that thicker 4 layers film of tricrystalline anatase-brookite-TiO2(B) phase mixture was similarly active as thinner 3 layers film of similar phase composition, which may be a consequence of the inhomogeneity of the thicker film.
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Quelantes/química , Membranas Artificiales , Transición de Fase , Procesos Fotoquímicos , Titanio/química , Espectrofotometría Ultravioleta , Espectrometría RamanRESUMEN
Several new methods for the digital discrimination of neutrons and gamma-rays in a mixed radiation field are presented. The methods introduced discriminate neutrons and gamma rays successfully in the digital domain. They are mathematically simple and exploit samples during the life time of the pulse, hence appropriate for field measurements. All these methods are applied to a set of mixed neutron and photon signals from a stilbene scintillator and their discrimination qualities are compared.
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A common way of speeding up powder diffraction measurements is the use of one- or two-dimensional detectors. This usually goes hand in hand with worse resolution and asymmetric peak profiles. In this work the influence of a straight linear detector on the resolution function in the Bragg-Brentano focusing geometry is discussed. Because of the straight nature of most modern detectors geometrical defocusing occurs, which heavily influences the line shape of diffraction lines at low angles. An easy approach to limit the resolution-degrading effects is presented. The presented algorithm selects an adaptive range of channels of the linear detector at low angles, resulting in increased resolution. At higher angles the whole linear detector is used and the data collection remains fast. Using this algorithm a well behaved resolution function is obtained in the full angular range, whereas using the full linear detector the resolution function varies within one pattern, which hinders line-shape and Rietveld analysis.