Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

Hard alpha-keratin degradation inside a tissue under high flux X-ray synchrotron micro-beam: a multi-scale time-resolved study.

PubMed

Leccia, Emilie; Gourrier, Aurélien; Doucet, Jean; Briki, Fatma

2010-04-01

X-rays interact strongly with biological organisms. Synchrotron radiation sources deliver very intense X-ray photon fluxes within micro- or submicro cross-section beams, resulting in doses larger than the MGy. The relevance of synchrotron radiation analyses of biological materials is therefore questionable since such doses, million times higher than the ones used in radiotherapy, can cause huge damages in tissues, with regard to not only DNA, but also proteic and lipid organizations. Very few data concerning the effect of very high X-ray doses in tissues are available in the literature. We present here an analysis of the structural phenomena which occur when the model tissue of human hair is irradiated by a synchrotron X-ray micro-beam. The choice of hair is supported by its hierarchical and partially ordered keratin structure which can be analysed inside the tissue by X-ray diffraction. To assess the damages caused by hard X-ray micro-beams (1 microm(2) cross-section), short exposure time scattering SAXS/WAXS patterns have been recorded at beamline ID13 (ESRF) after various irradiation times. Various modifications of the scattering patterns are observed, they provide fine insight of the radiation damages at various hierarchical levels and also unexpectedly provide information about the stability of the various hierarchical structural levels. It appears that the molecular level, i.e. the alpha helices which are stabilized by hydrogen bonds and the alpha-helical coiled coils which are stabilized by hydrophobic interactions, is more sensitive to radiation than the supramolecular architecture of the keratin filament and the filament packing within the keratin associated proteins matrix, which is stabilized by disulphide bonds. (c) 2009 Elsevier Inc. All rights reserved.

Observations of the structure and evolution of solar flares with a soft X-ray telescope

NASA Technical Reports Server (NTRS)

Vorpahl, J. A.; Gibson, E. G.; Landecker, P. B.; Mckenzie, D. L.; Underwood, J. M.

1975-01-01

Soft X ray flare events were observed with the S-056 X-ray telescope that was part of the ATM complement of instruments aboard SKYLAB. Analyses of these data are reported. The observations are summarized and a detailed discussion of the X-ray flare structures is presented. The data indicated that soft X-ray emitted by a flare come primarily from an intense well-defined core surrounded by a region of fainter, more diffuse emission. An analysis of flare evolution indicates evidence for preliminary heating and energy release prior to the main phase of the flare. Core features are found to be remarkably stable and retain their shape throughout a flare. Most changes in the overall configuration seem to be result of the appearance, disappearance or change in brightness of individual features, rather than the restructuring or reorientation of these features. Brief comparisons with several theories are presented.

TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka

Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speedmore » higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.« less

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Radiation damage and annealing in plutonium tetrafluoride

NASA Astrophysics Data System (ADS)

McCoy, Kaylyn; Casella, Amanda; Sinkov, Sergey; Sweet, Lucas; McNamara, Bruce; Delegard, Calvin; Jevremovic, Tatjana

2017-12-01

A sample of plutonium tetrafluoride that was separated prior to 1966 at the Hanford Site in Washington State was analyzed at the Pacific Northwest National Laboratory (PNNL) in 2015 and 2016. The plutonium tetrafluoride, as received, was an unusual color and considering the age of the plutonium, there were questions about the condition of the material. These questions had to be answered in order to determine the suitability of the material for future use or long-term storage. Therefore, thermogravimetric/differential thermal analysis and X-ray diffraction evaluations were conducted to determine the plutonium's crystal structure, oxide content, and moisture content; these analyses reported that the plutonium was predominately amorphous and tetrafluoride, with an oxide content near ten percent. Freshly fluorinated plutonium tetrafluoride is known to be monoclinic. During the initial thermogravimetric/differential thermal analyses, it was discovered that an exothermic event occurred within the material near 414 °C. X-ray diffraction analyses were conducted on the annealed tetrafluoride. The X-ray diffraction analyses indicated that some degree of recrystallization occurred in conjunction with the 414 °C event. The following commentary describes the series of thermogravimetric/differential thermal and X-ray diffraction analyses that were conducted as part of this investigation at PNNL.

Overview of nanoscale NEXAFS performed with soft X-ray microscopes.

PubMed

Guttmann, Peter; Bittencourt, Carla

2015-01-01

Today, in material science nanoscale structures are becoming more and more important. Not only for the further miniaturization of semiconductor devices like carbon nanotube based transistors, but also for newly developed efficient energy storage devices, gas sensors or catalytic systems nanoscale and functionalized materials have to be analysed. Therefore, analytical tools like near-edge X-ray absorption fine structure (NEXAFS) spectroscopy has to be applied on single nanostructures. Scanning transmission X-ray microscopes (STXM) as well as full-field transmission X-ray microscopes (TXM) allow the required spatial resolution to study individual nanostructures. In the soft X-ray energy range only STXM was used so far for NEXAFS studies. Due to its unique setup, the TXM operated by the Helmholtz-Zentrum Berlin (HZB) at the electron storage ring BESSY II is the first one in the soft X-ray range which can be used for NEXAFS spectroscopy studies which will be shown in this review. Here we will give an overview of the different microscopes used for NEXAFS studies and describe their advantages and disadvantages for different samples.

Improving small-angle X-ray scattering data for structural analyses of the RNA world

PubMed Central

Rambo, Robert P.; Tainer, John A.

2010-01-01

Defining the shape, conformation, or assembly state of an RNA in solution often requires multiple investigative tools ranging from nucleotide analog interference mapping to X-ray crystallography. A key addition to this toolbox is small-angle X-ray scattering (SAXS). SAXS provides direct structural information regarding the size, shape, and flexibility of the particle in solution and has proven powerful for analyses of RNA structures with minimal requirements for sample concentration and volumes. In principle, SAXS can provide reliable data on small and large RNA molecules. In practice, SAXS investigations of RNA samples can show inconsistencies that suggest limitations in the SAXS experimental analyses or problems with the samples. Here, we show through investigations on the SAM-I riboswitch, the Group I intron P4-P6 domain, 30S ribosomal subunit from Sulfolobus solfataricus (30S), brome mosaic virus tRNA-like structure (BMV TLS), Thermotoga maritima asd lysine riboswitch, the recombinant tRNAval, and yeast tRNAphe that many problems with SAXS experiments on RNA samples derive from heterogeneity of the folded RNA. Furthermore, we propose and test a general approach to reducing these sample limitations for accurate SAXS analyses of RNA. Together our method and results show that SAXS with synchrotron radiation has great potential to provide accurate RNA shapes, conformations, and assembly states in solution that inform RNA biological functions in fundamental ways. PMID:20106957

[X-ray semiotics of the morphological and functional changes in chronic bronchitis].

PubMed

Khomenko, A G; Dmitrieva, L I; Polak, J; Gapon'ko, G A; Starilova, I P

1985-01-01

The authors analysed structural disorders of a pulmonary pattern in patients with non-obstructive, obstructive and purulent bronchitis. Characteristic x-ray symptom-complexes were singled out for each clinical variant of the disease. In addition to roentgenomorphological changes functional disorders showing changes of biomechanics in patients with chronic bronchitis were revealed at roentgenopneumopolygraphy.

Application of a real-space three-dimensional image reconstruction method in the structural analysis of noncrystalline biological macromolecules enveloped by water in coherent x-ray diffraction microscopy.

PubMed

Kodama, Wataru; Nakasako, Masayoshi

2011-08-01

Coherent x-ray diffraction microscopy is a novel technique in the structural analyses of particles that are difficult to crystallize, such as the biological particles composing living cells. As water is indispensable for maintaining particles in functional structures, sufficient hydration of targeted particles is required during sample preparation for diffraction microscopy experiments. However, the water enveloping particles also contributes significantly to the diffraction patterns and reduces the electron-density contrast of the sample particles. In this study, we propose a protocol for the structural analyses of particles in water by applying a three-dimensional reconstruction method in real space for the projection images phase-retrieved from diffraction patterns, together with a developed density modification technique. We examined the feasibility of the protocol through three simulations involving a protein molecule in a vacuum, and enveloped in either a droplet or a cube-shaped water. The simulations were carried out for the diffraction patterns in the reciprocal planes normal to the incident x-ray beam. This assumption and the simulation conditions corresponded to experiments using x-ray wavelengths of shorter than 0.03 Å. The analyses demonstrated that our protocol provided an interpretable electron-density map. Based on the results, we discuss the advantages and limitations of the proposed protocol and its practical application for experimental data. In particular, we examined the influence of Poisson noise in diffraction patterns on the reconstructed three-dimensional electron density in the proposed protocol.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Cobalt Oxide Nanoclusters on Rutile Titania as Bifunctional Units for Water Oxidation Catalysis and Visible Light Absorption: Understanding the Structure-Activity Relationship.

PubMed

Maeda, Kazuhiko; Ishimaki, Koki; Okazaki, Megumi; Kanazawa, Tomoki; Lu, Daling; Nozawa, Shunsuke; Kato, Hideki; Kakihana, Masato

2017-02-22

The structure of cobalt oxide (CoO x ) nanoparticles dispersed on rutile TiO 2 (R-TiO 2 ) was characterized by X-ray diffraction, UV-vis-NIR diffuse reflectance spectroscopy, high-resolution transmission electron microscopy, X-ray absorption fine-structure spectroscopy, and X-ray photoelectron spectroscopy. The CoO x nanoparticles were loaded onto R-TiO 2 by an impregnation method from an aqueous solution containing Co(NO 3 ) 2 ·6H 2 O followed by heating in air. Modification of the R-TiO 2 with 2.0 wt % Co followed by heating at 423 K for 1 h resulted in the highest photocatalytic activity with good reproducibility. Structural analyses revealed that the activity of this photocatalyst depended strongly on the generation of Co 3 O 4 nanoclusters with an optimal distribution. These nanoclusters are thought to interact with the R-TiO 2 surface, resulting in visible light absorption and active sites for water oxidation.

Enhancing catalytic activity by narrowing local energy gaps--X-ray studies of a manganese water oxidation catalyst.

PubMed

Xiao, Jie; Khan, Munirah; Singh, Archana; Suljoti, Edlira; Spiccia, Leone; Aziz, Emad F

2015-03-01

Changes in the local electronic structure of the Mn 3d orbitals of a Mn catalyst derived from a dinuclear Mn(III) complex during the water oxidation cycle were investigated ex situ by X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) analyses. Detailed information about the Mn 3d orbitals, especially the local HOMO-LUMO gap on Mn sites revealed by RIXS analyses, indicated that the enhancement in catalytic activity (water oxidation) originated from the narrowing of the local HOMO-LUMO gap when electrical voltage and visible light illumination were applied simultaneously to the Mn catalytic system. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synchrotron-based XAS on structure investigation of La0.99-xSrx(Na, K, Ba)0.01MnO3 nanoparticles: Evidence of magnetic properties

NASA Astrophysics Data System (ADS)

Daengsakul, Sujittra; Saengplot, Saowalak; Kidkhunthod, Pinit; Pimsawat, Adulphan; Maensiri, Santi

2018-04-01

This work presents the structural study of La0.99-xSrx(Na, K, Ba)0.01MnO3 or LSAM nanoparticles synthesized using thermal-hydro decomposition method where A denotes Na, K, Sr and Ba, respectively. The effect of ionic radii size of A dopants or rA from the substitution of A for La and Sr on the MnO6 octrahedral structure, where the average size of the cations occupying in A-site or 〈rA〉 is fixed at ∼ 1.24 Å, is focused. The LSAM nanoparticles are carefully studied using X-ray diffraction (XRD) including Rietveld refinement and X-ray Absorption Spectroscopy (XAS) including X-ray Absorption Near edge Structure (XANES) and X-ray Absorption Fine Structure (EXAFS). The Rietveld refinement shows all nano-powder samples have rhombohedral structure. By XANES technique we found that the effect of A substitutions at A-site causes a slight change of mean oxidation state of Mn between 3.54 and 3.60. Furthermore, the structural distortion of MnO6 octrahedral in samples is analysed and obtained from EXAFS. The observed trend of ferromagnetism for all LSAM samples can be clearly explained by evidences of A-site doping, structural distortion around Mn atoms and mixing Mn3+/Mn4+ valence states.

Radiation damage and annealing in plutonium tetrafluoride

DOE Office of Scientific and Technical Information (OSTI.GOV)

McCoy, Kaylyn; Casella, Amanda; Sinkov, Sergey

Plutonium tetrafluoride that was separated prior to 1966 at the Hanford Site in Washington State was analyzed at the Pacific Northwest National Laboratory (PNNL) in 2015 and 2016. The plutonium tetrafluoride, as received, was an off-normal color and considering the age of the plutonium, there were questions about the condition of the material. These questions had to be answered in order to determine the suitability of the material for future use or long-term storage. Therefore, Thermogravimetric/Differential Thermal Analysis and X-ray Diffraction evaluations were conducted to determine the plutonium’s crystal structure, oxide content, and moisture content; these analyses reported that themore » plutonium was predominately amorphous and tetrafluoride, with an oxide content near ten percent. Freshly fluorinated plutonium tetrafluoride is known to be monoclinic. During the initial Thermogravimetric/Differential Thermal analyses, it was discovered that an exothermic event occurred within the material near 414°C. X-ray Diffraction analyses were conducted on the annealed tetrafluoride. The X-ray Diffraction analyses indicated that some degree of recrystallization occurred in conjunction with the 414°C event. The following commentary describes the series of Thermogravimetric/Differential Thermal and X-ray Diffraction analyses that were conducted as part of this investigation at PNNL, in collaboration with the University of Utah Nuclear Engineering Program.« less

[Diagnostic possibilities of digital volume tomography].

PubMed

Lemkamp, Michael; Filippi, Andreas; Berndt, Dorothea; Lambrecht, J Thomas

2006-01-01

Cone beam computed tomography allows high quality 3D images of cranio-facial structures. Although detail resolution is increased, x-ray exposition is reduced compared to classic computer tomography. The volume is analysed in three orthogonal plains, which can be rotated independently without quality loss. Cone beam computed tomography seems to be a less expensive and less x-ray exposing alternative to classic computer tomography.

Real-time x-ray scattering study of the initial growth of organic crystals on polymer brushes

DOE Office of Scientific and Technical Information (OSTI.GOV)

An, Sung Yup; Ahn, Kwangseok; Kim, Doris Yangsoo

2014-04-21

We studied the early-stage growth structures of pentacene organic crystals grown on polymer brushes using real-time x-ray scattering techniques. In situ x-ray reflectivity and atomic force microscopy analyses revealed that at temperatures close to the glass transition temperature of polymer brush, the pentacene overlayer on a polymer brush film showed incomplete condensation and 3D island structures from the first monolayer. A growth model based on these observations was used to quantitatively analyze the real-time anti-Bragg x-ray scattering intensities measured during pentacene growth to obtain the time-dependent layer coverage of the individual pentacene monolayers. The extracted total coverage confirmed significant desorptionmore » and incomplete condensation in the pentacene films deposited on the polymer brushes. These effects are ascribed to the change in the surface viscoelasticity of the polymer brushes around the glass transition temperature.« less

Synthesis, Structural and Antioxidant Studies of Some Novel N-Ethyl Phthalimide Esters

PubMed Central

Chandraju, Siddegowda; Win, Yip-Foo; Tan, Weng Kang; Quah, Ching Kheng; Fun, Hoong-Kun

2015-01-01

A series of N-ethyl phthalimide esters 4(a-n) were synthesized and characterized by spectroscopic studies. Further, the molecular structure of majority of compounds were analysed by single crystal X-ray diffraction studies. The X-ray analysis revealed the importance of substituents on the crystal stability and molecular packing. All the synthesized compounds were tested for in vitro antioxidant activity by DPPH radical scavenging, FRAP and CUPRAC methods. Few of them have shown good antioxidant activity. PMID:25742494

Synthesis, structural and antioxidant studies of some novel N-ethyl phthalimide esters.

PubMed

Chidan Kumar, C S; Loh, Wan-Sin; Chandraju, Siddegowda; Win, Yip-Foo; Tan, Weng Kang; Quah, Ching Kheng; Fun, Hoong-Kun

2015-01-01

A series of N-ethyl phthalimide esters 4(a-n) were synthesized and characterized by spectroscopic studies. Further, the molecular structure of majority of compounds were analysed by single crystal X-ray diffraction studies. The X-ray analysis revealed the importance of substituents on the crystal stability and molecular packing. All the synthesized compounds were tested for in vitro antioxidant activity by DPPH radical scavenging, FRAP and CUPRAC methods. Few of them have shown good antioxidant activity.

Coherent X-Ray Diffraction Imaging of Chloroplasts from Cyanidioschyzon merolae by Using X-Ray Free Electron Laser.

PubMed

Takayama, Yuki; Inui, Yayoi; Sekiguchi, Yuki; Kobayashi, Amane; Oroguchi, Tomotaka; Yamamoto, Masaki; Matsunaga, Sachihiro; Nakasako, Masayoshi

2015-07-01

Coherent X-ray diffraction imaging (CXDI) is a lens-less technique for visualizing the structures of non-crystalline particles with the dimensions of submicrometer to micrometer at a resolution of several tens of nanometers. We conducted cryogenic CXDI experiments at 66 K to visualize the internal structures of frozen-hydrated chloroplasts of Cyanidioschyzon merolae using X-ray free electron laser (XFEL) as a coherent X-ray source. Chloroplast dispersed specimen disks at a number density of 7/(10×10 µm(2)) were flash-cooled with liquid ethane without staining, sectioning or chemical labeling. Chloroplasts are destroyed at atomic level immediately after the diffraction by XFEL pulses. Thus, diffraction patterns with a good signal-to-noise ratio from single chloroplasts were selected from many diffraction patterns collected through scanning specimen disks to provide fresh specimens into the irradiation area. The electron density maps of single chloroplasts projected along the direction of the incident X-ray beam were reconstructed by using the iterative phase-retrieval method and multivariate analyses. The electron density map at a resolution of 70 nm appeared as a C-shape. In addition, the fluorescence image of proteins stained with Flamingo™ dye also appeared as a C-shape as did the autofluorescence from Chl. The similar images suggest that the thylakoid membranes with an abundance of proteins distribute along the outer membranes of chloroplasts. To confirm the present results statistically, a number of projection structures must be accumulated through high-throughput data collection in the near future. Based on the results, we discuss the feasibility of XFEL-CXDI experiments in the structural analyses of cellular organelles. © The Author 2015. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

Investigation of La and Al substitution on the spontaneous polarization and lattice dynamics of the Pb(1-x)LaxTi(1-x)AlxO3 ceramics

NASA Astrophysics Data System (ADS)

Yadav, Arun Kumar; Verma, Anita; Kumar, Sunil; Srihari, Velaga; Sinha, A. K.; Reddy, V. Raghavendra; Liu, Shun Wei; Biring, Sajal; Sen, Somaditya

2018-03-01

The phase purity and crystal structure of Pb(1-x)LaxTi(1-x)AlxO3 (0 ≤ x ≤ 0.25) samples (synthesized via the sol-gel process) were confirmed using synchrotron x-ray powder diffraction (XRD) (wavelength, λ = 0.44573 Å). Rietveld analyses of powder x-ray diffraction data confirmed the tetragonal structure for compositions with x ≤ 0.18 and cubic structure for the sample with x = 0.25. Temperature-dependent XRD was performed to investigate the structural change from tetragonal to cubic structure phase transition. Raman spectroscopy at room temperature also confirmed this phase transition with compositions. Field emission scanning electron microscopy (FESEM) provided information about the surface morphology while an energy dispersive x-ray spectrometer attached with FESEM confirmed the chemical compositions of samples. Temperature and frequency dependent dielectric studies showed that the tetragonal to cubic phase transition decreased from 680 K to 175 K with an increase in the x from 0.03 to 0.25, respectively. This is correlated with the structural studies. Electric field dependent spontaneous polarization showed a proper ferroelectric loop for 0.06 ≤ x ≤ 0.18 belonging to a tetragonal phase, while for x ≥ 0.25, the spontaneous polarization vanishes. Bipolar strain versus electric field revealed a butterfly loop for 0.06 ≤ x ≤ 0.18 compositions. Energy storage efficiency initially increases nominally with substitution but beyond x = 0.18 enhances considerably.

Single crystal X-ray structure of the artists' pigment zinc yellow

NASA Astrophysics Data System (ADS)

Simonsen, Kim Pilkjær; Christiansen, Marie Bitsch; Vinum, Morten Gotthold; Sanyova, Jana; Bendix, Jesper

2017-08-01

The artists' pigment zinc yellow is in general described as a complex potassium zinc chromate with the empirical formula 4ZnCrO4·K2O·3H2O. Even though the pigment has been in use since the second half of the 19th century also in large-scale industrial applications, the exact structure had hitherto been unknown. In this work, zinc yellow was synthesised by precipitation from an aqueous solution of zinc nitrate and potassium chromate under both neutral and basic conditions, and the products were compared with the pigment used in industrial paints. Analyses by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), and powder X-ray diffraction (PXRD), showed that the synthesised products and the industrial pigment were identical. Single-crystal X-ray crystallography determined the structure of zinc yellow as KZn2(CrO4)2(H2O)(OH) or as KZn2(CrO4)2(H3O2) emphasizing the μ-H3O2- moiety. Notably, the zinc yellow is isostructural to the recently structurally characterized cadmium analog and both belong to the natrochalcite structure type.

Structural Analyses of Phase Stability in Amorphous and Partially Crystallized Ge-Rich GeTe Films Prepared by Atomic Layer Deposition.

PubMed

Gwon, Taehong; Mohamed, Ahmed Yousef; Yoo, Chanyoung; Park, Eui-Sang; Kim, Sanggyun; Yoo, Sijung; Lee, Han-Koo; Cho, Deok-Yong; Hwang, Cheol Seong

2017-11-29

The local bonding structures of Ge x Te 1-x (x = 0.5, 0.6, and 0.7) films prepared through atomic layer deposition (ALD) with Ge(N(Si(CH 3 ) 3 ) 2 ) 2 and ((CH 3 ) 3 Si) 2 Te precursors were investigated using Ge K-edge X-ray absorption spectroscopy (XAS). The results of the X-ray absorption fine structure analyses show that for all of the compositions, the as-grown films were amorphous with a tetrahedral Ge coordination of a mixture of Ge-Te and Ge-Ge bonds but without any signature of Ge-GeTe decomposition. The compositional evolution in the valence band electronic structures probed through X-ray photoelectron spectroscopy suggests a substantial chemical influence of additional Ge on the nonstoichiometric GeTe. This implies that the ALD process can stabilize Ge-abundant bonding networks like -Te-Ge-Ge-Te- in amorphous GeTe. Meanwhile, the XAS results on the Ge-rich films that had undergone post-deposition annealing at 350 °C show that the parts of the crystalline Ge-rich GeTe became separated into Ge crystallites and rhombohedral GeTe in accordance with the bulk phase diagram, whereas the disordered GeTe domains still remained, consistent with the observations of transmission electron microscopy and Raman spectroscopy. Therefore, amorphousness in GeTe may be essential for the nonsegregated Ge-rich phases and the low growth temperature of the ALD enables the achievement of the structurally metastable phases.

Radiation damage and annealing in plutonium tetrafluoride

DOE PAGES

McCoy, Kaylyn; Casella, Amanda; Sinkov, Sergey; ...

2017-08-03

A sample of plutonium tetrafluoride that was separated prior to 1966 at the Hanford Site in Washington State was analyzed at the Pacific Northwest National Laboratory (PNNL) in 2015 and 2016. The plutonium tetrafluoride, as received, was an unusual color and considering the age of the plutonium, there were questions about the condition of the material. These questions had to be answered in order to determine the suitability of the material for future use or long-term storage. Therefore, thermogravimetric/differential thermal analysis and X-ray diffraction evaluations were conducted to determine the plutonium's crystal structure, oxide content, and moisture content; these analysesmore » reported that the plutonium was predominately amorphous and tetrafluoride, with an oxide content near ten percent. Freshly fluorinated plutonium tetrafluoride is known to be monoclinic. And during the initial thermogravimetric/differential thermal analyses, it was discovered that an exothermic event occurred within the material near 414 °C. X-ray diffraction analyses were conducted on the annealed tetrafluoride. The X-ray diffraction analyses indicated that some degree of recrystallization occurred in conjunction with the 414 °C event. This commentary describes the series of thermogravimetric/differential thermal and X-ray diffraction analyses that were conducted as part of this investigation at PNNL.« less

Monte Carlo Simulation to Determine Geometry Effects on Quantitative X-ray Microanalysis in Plant Cell Walls Using Gelatin Standards

NASA Astrophysics Data System (ADS)

Tylko, Grzegorz; Dubchak, Sergyi; Banach, Zuzanna; Turnau, Katarzyna

2010-04-01

Monte Carlo simulations of gelatin matrices with known elemental concentrations confirmed the suitability of protein standards to quantify elements of cellulose material in x-ray microanalysis. However, gelatin standards and cellulose plant cell walls differ in structure, what influences x-ray generation and emission in both specimens. The goal of the project was to establish the influence of gelatin structure on x-ray generation and its usefulness to calculate elemental concentrations in plant cell walls of different width. Roots of Medicago truncatula as well as gelatin standards with known elemental composition were prepared according to freeze-drying protocols. The thermanox polymer was chosen to establish background formation for flat and compact organic materials. All analyses were performed with the scanning electron microscope operated at 10 keV and probe current of 350 pA. The Monte Carlo code Casino was applied to calculate the intensities of the generated and the emitted x-rays from biological matrix of different width. No topography effects of gelatin structure were visible when the raster mode of electron impact was applied to the specimen. Monte Carlo simulations of gelatin of different width revealed that a significant decrease of the generated x-ray intensity appears at the width of the specimen around 3.5 μm. However, an increase of emission of low energy x-ray intensities (Na, Mg) was noted at 3.5 μm size with constant emission of higher energy x-rays (Cl, K) down to 2.5 μm width. It determines the minimal size of plant specimen useful for comparison to bulk gelatin standard when quantitative analysis is performed for biologically important elements.

Fine structure of the K X-ray absorption spectra of titanium in some hydrides, borides, and silicides (in Russian)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vainshtein, �. E.; Zhurakovskii, E. A.

1959-08-01

X-ray spectral analyses confirmed the hypothesis on the metal-like state of hydrogen in tithnium hydrides. Experiments with titunium borides and silicides indicate the special character and degree of the 3d--level participation in the metallic'' bond between the atoms of various complexes. The structure of metalloid elements becomes more complicated with an increase in the specific number of boron and silicon atoms and the bond between the atoms tends to become covalent. (R.V.J.)

Determination of Arsenic Poisoning and Metabolism in Hair by Synchrotron Radiation: The Case of Phar Lap

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kempson, Ivan M.; Henry, Dermot A.; U. South Australia)

2010-08-26

Fresh physical evidence about the demise of the racehorse Phar Lap (see photograph) has been gathered from the study of mane hair samples by synchrotron radiation analysis with high resolution X-ray fluorescence (XRF) and X-ray absorption near edge structure (XANES) analyses. The results are indicative of arsenic ingestion and metabolism, and show that the racing champion died from arsenic poisoning.

Structure of the Full-length VEGFR-1 Extracellular Domain in Complex with VEGF-A.

PubMed

Markovic-Mueller, Sandra; Stuttfeld, Edward; Asthana, Mayanka; Weinert, Tobias; Bliven, Spencer; Goldie, Kenneth N; Kisko, Kaisa; Capitani, Guido; Ballmer-Hofer, Kurt

2017-02-07

Vascular endothelial growth factors (VEGFs) regulate blood and lymph vessel development upon activation of three receptor tyrosine kinases: VEGFR-1, -2, and -3. Partial structures of VEGFR/VEGF complexes based on single-particle electron microscopy, small-angle X-ray scattering, and X-ray crystallography revealed the location of VEGF binding and domain arrangement of individual receptor subdomains. Here, we describe the structure of the full-length VEGFR-1 extracellular domain in complex with VEGF-A at 4 Å resolution. We combined X-ray crystallography, single-particle electron microscopy, and molecular modeling for structure determination and validation. The structure reveals the molecular details of ligand-induced receptor dimerization, in particular of homotypic receptor interactions in immunoglobulin homology domains 4, 5, and 7. Functional analyses of ligand binding and receptor activation confirm the relevance of these homotypic contacts and identify them as potential therapeutic sites to allosterically inhibit VEGFR-1 activity. Copyright © 2017 Elsevier Ltd. All rights reserved.

Plutonium-uranium mixed oxide characterization by coupling micro-X-ray diffraction and absorption investigations

NASA Astrophysics Data System (ADS)

Degueldre, C.; Martin, M.; Kuri, G.; Grolimund, D.; Borca, C.

2011-09-01

Plutonium-uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The potential differences of metal redox state and microstructural developments of the matrix before and after irradiation are commonly analysed by electron probe microanalysis. In this work the structure and next-neighbor atomic environments of Pu and U oxide features within unirradiated homogeneous MOX and irradiated (60 MW d kg -1) MOX samples was analysed by micro-X-ray fluorescence (μ-XRF), micro-X-ray diffraction (μ-XRD) and micro-X-ray absorption fine structure (μ-XAFS) spectroscopy. The grain properties, chemical bonding, valences and stoichiometry of Pu and U are determined from the experimental data gained for the unirradiated as well as for irradiated fuel material examined in the center of the fuel as well as in its peripheral zone (rim). The formation of sub-grains is observed as well as their development from the center to the rim (polygonization). In the irradiated sample Pu remains tetravalent (>95%) and no (<5%) Pu(V) or Pu(VI) can be detected while the fuel could undergo slight oxidation in the rim zone. Any slight potential plutonium oxidation is buffered by the uranium dioxide matrix while locally fuel cladding interaction could also affect the redox of the fuel.

Crystal Structure of Two V-shaped Ligands with N-Heterocycles

NASA Astrophysics Data System (ADS)

Wang, Gao-Feng; Sun, Shu-Wen; Zhang, Xiao; Sun, Shu-Gang

2017-12-01

Two V-shaped ligands with N-heterocycles, bis(4-(1 H-imidazol-1-yl) phenyl)methanone ( 1), and bis(4-(1 H-benzo[d]imidazol-1-yl)phenyl)methanone ( 2) have been synthesized and characterized by elemental analyses, IR and 1 H NMR spectroscopy. Crystal structures of 1 and 2 have been determined by X-ray diffraction. The crystal of 1 is monoclinic, sp. gr. P21/ c, Z = 4. The crystal of 2 is orthorhombic, sp. gr. Fdd2, Z = 8. X-ray diffraction analyses show that the V-shaped angles of 1 and 2 are 122.72(15)° and 120.7(4)°, respectively. Intermolecular C-H···O, C-H···N, C-H···π, and π···π interactions link the components into three-dimensional networks in the crystal structures.

Production, Purification and Preliminary X-ray Crystallographic Studies of Adeno-Associated Virus Serotype 9

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mitchell, M.; Nam, H; Carter, A

2009-01-01

Adeno-associated virus (AAV) serotype 9, which is under development for gene-delivery applications, shows significantly enhanced capsid-associated transduction efficiency in muscle compared with other AAV serotypes. With the aim of characterizing the structural determinants of this property, the purification, crystallization and preliminary X-ray crystallographic analyses of the AAV9 viral capsid are reported. The crystals diffracted X-rays to 2.8 A resolution using synchrotron radiation and belonged to the trigonal space group P32, with unit-cell parameters a = b = 251.0, c = 640.0 A. There are three complete viral capsids in the crystal unit cell. The orientation and position of the asymmetricmore » unit capsid have been determined by molecular-replacement methods and structure determination is in progress.« less

X-ray absorption spectroscopic studies of mononuclear non-heme iron enzymes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Westre, Tami E.

Fe-K-edge X-ray absorption spectroscopy (XAS) has been used to investigate the electronic and geometric structure of the iron active site in non-heme iron enzymes. A new theoretical extended X-ray absorption fine structure (EXAFS) analysis approach, called GNXAS, has been tested on data for iron model complexes to evaluate the utility and reliability of this new technique, especially with respect to the effects of multiple-scattering. In addition, a detailed analysis of the 1s→3d pre-edge feature has been developed as a tool for investigating the oxidation state, spin state, and geometry of iron sites. Edge and EXAFS analyses have then been appliedmore » to the study of non-heme iron enzyme active sites.« less

Solution XAS Analysis for Exploring the Active Species in Homogeneous Vanadium Complex Catalysis

NASA Astrophysics Data System (ADS)

Nomura, Kotohiro; Mitsudome, Takato; Tsutsumi, Ken; Yamazoe, Seiji

2018-06-01

Selected examples in V K-edge X-ray Absorption Near Edge Structure (XANES) analysis of a series of vanadium complexes containing imido ligands (possessing metal-nitrogen double bond) in toluene solution have been introduced, and their pre-edge and the edge were affected by their structures and nature of ligands. Selected results in exploring the oxidation states of the active species in ethylene dimerization/polymerization using homogeneous vanadium catalysts [consisting of (imido)vanadium(V) complexes and Al cocatalysts] by X-ray absorption spectroscopy (XAS) analyses have been introduced. It has been demonstrated that the method should provide more clear information concerning the active species in situ, especially by combination with the other methods (NMR and ESR spectra, X-ray crystallographic analysis, and reaction chemistry), and should be powerful tool for study of catalysis mechanism as well as for the structural analysis in solution.

On the consistency of QCBED structure factor measurements for TiO 2 (Rutile)

DOE PAGES

Jiang, Bin; Zuo, Jian -Min; Friis, Jesper; ...

2003-09-16

The same Bragg reflection in TiO 2 from twelve different CBED patterns (from different crystals, orientations and thicknesses) are analysed quantitatively in order to evaluate the consistency of the QCBED method for bond-charge mapping. The standard deviation in the resulting distribution of derived X-ray structure factors is found to be an order of magnitude smaller than that in conventional X-ray work, and the standard error (0.026% for F X(110)) is slightly better than obtained by the X-ray Pendellosung method applied to silicon. This is sufficiently accuracy to distinguish between atomic, covalent and ionic models of bonding. We describe the importancemore » of extracting experimental parameters from CCD camera characterization, and of surface oxidation and crystal shape. Thus, the current experiments show that the QCBED method is now a robust and powerful tool for low order structure factor measurement, which does not suffer from the large extinction (multiple scattering) errors which occur in inorganic X-ray crystallography, and may be applied to nanocrystals. Our results will be used to understand the role of d electrons in the chemical bonding of TiO 2.« less

Dissecting Diffuse X-ray Emission in 30 Doradus with T-ReX

NASA Astrophysics Data System (ADS)

Townsley, Leisa K.; Broos, Patrick

2017-08-01

30 Doradus (the Tarantula Nebula) offers us a microscope on starburst astrophysics, having endured 25 Myrs of the birth and death of the most massive stars known. Across 30 Dor's 250-pc extent, stellar winds and supernovae have carved its ISM into an amazing display of arcs, pillars, and bubbles. For over 40 years, we have also known that 30 Dor is a bright X-ray emitter, so its familiar stars and cold ISM structures suffer irradiation by multi-million-degree plasmas. The 2-Ms Chandra X-ray Visionary Project ``The Tarantula -- Revealed by X-rays'' (T-ReX) exploits Chandra's fine spatial resolution and the ACIS-I field of view to study ISM interfaces on 1--10 pc scales across the entire 30 Dor complex. Here we give preliminary results from ongoing analyses of these data, focusing on the diffuse X-ray emission. Massive star winds and cavity supernovae over the millenia have contributed to a broad mix of X-ray-emitting plasmas and absorbing columns, showing that 30 Dor's hot ISM is just as complex and confusing as that seen at colder temperatures.

Effect of chromium underlayer on the properties of nano-crystalline diamond films

NASA Astrophysics Data System (ADS)

Garratt, E.; AlFaify, S.; Yoshitake, T.; Katamune, Y.; Bowden, M.; Nandasiri, M.; Ghantasala, M.; Mancini, D. C.; Thevuthasan, S.; Kayani, A.

2013-01-01

This paper investigated the effect of chromium underlayer on the structure, microstructure, and composition of the nano-crystalline diamond films. Nano-crystalline diamond thin films were deposited at high temperature in microwave-induced plasma diluted with nitrogen, on single crystal silicon substrate with a thin film of chromium as an underlayer. Characterization of the film was implemented using non-Rutherford backscattering spectrometry, Raman spectroscopy, near-edge x-ray absorption fine structure, x-ray diffraction, and atomic force microscopy. Nanoindentation studies showed that the films deposited on chromium underlayer have higher hardness values compared to those deposited on silicon without an underlayer. Diamond and graphitic phases of the films evaluated by x-ray and optical spectroscopic analyses determined consistency between the sp2 and sp3 phases of carbon in chromium sample to that of diamond grown on silicon. Diffusion of chromium was observed using ion beam analysis which was correlated with the formation of chromium complexes by x-ray diffraction.

X-ray crystallography and its impact on understanding bacterial cell wall remodeling processes.

PubMed

Büttner, Felix Michael; Renner-Schneck, Michaela; Stehle, Thilo

2015-02-01

The molecular structure of matter defines its properties and function. This is especially true for biological macromolecules such as proteins, which participate in virtually all biochemical processes. A three dimensional structural model of a protein is thus essential for the detailed understanding of its physiological function and the characterization of essential properties such as ligand binding and reaction mechanism. X-ray crystallography is a well-established technique that has been used for many years, but it is still by far the most widely used method for structure determination. A particular strength of this technique is the elucidation of atomic details of molecular interactions, thus providing an invaluable tool for a multitude of scientific projects ranging from the structural classification of macromolecules over the validation of enzymatic mechanisms or the understanding of host-pathogen interactions to structure-guided drug design. In the first part of this review, we describe essential methodological and practical aspects of X-ray crystallography. We provide some pointers that should allow researchers without a background in structural biology to assess the overall quality and reliability of a crystal structure. To highlight its potential, we then survey the impact X-ray crystallography has had on advancing an understanding of a class of enzymes that modify the bacterial cell wall. A substantial number of different bacterial amidase structures have been solved, mostly by X-ray crystallography. Comparison of these structures highlights conserved as well as divergent features. In combination with functional analyses, structural information on these enzymes has therefore proven to be a valuable template not only for understanding their mechanism of catalysis, but also for targeted interference with substrate binding. Copyright © 2015 Elsevier GmbH. All rights reserved.

Near-edge X-ray absorption spectra for metallic Cu and Mn

NASA Astrophysics Data System (ADS)

Greaves, G. N.; Durham, P. J.; Diakun, G.; Quinn, P.

1981-11-01

The measurement of X-ray absorption fine structure of metals- both in the extended region (EXAFS) as well as in the near edge region (XANES)-has been widely discussed (see refs 1-6 for Cu and refs 7-9 for Mn). The recent availability of intense X-ray fluxes from storage rings has usually been exploited for EXAFS leaving the XANES often with poorer resolution than earlier work performed on conventional sources (for example, compare the near edge structure for copper in ref. 1 with refs 3 or 6). In addition, whilst the theory and analysis of EXAFS is relatively well-established2,10, a theory for the strong scattering regime near to the absorption edge has only recently been developed11. We report here the first high resolution XANES spectra for Cu and Mn which were performed at the SRS storage ring at Daresbury. Although both metals have close-packed structures consisting of atoms of similar size their local atomic structure is different in detail. Significant differences are found in their respective XANES reflecting the senstivity of this region of the X-ray absorption fine structure to the local atomic structure. Spectra for the two metals have been analysed using the new multiple scattering formalism. This is a real space calculation and unlike a conventional band structure approach it does not require structural periodicity but works from the local arrangement of atoms.

Structural, vibrational and luminescence properties of the (1−x)CaWO{sub 4}−xCdWO{sub 4} system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; CEA/DEN, Département d’Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache, 13108, Saint-Paul-lez-Durance

2014-11-15

In the present work, we investigate the structural, microstructural, vibrational and luminescence properties of the system (1−x)CaWO{sub 4}−xCdWO{sub 4} with x ranging between 0 and 1. Polycrystalline samples were elaborated using a coprecipitation technique followed by thermal treatment at 1000 °C. The samples were then characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy and luminescence analyses. X-ray diffraction profile analyses using Rietveld method showed that two kinds of solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4} having scheelite and wolframite structures, with respectively tetragonal and monoclinic crystal cells, were observed, with a biphasic system for compositions x=0.6 and 0.7. The scanningmore » electron microscopy experiments showed a complex evolution of morphologies and crystallite sizes as x increased. The vibration modes of Raman spectra were characteristic of composition-dependent disordered solid solutions with decreasing wavenumbers as x increased. Luminescence experiments were performed under UV-laser light irradiation. The energies of emission bands increased linearly with cadmium composition x. The integrated intensity of luminescence reached a maximum value for the substituted wolframite phase with composition x=0.8. - Graphical abstract: Luminescence on UV excitation (364.5 nm) of (1−x)CaWO{sub 4−x}CdWO{sub 4} system, elaborated from coprecipitation technique at 1000 °C, with 0« less

Synthesis, X-ray crystal structures and thermal analyses of some new antimicrobial zinc complexes: New configurations and nano-size structures.

PubMed

Masoudiasl, A; Montazerozohori, M; Naghiha, R; Assoud, A; McArdle, P; Safi Shalamzari, M

2016-04-01

Some new five coordinated ZnLX2 complexes, where L is N3-Schiff base ligand obtained by condensation reaction between diethylenetriamine and (E)-3-(2-nitrophenyl)acrylaldehyde and X (Cl(-), Br(-), I(-), N3(-) and NCS(-)), were synthesized and characterized by FT-IR, (1)H and (13)CNMR, UV-visible, ESI-mass spectra and molar conductivity measurements. The structures of zinc iodide and thiocyanate complexes were determined by X-ray crystallographic analysis. The X-ray results showed that the Zn (II) center in these complexes is five-coordinated in a distorted trigonal-bipyramidal configuration. Zinc iodide and thiocyanate complexes crystallize in the monoclinic and triclinic systems with space groups of C2/c and P1- with eight and two molecules per unit cell respectively. The crystal packing of the complexes consists of intermolecular interactions such as C-H(…)O and C-H(…)I, C-H(···)S, N(…)O, together with π-π stacking and some other unexpected interactions. The mentioned interactions cause three-dimensional supramolecular structure in the solid state. Zinc complexes were also prepared in nano-structure by sonochemical method confirmed by XRD, SEM and TEM analyses. Moreover, ZnO nanoparticles were synthesized by direct thermolysis of zinc iodide complex. Furthermore, antimicrobial and thermal properties of the compounds were completely investigated. Copyright © 2016 Elsevier B.V. All rights reserved.

Spectroscopic evidence for uranium bearing precipitates in vadose zone sediments at the Hanford 300-area site

USGS Publications Warehouse

Arai, Y.; Marcus, M.A.; Tamura, N.; Davis, J.A.; Zachara, J.M.

2007-01-01

Uranium (U) solid-state speciation in vadose zone sediments collected beneath the former North Process Pond (NPP) in the 300 Area of the Hanford site (Washington) was investigated using multi-scale techniques. In 30 day batch experiments, only a small fraction of total U (???7.4%) was released to artificial groundwater solutions equilibrated with 1% pCO2. Synchrotron-based micro-X-ray fluorescence spectroscopy analyses showed that U was distributed among at least two types of species: (i) U discrete grains associated with Cu and (ii) areas with intermediate U concentrations on grains and grain coatings. Metatorbernite (Cu[UO2]2[PO 4]2??8H2O) and uranophane (Ca[UO 2]2[SiO3(OH)]2?? 5H 2O) at some U discrete grains, and muscovite at U intermediate concentration areas, were identified in synchrotron-based micro-X-ray diffraction. Scanning electron microscopy/energy dispersive X-ray analyses revealed 8-10 ??m size metatorbernite particles that were embedded in C-, Al-, and Si-rich coatings on quartz and albite grains. In ??- and bulk-X-ray absorption structure (??-XAS and XAS) spectroscopy analyses, the structure of metatorbernite with additional U-C and U-U coordination environments was consistently observed at U discrete grains with high U concentrations. The consistency of the ??- and bulk-XAS analyses suggests that metatorbernite may comprise a significant fraction of the total U in the sample. The entrapped, micrometer-sized metatorbernite particles in C-, Al-, and Si-rich coatings, along with the more soluble precipitated uranyl carbonates and uranophane, likely control the long-term release of U to water associated with the vadose zone sediments. ?? 2007 American Chemical Society.

Robust, high-throughput solution structural analyses by small angle X-ray scattering (SAXS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hura, Greg L.; Menon, Angeli L.; Hammel, Michal

2009-07-20

We present an efficient pipeline enabling high-throughput analysis of protein structure in solution with small angle X-ray scattering (SAXS). Our SAXS pipeline combines automated sample handling of microliter volumes, temperature and anaerobic control, rapid data collection and data analysis, and couples structural analysis with automated archiving. We subjected 50 representative proteins, mostly from Pyrococcus furiosus, to this pipeline and found that 30 were multimeric structures in solution. SAXS analysis allowed us to distinguish aggregated and unfolded proteins, define global structural parameters and oligomeric states for most samples, identify shapes and similar structures for 25 unknown structures, and determine envelopes formore » 41 proteins. We believe that high-throughput SAXS is an enabling technology that may change the way that structural genomics research is done.« less

Interaction Analysis of FABP4 Inhibitors by X-ray Crystallography and Fragment Molecular Orbital Analysis.

PubMed

Tagami, Uno; Takahashi, Kazutoshi; Igarashi, Shunsuke; Ejima, Chieko; Yoshida, Tomomi; Takeshita, Sen; Miyanaga, Wataru; Sugiki, Masayuki; Tokumasu, Munetaka; Hatanaka, Toshihiro; Kashiwagi, Tatsuki; Ishikawa, Kohki; Miyano, Hiroshi; Mizukoshi, Toshimi

2016-04-14

X-ray crystal structural determination of FABP4 in complex with four inhibitors revealed the complex binding modes, and the resulting observations led to improvement of the inhibitory potency of FABP4 inhibitors. However, the detailed structure-activity relationship (SAR) could not be explained from these structural observations. For a more detailed understanding of the interactions between FABP4 and inhibitors, fragment molecular orbital analyses were performed. These analyses revealed that the total interfragment interaction energies of FABP4 and each inhibitor correlated with the ranking of the K i value for the four inhibitors. Furthermore, interactions between each inhibitor and amino acid residues in FABP4 were identified. The oxygen atom of Lys58 in FABP4 was found to be very important for strong interactions with FABP4. These results might provide useful information for the development of novel potent FABP4 inhibitors.

Order-disorder phase transitions and their influence on the structure and vibrational properties of new hybrid material: 2-Amino-4-methyl-3-nitropyridinium trifluoroacetate

NASA Astrophysics Data System (ADS)

Lorenc, J.; Bryndal, I.; Syska, W.; Wandas, M.; Marchewka, M.; Pietraszko, A.; Lis, T.; Mączka, M.; Hermanowicz, K.; Hanuza, J.

2010-08-01

New organic-organic salt, 2-amino-4-methyl-3-nitropyridinium trifluoroacetate, has been synthesised and characterised by FT-IR, FT-Raman, DSC and single crystal X-ray crystallography. The 2-amino-4-methyl-3-nitropyridinium trifluoroacetate undergoes a reversible phase transition at ˜162 K. The X-ray structures, vibrational spectra and quantum chemical DFT calculations (B3LYP/6-31G(d,p) approach) have been analysed for high-temperature and low-temperature modifications of the compound, which both crystallize in orthorhombic space group Pbca with two non-equivalent cations and two anions in the asymmetric unit. Their crystal and molecular structures have been compared and the role of the intermolecular interactions in these crystals has been analysed. The mechanisms of the phase transition have been proposed.

Robust X-ray angular correlations for the study of meso-structures

DOE PAGES

Lhermitte, Julien R.; Tian, Cheng; Stein, Aaron; ...

2017-05-08

As self-assembling nanomaterials become more sophisticated, it is becoming increasingly important to measure the structural order of finite-sized assemblies of nano-objects. These mesoscale clusters represent an acute challenge to conventional structural probes, owing to the range of implicated size scales (10 nm to several micrometres), the weak scattering signal and the dynamic nature of meso-clusters in native solution environments. The high X-ray flux and coherence of modern synchrotrons present an opportunity to extract structural information from these challenging systems, but conventional ensemble X-ray scattering averages out crucial information about local particle configurations. Conversely, a single meso-cluster scatters too weakly tomore » recover the full diffraction pattern. Using X-ray angular cross-correlation analysis, it is possible to combine multiple noisy measurements to obtain robust structural information. This paper explores the key theoretical limits and experimental challenges that constrain the application of these methods to probing structural order in real nanomaterials. A metric is presented to quantify the signal-to-noise ratio of angular correlations, and it is used to identify several experimental artifacts that arise. In particular, it is found that background scattering, data masking and inter-cluster interference profoundly affect the quality of correlation analyses. A robust workflow is demonstrated for mitigating these effects and extracting reliable angular correlations from realistic experimental data.« less

Photosynthetic microorganism-mediated synthesis of akaganeite (beta-FeOOH) nanorods.

PubMed

Brayner, Roberta; Yéprémian, Claude; Djediat, Chakib; Coradin, Thibaud; Herbst, Fréderic; Livage, Jacques; Fiévet, Fernand; Couté, Alain

2009-09-01

Common Anabaena and Calothrix cyanobacteria and Klebsormidium green algae are shown to form intracellularly akaganeite beta-FeOOH nanorods of well-controlled size and unusual morphology at room temperature. X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy X-ray energy dispersive spectrometry (SEM-EDS) analyses are used to investigate particle structure, size, and morphology. A mechanism involving iron-siderophore complex formation is proposed and compared with iron biomineralization in magnetotactic bacteria.

A detailed X-ray investigation of ζ Puppis. IV. Further characterization of the variability

NASA Astrophysics Data System (ADS)

Nazé, Yaël; Ramiaramanantsoa, Tahina; Stevens, Ian R.; Howarth, Ian D.; Moffat, Anthony F. J.

2018-01-01

Context. One of the optically brightest and closest massive stars, ζ Pup, is also a bright X-ray source. Previously, its X-ray emission was found to be variable with light curves harbouring "trends" with a typical timescale longer than the exposure length, i.e. >1 d. The origin of these changes was proposed to be linked to large-scale structures in the wind of ζ Pup, but further characterization of the variability at high energies was needed to investigate this scenario. Aims: Since the previous papers of this series, a number of new X-ray observations have become available. Furthermore, a cyclic behaviour with a 1.78 d period was identified in long optical photometric runs, which is thought to be associated with the launching mechanism of large-scale wind structures. Methods: We analysed these new X-ray data, revisited the old data, and compared the X-ray light curves with the optical data, notably those taken simultaneously. Results: The behaviour of ζ Pup in X-rays cannot be explained in terms of a perfect clock because the amplitude and shape of its variations change with time. For example, ζ Pup was much more strongly variable between 2007 and 2011 than before and after this interval. Comparing the X-ray spectra of the star at maximum and minimum brightness yields no compelling difference beyond the overall flux change: the temperatures, absorptions, and line shapes seem to remain constant, well within errors. The only common feature between X-ray datasets is that the variation amplitudes appear maximum in the medium (0.6-1.2 keV) energy band. Finally, no clear and coherent correlation can be found between simultaneous X-ray and optical data. Only a subgroup of observations may be combined coherently with the optical period of 1.78 d, although the simultaneous optical behaviour is unknown. Conclusions: The currently available data do not reveal any obvious, permanent, and direct correlation between X-ray and optical variations. The origin of the X-ray variability therefore still needs to be ascertained, highlighting the need for long-term monitoring in multiwavelengths, i.e. X-ray, UV, and optical.

Quick-scanning x-ray absorption spectroscopy system with a servo-motor-driven channel-cut monochromator with a temporal resolution of 10 ms.

PubMed

Nonaka, T; Dohmae, K; Araki, T; Hayashi, Y; Hirose, Y; Uruga, T; Yamazaki, H; Mochizuki, T; Tanida, H; Goto, S

2012-08-01

We have developed a quick-scanning x-ray absorption fine structure (QXAFS) system and installed it at the recently constructed synchrotron radiation beamline BL33XU at the SPring-8. Rapid acquisition of high-quality QXAFS data was realized by combining a servo-motor-driven Si channel-cut monochromator with a tapered undulator. Two tandemly aligned monochromators with channel-cut Si(111) and Si(220) crystals covered energy ranges of 4.0-28.2 keV and 6.6-46.0 keV, respectively. The system allows the users to adjust instantly the energy ranges of scans, the starting angles of oscillations, and the frequencies. The channel-cut crystals are cooled with liquid nitrogen to enable them to withstand the high heat load from the undulator radiation. Deformation of the reflecting planes is reduced by clamping each crystal with two cooling blocks. Performance tests at the Cu K-edge demonstrated sufficiently high data quality for x-ray absorption near-edge structure and extended x-ray absorption fine-structure analyses with temporal resolutions of up to 10 and 25 ms, respectively.

Effect of iron oxide reductive dissolution on the transformation and immobilization of arsenic in soils: New insights from X-ray photoelectron and X-ray absorption spectroscopy.

PubMed

Fan, Jian-Xin; Wang, Yu-Jun; Liu, Cun; Wang, Li-Hua; Yang, Ke; Zhou, Dong-Mei; Li, Wei; Sparks, Donald L

2014-08-30

The geochemical behavior and speciation of arsenic (As) in paddy soils is strongly controlled by soil redox conditions and the sequestration by soil iron oxyhydroxides. Hence, the effects of iron oxide reductive dissolution on the adsorption, transformation and precipitation of As(III) and As(V) in soils were investigated using batch experiments and synchrotron based techniques to gain a deeper understanding at both macroscopic and microscopic scales. The results of batch sorption experiments revealed that the sorption capacity of As(V) on anoxic soil was much higher than that on control soil. Synchrotron based X-ray fluorescence (μ-XRF) mapping studies indicated that As was heterogeneously distributed and was mainly associated with iron in the soil. X-ray absorption near edge structure (XANES), micro-X-ray absorption near edge structure (μ-XANES) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the primary speciation of As in the soil is As(V). These results further suggested that, when As(V) was introduced into the anoxic soil, the rapid coprecipitation of As(V) with ferric/ferrous ion prevented its reduction to As(III), and was the main mechanism controlling the immobilization of As. This research could improve the current understanding of soil As chemistry in paddy and wetland soils. Copyright © 2014 Elsevier B.V. All rights reserved.

Online in situ x-ray diffraction setup for structural modification studies during swift heavy ion irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grygiel, C.; Lebius, H.; Bouffard, S.

2012-01-15

The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present an x-ray diffractometer called ALIX (''Analyse en Ligne sur IRRSUD par diffraction de rayons X''), which has been set up at the low-energy beamline (IRRadiation SUD - IRRSUD) of the Grand Accelerateur National d'Ions Lourds facility, to allow the study of structural modification kinetics as a function of the ion fluence. The x-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to x-ray pattern recording. We present the capability of ALIXmore » to perform simultaneous irradiation-diffraction by using energy discrimination between x-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation-diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO{sub 3}. We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO{sub 3}, which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO{sub 3}, defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.« less

Structural characterization and aging of glassy pharmaceuticals made using acoustic levitation.

PubMed

Benmore, Chris J; Weber, J K R; Tailor, Amit N; Cherry, Brian R; Yarger, Jeffery L; Mou, Qiushi; Weber, Warner; Neuefeind, Joerg; Byrn, Stephen R

2013-04-01

Here, we report the structural characterization of several amorphous drugs made using the method of quenching molten droplets suspended in an acoustic levitator. (13) C NMR, X-ray, and neutron diffraction results are discussed for glassy cinnarizine, carbamazepine, miconazole nitrate, probucol, and clotrimazole. The (13) C NMR results did not find any change in chemical bonding induced by the amorphization process. High-energy X-ray diffraction results were used to characterize the ratio of crystalline to amorphous material present in the glasses over a period of 8 months. All the glasses were stable for at least 6 months except carbamazepine, which has a strong tendency to crystallize within a few months. Neutron and X-ray pair distribution function analyses were applied to the glassy materials, and the results were compared with their crystalline counterparts. The two diffraction techniques yielded similar results in most cases and identified distinct intramolecular and intermolecular correlations. The intramolecular scattering was calculated based on the crystal structure and fit to the measured X-ray structure factor. The resulting intermolecular pair distribution functions revealed broad-nearest and next-nearest neighbor molecule-molecule correlations. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:1290-1300, 2013. Copyright © 2013 Wiley Periodicals, Inc.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-05-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

PubMed Central

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-01-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

Morphological imaging and quantification of axial xylem tissue in Fraxinus excelsior L. through X-ray micro-computed tomography.

PubMed

Koddenberg, Tim; Militz, Holger

2018-05-05

The popularity of X-ray based imaging methods has continued to increase in research domains. In wood research, X-ray micro-computed tomography (XμCT) is useful for structural studies examining the three-dimensional and complex xylem tissue of trees qualitatively and quantitatively. In this study, XμCT made it possible to visualize and quantify the spatial xylem organization of the angiosperm species Fraxinus excelsior L. on the microscopic level. Through image analysis, it was possible to determine morphological characteristics of the cellular axial tissue (vessel elements, fibers, and axial parenchyma cells) three-dimensionally. X-ray imaging at high resolutions provides very distinct visual insight into the xylem structure. Numerical analyses performed through semi-automatic procedures made it possible to quickly quantify cell characteristics (length, diameter, and volume of cells). Use of various spatial resolutions (0.87-5 μm) revealed boundaries users should be aware of. Nevertheless, our findings, both qualitative and quantitative, demonstrate XμCT to be a valuable tool for studying the spatial cell morphology of F. excelsior. Copyright © 2018. Published by Elsevier Ltd.

A protocol for searching the most probable phase-retrieved maps in coherent X-ray diffraction imaging by exploiting the relationship between convergence of the retrieved phase and success of calculation.

PubMed

Sekiguchi, Yuki; Hashimoto, Saki; Kobayashi, Amane; Oroguchi, Tomotaka; Nakasako, Masayoshi

2017-09-01

Coherent X-ray diffraction imaging (CXDI) is a technique for visualizing the structures of non-crystalline particles with size in the submicrometer to micrometer range in material sciences and biology. In the structural analysis of CXDI, the electron density map of a specimen particle projected along the direction of the incident X-rays can be reconstructed only from the diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction, relying entirely on the computational procedure, sometimes fails because diffraction patterns miss the data in small-angle regions owing to the beam stop and saturation of the detector pixels, and are modified by Poisson noise in X-ray detection. To date, X-ray free-electron lasers have allowed us to collect a large number of diffraction patterns within a short period of time. Therefore, the reconstruction of correct electron density maps is the bottleneck for efficiently conducting structure analyses of non-crystalline particles. To automatically address the correctness of retrieved electron density maps, a data analysis protocol to extract the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a single diffraction pattern is proposed. Through monitoring the variations of the phase values during PR calculations, the tendency for the PR calculations to succeed when the retrieved phase sets converged on a certain value was found. On the other hand, if the phase set was in persistent variation, the PR calculation tended to fail to yield the correct electron density map. To quantify this tendency, here a figure of merit for the variation of the phase values during PR calculation is introduced. In addition, a PR protocol to evaluate the similarity between a map of the highest figure of merit and other independently reconstructed maps is proposed. The protocol is implemented and practically examined in the structure analyses for diffraction patterns from aggregates of gold colloidal particles. Furthermore, the feasibility of the protocol in the structure analysis of organelles from biological cells is examined.

STARPROBE: A design study for an X-ray imaging instrument

NASA Technical Reports Server (NTRS)

1981-01-01

The primary objective of the X-ray imaging telescope on STARPROBE is the acquisition of very high spacial resolution observations during the spacecraft's perihelion passage. Design parameters, telescope prefilters, and structural and thermal analyses of the equipment are described and discussed. It is believed that the spatial resolution of the information recorded by the baseline design would be at least a factor of 10 better than can be reasonably expected from Earth orbit. Thermal models used in the study are also discussed.

Enhanced saturation of sputtered amorphous SiN film frameworks using He- and Ne-Penning effects

NASA Astrophysics Data System (ADS)

Sugimoto, Iwao; Nakano, Satoko; Kuwano, Hiroki

1994-06-01

Optical emission spectroscopy reveals that helium and neon gases enhance the nitridation reactivity of the nitrogen plasma by Penning effects during magnetron sputtering of the silicon target. These excited nitrogen plasmas promote the saturation of frameworks of the resultant silicon nitride films. X-ray photoelectron spectroscopy, electron spin resonance, and x-ray diffraction analyses provide insight into the structure of these films, and thermal desorption mass spectroscopy reveals the behavior of volatile species in these films.

Ensemble X-ray variability of active galactic nuclei. II. Excess variance and updated structure function

NASA Astrophysics Data System (ADS)

Vagnetti, F.; Middei, R.; Antonucci, M.; Paolillo, M.; Serafinelli, R.

2016-09-01

Context. Most investigations of the X-ray variability of active galactic nuclei (AGN) have been concentrated on the detailed analyses of individual, nearby sources. A relatively small number of studies have treated the ensemble behaviour of the more general AGN population in wider regions of the luminosity-redshift plane. Aims: We want to determine the ensemble variability properties of a rich AGN sample, called Multi-Epoch XMM Serendipitous AGN Sample (MEXSAS), extracted from the fifth release of the XMM-Newton Serendipitous Source Catalogue (XMMSSC-DR5), with redshift between ~0.1 and ~5, and X-ray luminosities in the 0.5-4.5 keV band between ~1042 erg/s and ~1047 erg/s. Methods: We urge caution on the use of the normalised excess variance (NXS), noting that it may lead to underestimate variability if used improperly. We use the structure function (SF), updating our previous analysis for a smaller sample. We propose a correction to the NXS variability estimator, taking account of the light curve duration in the rest frame on the basis of the knowledge of the variability behaviour gained by SF studies. Results: We find an ensemble increase of the X-ray variability with the rest-frame time lag τ, given by SF ∝ τ0.12. We confirm an inverse dependence on the X-ray luminosity, approximately as SF ∝ LX-0.19. We analyse the SF in different X-ray bands, finding a dependence of the variability on the frequency as SF ∝ ν-0.15, corresponding to a so-called softer when brighter trend. In turn, this dependence allows us to parametrically correct the variability estimated in observer-frame bands to that in the rest frame, resulting in a moderate (≲15%) shift upwards (V-correction). Conclusions: Ensemble X-ray variability of AGNs is best described by the structure function. An improper use of the normalised excess variance may lead to an underestimate of the intrinsic variability, so that appropriate corrections to the data or the models must be applied to prevent these effects. Full Table 1 is only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/593/A55

Determination of copper binding in Pseudomonas putida CZ1 by chemical modifications and X-ray absorption spectroscopy.

PubMed

Chen, XinCai; Shi, JiYan; Chen, YingXu; Xu, XiangHua; Chen, LiTao; Wang, Hui; Hu, TianDou

2007-03-01

Previously performed studies have shown that Pseudomonas putida CZ1 biomass can bind an appreciable amount of Cu(II) and Zn(II) ions from aqueous solutions. The mechanisms of Cu- and Zn-binding by P. putida CZ1 were ascertained by chemical modifications of the biomass followed by Fourier transform infrared and X-ray absorption spectroscopic analyses of the living or nonliving cells. A dramatic decrease in Cu(II)- and Zn(II)-binding resulted after acidic methanol esterification of the nonliving cells, indicating that carboxyl functional groups play an important role in the binding of metal to the biomaterial. X-ray absorption spectroscopy was used to determine the speciation of Cu ions bound by living and nonliving cells, as well as to elucidate which functional groups were involved in binding of the Cu ions. The X-ray absorption near-edge structure spectra analysis showed that the majority of the Cu was bound in both samples as Cu(II). The fitting results of Cu K-edge extended X-ray absorption fine structure spectra showed that N/O ligands dominated in living and nonliving cells. Therefore, by combining different techniques, our results indicate that carboxyl functional groups are the major ligands responsible for the metal binding in P. putida CZ1.

In situ chemical analyses of extraterrestrial bodies

NASA Technical Reports Server (NTRS)

Economou, Thanasis E.; Turkevich, Anthony L.

1988-01-01

One of the most important tasks on any sample return mission will have to be a quick sample characterization in order to guarantee a variety of collected samples. An alpha particle instrument with alpha, proton and X-ray modes can provide a quick and almost complete chemical analysis of Mars samples. This instrument is based on three interactions of the alpha particles from a radioactive source with matter: elastic scattering of the alpha particles by nuclei (alpha mode), (alpha,p) nuclear reaction with some light elements (proton mode), and excitation of the atomic structure of atoms by alpha particles, leading to emission of characteristic X-rays of the lunar surface at three sites during the Surveyor mission of 1967 to 1968. Since then the instrument has been improved and miniaturized substantially. As shown in the past, the alpha particle instrument can operate under Martian conditions without any degradation in the performance. The alpha and proton modes can provide vital information about the light elements, while the X-ray mode with its ambient temperature X-ray detector will be useful for the heavier elements. The excitation of the atomic structure is provided by the same alpha radioactive source that is used by alpha and proton modes or by an auxiliary X-ray source that is selected to enhance the sensitivity to some important geochemical elements.

Investigation of Synthetic Mg(1.3)V(1.7)O4 Spinel with MgO Inclusions: Case Study of a Spinel with an Apparently occupied Interstitial Site

NASA Technical Reports Server (NTRS)

Uchida, Hinako; Righter, Kevin; Lavina, Barbara; Nowell, Matthew M.; Wright, Stuart I.; Downs, Robert T.; Yang, Hexiong

2007-01-01

A magnesium vanadate spinel crystal, ideally MgV2O4, synthesized at 1 bar, 1200 C and equilibrated under FMQ + 1.3 log f(sub o2) condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies, along with the presence of 0.053 apfu Mg at an interstitial octahedral site . Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (less than or equal to 3microns) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscop[y (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (approx. 9%) of periclase reflections, which eliminated the interstitial Mg. This study provides insight into possible origins of refined interstitial cations reported in the the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.

Non Destructive 3D X-Ray Imaging of Nano Structures & Composites at Sub-30 NM Resolution, With a Novel Lab Based X-Ray Microscope

DTIC Science & Technology

2006-11-01

NON DESTRUCTIVE 3D X-RAY IMAGING OF NANO STRUCTURES & COMPOSITES AT SUB-30 NM RESOLUTION, WITH A NOVEL LAB BASED X- RAY MICROSCOPE S H Lau...article we describe a 3D x-ray microscope based on a laboratory x-ray source operating at 2.7, 5.4 or 8.0 keV hard x-ray energies. X-ray computed...tomography (XCT) is used to obtain detailed 3D structural information inside optically opaque materials with sub-30 nm resolution. Applications include

Comparative Analysis of Microbial Communities in Iron-Dominated Flocculent Mats in Deep-Sea Hydrothermal Environments

PubMed Central

Kikuchi, Sakiko; Mitsunobu, Satoshi; Takaki, Yoshihiro; Yamanaka, Toshiro; Toki, Tomohiro; Noguchi, Takuroh; Nakamura, Kentaro; Abe, Mariko; Hirai, Miho; Yamamoto, Masahiro; Uematsu, Katsuyuki; Miyazaki, Junichi; Nunoura, Takuro; Takahashi, Yoshio; Takai, Ken

2016-01-01

ABSTRACT It has been suggested that iron is one of the most important energy sources for photosynthesis-independent microbial ecosystems in the ocean crust. Iron-metabolizing chemolithoautotrophs play a key role as primary producers, but little is known about their distribution and diversity and their ecological role as submarine iron-metabolizing chemolithotrophs, particularly the iron oxidizers. In this study, we investigated the microbial communities in several iron-dominated flocculent mats found in deep-sea hydrothermal fields in the Mariana Volcanic Arc and Trough and the Okinawa Trough by culture-independent molecular techniques and X-ray mineralogical analyses. The abundance and composition of the 16S rRNA gene phylotypes demonstrated the ubiquity of zetaproteobacterial phylotypes in iron-dominated mat communities affected by hydrothermal fluid input. Electron microscopy with energy-dispersive X-ray microanalysis and X-ray absorption fine structure (XAFS) analysis revealed the chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species and the potential contribution of Zetaproteobacteria to the in situ generation. These results suggest that putative iron-oxidizing chemolithoautotrophs play a significant ecological role in producing iron-dominated flocculent mats and that they are important for iron and carbon cycles in deep-sea low-temperature hydrothermal environments. IMPORTANCE We report novel aspects of microbiology from iron-dominated flocculent mats in various deep-sea environments. In this study, we examined the relationship between Zetaproteobacteria and iron oxides across several hydrothermally influenced sites in the deep sea. We analyzed iron-dominated mats using culture-independent molecular techniques and X-ray mineralogical analyses. The scanning electron microscopy–energy-dispersive X-ray spectroscopy SEM-EDS analysis and X-ray absorption fine structure (XAFS) analysis revealed chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species as well as the potential contribution of the zetaproteobacterial population to the in situ production. These key findings provide important information for understanding the mechanisms of both geomicrobiological iron cycling and the formation of iron-dominated mats in deep-sea hydrothermal fields. PMID:27422841

Quantifying Mesoscale Neuroanatomy Using X-Ray Microtomography

PubMed Central

Gray Roncal, William; Prasad, Judy A.; Fernandes, Hugo L.; Gürsoy, Doga; De Andrade, Vincent; Fezzaa, Kamel; Xiao, Xianghui; Vogelstein, Joshua T.; Jacobsen, Chris; Körding, Konrad P.

2017-01-01

Methods for resolving the three-dimensional (3D) microstructure of the brain typically start by thinly slicing and staining the brain, followed by imaging numerous individual sections with visible light photons or electrons. In contrast, X-rays can be used to image thick samples, providing a rapid approach for producing large 3D brain maps without sectioning. Here we demonstrate the use of synchrotron X-ray microtomography (µCT) for producing mesoscale (∼1 µm 3 resolution) brain maps from millimeter-scale volumes of mouse brain. We introduce a pipeline for µCT-based brain mapping that develops and integrates methods for sample preparation, imaging, and automated segmentation of cells, blood vessels, and myelinated axons, in addition to statistical analyses of these brain structures. Our results demonstrate that X-ray tomography achieves rapid quantification of large brain volumes, complementing other brain mapping and connectomics efforts. PMID:29085899

[Fine stereo structure for natural organic molecules, a preliminary study. II. Melting point influenced by structure factors].

PubMed

Lu, Y; Zheng, Q; Lu, D; Ma, P; Chen, Y

1995-06-01

Crystal structures of two compounds from Tripterygium wilfordii Hook f. have been determined by X-ray diffraction method. Structure factors influencing melting point of solid state have been analysed. Crystal class (or space group), recrystallization solvent, force between molecules and fine changes of molecular structures will all cause melting point changes of crystal substance.

Predicting protein crystallization propensity from protein sequence

PubMed Central

2011-01-01

The high-throughput structure determination pipelines developed by structural genomics programs offer a unique opportunity for data mining. One important question is how protein properties derived from a primary sequence correlate with the protein’s propensity to yield X-ray quality crystals (crystallizability) and 3D X-ray structures. A set of protein properties were computed for over 1,300 proteins that expressed well but were insoluble, and for ~720 unique proteins that resulted in X-ray structures. The correlation of the protein’s iso-electric point and grand average hydropathy (GRAVY) with crystallizability was analyzed for full length and domain constructs of protein targets. In a second step, several additional properties that can be calculated from the protein sequence were added and evaluated. Using statistical analyses we have identified a set of the attributes correlating with a protein’s propensity to crystallize and implemented a Support Vector Machine (SVM) classifier based on these. We have created applications to analyze and provide optimal boundary information for query sequences and to visualize the data. These tools are available via the web site http://bioinformatics.anl.gov/cgi-bin/tools/pdpredictor. PMID:20177794

X-ray CT core imaging of Oman Drilling Project on D/V CHIKYU

NASA Astrophysics Data System (ADS)

Michibayashi, K.; Okazaki, K.; Leong, J. A. M.; Kelemen, P. B.; Johnson, K. T. M.; Greenberger, R. N.; Manning, C. E.; Harris, M.; de Obeso, J. C.; Abe, N.; Hatakeyama, K.; Ildefonse, B.; Takazawa, E.; Teagle, D. A. H.; Coggon, J. A.

2017-12-01

We obtained X-ray computed tomography (X-ray CT) images for all cores (GT1A, GT2A, GT3A and BT1A) in Oman Drilling Project Phase 1 (OmanDP cores), since X-ray CT scanning is a routine measurement of the IODP measurement plan onboard Chikyu, which enables the non-destructive observation of the internal structure of core samples. X-ray CT images provide information about chemical compositions and densities of the cores and is useful for assessing sample locations and the quality of the whole-round samples. The X-ray CT scanner (Discovery CT 750HD, GE Medical Systems) on Chikyu scans and reconstructs the image of a 1.4 m section in 10 minutes and produces a series of scan images, each 0.625 mm thick. The X-ray tube (as an X-ray source) and the X-ray detector are installed inside of the gantry at an opposing position to each other. The core sample is scanned in the gantry with the scanning rate of 20 mm/sec. The distribution of attenuation values mapped to an individual slice comprises the raw data that are used for subsequent image processing. Successive two-dimensional (2-D) slices of 512 x 512 pixels yield a representation of attenuation values in three-dimensional (3-D) voxels of 512 x 512 by 1600 in length. Data generated for each core consist of core-axis-normal planes (XY planes) of X-ray attenuation values with dimensions of 512 × 512 pixels in 9 cm × 9 cm cross-section, meaning at the dimensions of a core section, the resolution is 0.176 mm/pixel. X-ray intensity varies as a function of X-ray path length and the linear attenuation coefficient (LAC) of the target material is a function of the chemical composition and density of the target material. The basic measure of attenuation, or radiodensity, is the CT number given in Hounsfield units (HU). CT numbers of air and water are -1000 and 0, respectively. Our preliminary results show that CT numbers of OmanDP cores are well correlated to gamma ray attenuation density (GRA density) as a function of chemical composition and mineral density, so that their profiles with respect to the core depth provide quick lithological information such as mineral identification and phase boundary etc. Moreover, X-ray CT images can be used for 3-D fabric analyses of the whole core even after core cutting into halves for individual analyses.

Yes, one can obtain better quality structures from routine X-ray data collection.

PubMed

Sanjuan-Szklarz, W Fabiola; Hoser, Anna A; Gutmann, Matthias; Madsen, Anders Østergaard; Woźniak, Krzysztof

2016-01-01

Single-crystal X-ray diffraction structural results for benzidine dihydrochloride, hydrated and protonated N,N,N,N-peri(dimethylamino)naphthalene chloride, triptycene, dichlorodimethyltriptycene and decamethylferrocene have been analysed. A critical discussion of the dependence of structural and thermal parameters on resolution for these compounds is presented. Results of refinements against X-ray data, cut off to different resolutions from the high-resolution data files, are compared to structural models derived from neutron diffraction experiments. The Independent Atom Model (IAM) and the Transferable Aspherical Atom Model (TAAM) are tested. The average differences between the X-ray and neutron structural parameters (with the exception of valence angles defined by H atoms) decrease with the increasing 2θmax angle. The scale of differences between X-ray and neutron geometrical parameters can be significantly reduced when data are collected to the higher, than commonly used, 2θmax diffraction angles (for Mo Kα 2θmax > 65°). The final structural and thermal parameters obtained for the studied compounds using TAAM refinement are in better agreement with the neutron values than the IAM results for all resolutions and all compounds. By using TAAM, it is still possible to obtain accurate results even from low-resolution X-ray data. This is particularly important as TAAM is easy to apply and can routinely be used to improve the quality of structural investigations [Dominiak (2015 ▸). LSDB from UBDB. University of Buffalo, USA]. We can recommend that, in order to obtain more adequate (more accurate and precise) structural and displacement parameters during the IAM model refinement, data should be collected up to the larger diffraction angles, at least, for Mo Kα radiation to 2θmax = 65° (sin θmax/λ < 0.75 Å(-1)). The TAAM approach is a very good option to obtain more adequate results even using data collected to the lower 2θmax angles. Also the results of translation-libration-screw (TLS) analysis and vibrational entropy values are more reliable for 2θmax > 65°.

Facile fabrication of mesoporous Fe-Ti-SBA15 silica with enhanced visible-light-driven simultaneous photocatalytic degradation and reduction reactions

NASA Astrophysics Data System (ADS)

Chang, Fei; Jiao, Mingzhi; Xu, Quan; Deng, Baoqing; Hu, Xuefeng

2018-03-01

A series of mesoporous iron-titanium-containing silica Fe-TiO2-SBA15 (FTS) were constructed via a facile one-pot hydrothermal route and subsequently characterized by X-ray diffraction patterns, UV-vis diffuse reflection spectroscopy, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption-desorption, X-ray photoelectron spectroscopy, and X-ray energy dispersion spectroscopy. By analyses, these samples possessed ordered two-dimensional hexagonal mesoporous structures, mainly involving mixed dual-phases of anatase and rutile TiO2, like commercial titania P25. The UV-vis diffuse reflection spectra demonstrated the presence of Fe species that was further confirmed by the X-ray photoelectron spectra and X-ray energy dispersion spectrum. The existence of Fe species in form of Fe3+ cations played an important role on the phase composition and electronic structure of these samples. With structural and morphological merits, these samples exhibited relatively high photocatalytic efficiency toward the degradation of dye methylene blue (MB) and reduction of Cr(VI) under visible-light irradiation, comparing with P25. In addition, among all candidates, the sample with a Fe/Si molar ratio of 0.03 showed the highest catalytic performance under optimal conditions, especially in the coexistence of both MB and Cr(VI), revealing an obviously synergistic effect when the consumption of both contaminants occurred. Finally, a primary catalytic mechanism was speculated on basis of active species capture experiments.

Precision mechanical structure of an ultra-high-resolution spectrometer for inelastic X-ray scattering instrument

DOEpatents

Shu, Deming; Shvydko, Yuri; Stoupin, Stanislav A.; Khachatryan, Ruben; Goetze, Kurt A.; Roberts, Timothy

2015-04-14

A method and an ultrahigh-resolution spectrometer including a precision mechanical structure for positioning inelastic X-ray scattering optics are provided. The spectrometer includes an X-ray monochromator and an X-ray analyzer, each including X-ray optics of a collimating (C) crystal, a pair of dispersing (D) element crystals, anomalous transmission filter (F) and a wavelength (W) selector crystal. A respective precision mechanical structure is provided with the X-ray monochromator and the X-ray analyzer. The precision mechanical structure includes a base plate, such as an aluminum base plate; positioning stages for D-crystal alignment; positioning stages with an incline sensor for C/F/W-crystal alignment, and the positioning stages including flexure-based high-stiffness structure.

Design of a medium size x-ray mirror module based on thin glass foils

NASA Astrophysics Data System (ADS)

Basso, Stefano; Civitani, Marta; Pareschi, Giovanni

2016-07-01

The hot slumping glass technology for X-ray mirror is under development and in the last years the results have been improved. Nustar is the first X-ray telescope based on slumped glass foils and it benefit is the low cost compared to the direct polishing of glass. With the slumping technique it is possible to maintain the glass mass to low values with respect to the direct polishing, but in general the angular resolution is worst. A further technique based on glass is the cold shaping of foils. The improved capabilities of manufacturing thin glass foils, pushed by the industrial application for screens, open new possibilities for X-ray mirror. The increase in strength of thin tempered glasses, the reduction of thickness errors and the good roughness of flat foils are potentially great advantages. In this paper a design of a mediumsize X-ray mirror module is analysed. It is based on integration of glass foils, stacked directly on a supporting structure that is part of the X-ray telescope using stiffening ribs as spacer between foils. The alignment of each stack is performed directly into the integration machine avoiding the necessity of the alignment of different stacked modules. A typical module (glass optic and metallic structure) provides an effective area of 10 cm2/kg at 1 keV (with a mass of about 50- 100 kg and a focal length of 10 m).

Bendable X-ray Optics for High Resolution Imaging

NASA Technical Reports Server (NTRS)

Gubarev, M.; Ramsey, B.; Kilaru, K.; Atkins, C.; Broadway, D.

2014-01-01

Current state-of the-art for x-ray optics fabrication calls for either the polishing of massive substrates into high-angular-resolution mirrors or the replication of thin, lower-resolution, mirrors from perfectly figured mandrels. Future X-ray Missions will require a change in this optics fabrication paradigm in order to achieve sub-arcsecond resolution in light-weight optics. One possible approach to this is to start with perfectly flat, light-weight surface, bend it into a perfect cone, form the desired mirror figure by material deposition, and insert the resulting mirror into a telescope structure. Such an approach is currently being investigated at MSFC, and a status report will be presented detailing the results of finite element analyses, bending tests and differential deposition experiments.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Spatial structure and temporal development of a solar X-ray flare observed from Skylab on June 15, 1973

NASA Technical Reports Server (NTRS)

Pallavicini, R.; Vaiana, G. S.; Kahler, S. W.; Krieger, A. S.

1975-01-01

Morphological and quantitative analyses are presented of a 1B solar flare that was observed with high spatial and temporal resolution by the S-054 grazing-incidence X-ray telescope aboard Skylab. It is found that the flare had the configuration of a compact region with a characteristic size of the order of 30 arcsec at the intensity peak, the interior of the region appeared to be highly structured and to consist of temporally changing complex loop systems, brightening over an extended part of the active region preceded the flare onset, and the impulsive phase was marked by rapid brightening in the loop structures. The X-ray photographs also indicate that the X-ray emission was centered over the neutral line of the longitudinal magnetic field, loop systems formed at successively increasing heights during the decay phase, and different regions of the flare had distinctly different light curves. The flux profiles for the different regions are shown to suggest continued heating during the decay phase. It is concluded that flare models should be based on a multiplicity of volumes ordered in loops of successively larger scale lengths and heights rather than on a single point of energy release and deposition.

Electron Microscopy and Analytical X-ray Characterization of Compositional and Nanoscale Structural Changes in Fossil Bone

NASA Astrophysics Data System (ADS)

Boatman, Elizabeth Marie

The nanoscale structure of compact bone contains several features that are direct indicators of bulk tissue mechanical properties. Fossil bone tissues represent unique opportunities to understand the compact bone structure/property relationships from a deep time perspective, offering a possible array of new insights into bone diseases, biomimicry of composite materials, and basic knowledge of bioapatite composition and nanoscale bone structure. To date, most work with fossil bone has employed microscale techniques and has counter-indicated the survival of bioapatite and other nanoscale structural features. The obvious disconnect between the use of microscale techniques and the discernment of nanoscale structure has prompted this work. The goal of this study was to characterize the nanoscale constituents of fossil compact bone by applying a suite of diffraction, microscopy, and spectrometry techniques, representing the highest levels of spatial and energy resolution available today, and capable of complementary structural and compositional characterization from the micro- to the nanoscale. Fossil dinosaur and crocodile long bone specimens, as well as modern ratite and crocodile femurs, were acquired from the UC Museum of Paleontology. Preserved physiological features of significance were documented with scanning electron microscopy back-scattered imaging. Electron microprobe wavelength-dispersive X-ray spectroscopy (WDS) revealed fossil bone compositions enriched in fluorine with a complementary loss of oxygen. X-ray diffraction analyses demonstrated that all specimens were composed of apatite. Transmission electron microscopy (TEM) imaging revealed preserved nanocrystallinity in the fossil bones and electron diffraction studies further identified these nanocrystallites as apatite. Tomographic analyses of nanoscale elements imaged by TEM and small angle X-ray scattering were performed, with the results of each analysis further indicating that nanoscale structure is highly conserved in these four fossil specimens. Finally, the results of this study indicate that bioapatite can be preserved in even the most ancient vertebrate specimens, further supporting the idea that fossilization is a preservational process. This work also underlines the importance of using appropriately selected characterization and analytical techniques for the study of fossil bone, especially from the perspective of spatial resolution and the scale of the bone structural features in question.

Interaction Analysis of FABP4 Inhibitors by X-ray Crystallography and Fragment Molecular Orbital Analysis

PubMed Central

2016-01-01

X-ray crystal structural determination of FABP4 in complex with four inhibitors revealed the complex binding modes, and the resulting observations led to improvement of the inhibitory potency of FABP4 inhibitors. However, the detailed structure–activity relationship (SAR) could not be explained from these structural observations. For a more detailed understanding of the interactions between FABP4 and inhibitors, fragment molecular orbital analyses were performed. These analyses revealed that the total interfragment interaction energies of FABP4 and each inhibitor correlated with the ranking of the Ki value for the four inhibitors. Furthermore, interactions between each inhibitor and amino acid residues in FABP4 were identified. The oxygen atom of Lys58 in FABP4 was found to be very important for strong interactions with FABP4. These results might provide useful information for the development of novel potent FABP4 inhibitors. PMID:27096055

Use of a Passive Reaction Wheel Jitter Isolation System to Meet the Advanced X-Ray Astrophysics Facility Imaging Performance Requirements

NASA Technical Reports Server (NTRS)

Pendergast, Karl J.; Schauwecker, Christopher J.

1998-01-01

Third in the series of NASA great observatories, the Advanced X-Ray Astrophysics Facility (AXAF) is scheduled for launch from the Space Shuttle in November of 1998. Following in the path of the Hubble Space Telescope and the Compton Gamma Ray Observatory, this observatory will image light at X-ray wavelengths, facilitating the detailed study of such phenomena as supernovae and quasars. The AXAF project is sponsored by the Marshall Space Flight Center in Huntsville, Alabama. Because of exacting requirements on the performance of the AXAF optical system, it was necessary to reduce the transmission of reaction wheel jitter disturbances to the observatory. This reduction was accomplished via use of a passive mechanical isolation system to interface the reaction wheels with the spacecraft central structure. In addition to presenting a description of the spacecraft, the isolation system, and the key image quality requirement flowdown, this paper details the analyses performed in support of system-level imaging performance requirement verification. These analyses include the identification of system-level requirement suballocations, quantification of imaging and pointing performance, and formulation of unit-level isolation system transmissibility requirements. Given in comparison to the non-isolated system imaging performance, the results of these analyses clearly illustrate the effectiveness of an innovative reaction wheel passive isolation system.

Relationship between radiation dose reduction and image quality change in photostimulable phosphor luminescence X-ray imaging systems.

PubMed

Sakurai, T; Kawamata, R; Kozai, Y; Kaku, Y; Nakamura, K; Saito, M; Wakao, H; Kashima, I

2010-05-01

The aim of the study was to clarify the change in image quality upon X-ray dose reduction and to re-analyse the possibility of X-ray dose reduction in photostimulable phosphor luminescence (PSPL) X-ray imaging systems. In addition, the study attempted to verify the usefulness of multiobjective frequency processing (MFP) and flexible noise control (FNC) for X-ray dose reduction. Three PSPL X-ray imaging systems were used in this study. Modulation transfer function (MTF), noise equivalent number of quanta (NEQ) and detective quantum efficiency (DQE) were evaluated to compare the basic physical performance of each system. Subjective visual evaluation of diagnostic ability for normal anatomical structures was performed. The NEQ, DQE and diagnostic ability were evaluated at base X-ray dose, and 1/3, 1/10 and 1/20 of the base X-ray dose. The MTF of the systems did not differ significantly. The NEQ and DQE did not necessarily depend on the pixel size of the system. The images from all three systems had a higher diagnostic utility compared with conventional film images at the base and 1/3 X-ray doses. The subjective image quality was better at the base X-ray dose than at 1/3 of the base dose in all systems. The MFP and FNC-processed images had a higher diagnostic utility than the images without MFP and FNC. The use of PSPL imaging systems may allow a reduction in the X-ray dose to one-third of that required for conventional film. It is suggested that MFP and FNC are useful for radiation dose reduction.

Assessing the Chemical Accuracy of Protein Structures via Peptide Acidity

PubMed Central

Anderson, Janet S.; Hernández, Griselda; LeMaster, David M.

2012-01-01

Although the protein native state is a Boltzmann conformational ensemble, practical applications often require a representative model from the most populated region of that distribution. The acidity of the backbone amides, as reflected in hydrogen exchange rates, is exquisitely sensitive to the surrounding charge and dielectric volume distribution. For each of four proteins, three independently determined X-ray structures of differing crystallographic resolution were used to predict exchange for the static solvent-exposed amide hydrogens. The average correlation coefficients range from 0.74 for ubiquitin to 0.93 for Pyrococcus furiosus rubredoxin, reflecting the larger range of experimental exchange rates exhibited by the latter protein. The exchange prediction errors modestly correlate with the crystallographic resolution. MODELLER 9v6-derived homology models at ~60% sequence identity (36% identity for chymotrypsin inhibitor CI2) yielded correlation coefficients that are ~0.1 smaller than for the cognate X-ray structures. The most recently deposited NOE-based ubiquitin structure and the original NMR structure of CI2 fail to provide statistically significant predictions of hydrogen exchange. However, the more recent RECOORD refinement study of CI2 yielded predictions comparable to the X-ray and homology model-based analyses. PMID:23182463

Low temperature nucleation of Griffiths Phase in Co doped LaMnO3 nanostructures

NASA Astrophysics Data System (ADS)

Adeela, N.; Khan, U.; Naz, S.; Iqbal, M.; Irfan, M.; Cheng, Y.

2017-11-01

We have reported magnetic properties of La1-xCoxMnO3 nanostructures synthesized by hydrothermal route. The crystal structure has been characterized by X-ray diffraction (XRD) technique, which shows rhombohedral perovskite structure at room temperature. Scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS) have been used to analyse morphology and chemical composition of prepared nanoparticles. Magnetic hysteresis loops of all the samples exhibit ferromagnetic behaviour at 10 K. Inverse susceptibility graphs as a function of temperature represent deviation from Curie Weiss law. The indication for short range ferromagnetic clusters well above Curie temperature is observed due to the Griffiths Phase (GP). It is proposed that the presence of GP arises from induced size effects of La and Co ions.

Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

DOE PAGES

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

2016-11-04

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

Lattice and Valence Electronic Structures of Crystalline Octahedral Molybdenum Halide Clusters-Based Compounds, Cs2[Mo6X14] (X = Cl, Br, I), Studied by Density Functional Theory Calculations.

PubMed

Saito, Norio; Cordier, Stéphane; Lemoine, Pierric; Ohsawa, Takeo; Wada, Yoshiki; Grasset, Fabien; Cross, Jeffrey S; Ohashi, Naoki

2017-06-05

The electronic and crystal structures of Cs 2 [Mo 6 X 14 ] (X = Cl, Br, I) cluster-based compounds were investigated by density functional theory (DFT) simulations and experimental methods such as powder X-ray diffraction, ultraviolet-visible spectroscopy, and X-ray photoemission spectroscopy (XPS). The experimentally determined lattice parameters were in good agreement with theoretically optimized ones, indicating the usefulness of DFT calculations for the structural investigation of these clusters. The calculated band gaps of these compounds reproduced those experimentally determined by UV-vis reflectance within an error of a few tenths of an eV. Core-level XPS and effective charge analyses indicated bonding states of the halogens changed according to their sites. The XPS valence spectra were fairly well reproduced by simulations based on the projected electron density of states weighted with cross sections of Al K α , suggesting that DFT calculations can predict the electronic properties of metal-cluster-based crystals with good accuracy.

Electronic and atomic structures of Ti{sub 1-x}Al{sub x}N thin films related to their damage behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tuilier, M.-H.; Pac, M.-J.; Girleanu, M.

2008-04-15

Ti and Al K-edge x-ray absorption spectroscopy is used to investigate the electronic structure of Ti{sub 1-x}Al{sub x}N thin films deposited by reactive magnetron sputtering. The experimental near edge spectra of TiN and AlN are interpreted in the light of unoccupied density of state band structure calculations. The comparison of the structural parameters derived from x-ray absorption fine structure and x-ray diffraction reveals segregation between Al-rich and Ti-rich domains within the Ti{sub 1-x}Al{sub x}N films. Whereas x-ray diffraction probes only the crystallized domains, the structural information derived from extended x-ray absorption fine structure analysis turns on both crystalline and grainmore » boundaries. The results are discussed by considering the damage behavior of the films depending on the composition.« less

Electronic structure and optical properties of CdSxSe1-x solid solution nanostructures from X-ray absorption near edge structure, X-ray excited optical luminescence, and density functional theory investigations

NASA Astrophysics Data System (ADS)

Murphy, M. W.; Yiu, Y. M.; Ward, M. J.; Liu, L.; Hu, Y.; Zapien, J. A.; Liu, Yingkai; Sham, T. K.

2014-11-01

The electronic structure and optical properties of a series of iso-electronic and iso-structural CdSxSe1-x solid solution nanostructures have been investigated using X-ray absorption near edge structure, extended X-ray absorption fine structure, and X-ray excited optical luminescence at various absorption edges of Cd, S, and Se. It is found that the system exhibits compositions, with variable local structure in-between that of CdS and CdSe accompanied by tunable optical band gap between that of CdS and CdSe. Theoretical calculation using density functional theory has been carried out to elucidate the observations. It is also found that luminescence induced by X-ray excitation shows new optical channels not observed previously with laser excitation. The implications of these observations are discussed.

Influence of annealing on X-ray radiation sensing properties of TiO2 thin film

NASA Astrophysics Data System (ADS)

Sarma, M. P.; Kalita, J. M.; Wary, G.

2018-03-01

A recent study shows that the titanium dioxide (TiO2) thin film synthesised by a chemical bath deposition technique is a very useful material for the X-ray radiation sensor. In this work, we reported the influence of annealing on the X-ray radiation detection sensitivity of the TiO2 film. The films were annealed at 333 K, 363 K, 393 K, 473 K, and 573 K for 1 hour. Structural analyses showed that the microstrain and dislocation density decreased whereas the average crystallite size increased with annealing. The band gap of the films also decreased from 3.26 eV to 3.10 eV after annealing. The I-V characteristics record under the dark condition and under the X-ray irradiation showed that the conductivity increased with annealing. The influence of annealing on the detection sensitivity was negligible if the bias voltage applied across the films was low (within 0.2 V‒1.0 V). At higher bias voltage (>1.0 V), the contribution of electrons excited by X-ray became less significant which affected the detection sensitivity.

Weak lensing calibration of mass bias in the REFLEX+BCS X-ray galaxy cluster catalogue

NASA Astrophysics Data System (ADS)

Simet, Melanie; Battaglia, Nicholas; Mandelbaum, Rachel; Seljak, Uroš

2017-04-01

The use of large, X-ray-selected Galaxy cluster catalogues for cosmological analyses requires a thorough understanding of the X-ray mass estimates. Weak gravitational lensing is an ideal method to shed light on such issues, due to its insensitivity to the cluster dynamical state. We perform a weak lensing calibration of 166 galaxy clusters from the REFLEX and BCS cluster catalogue and compare our results to the X-ray masses based on scaled luminosities from that catalogue. To interpret the weak lensing signal in terms of cluster masses, we compare the lensing signal to simple theoretical Navarro-Frenk-White models and to simulated cluster lensing profiles, including complications such as cluster substructure, projected large-scale structure and Eddington bias. We find evidence of underestimation in the X-ray masses, as expected, with = 0.75 ± 0.07 stat. ±0.05 sys. for our best-fitting model. The biases in cosmological parameters in a typical cluster abundance measurement that ignores this mass bias will typically exceed the statistical errors.

Solvation structure of the halides from x-ray absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Antalek, Matthew; Hedman, Britt; Sarangi, Ritimukta, E-mail: ritis@slac.stanford.edu

2016-07-28

Three-dimensional models for the aqueous solvation structures of chloride, bromide, and iodide are reported. K-edge extended X-ray absorption fine structure (EXAFS) and Minuit X-ray absorption near edge (MXAN) analyses found well-defined single shell solvation spheres for bromide and iodide. However, dissolved chloride proved structurally distinct, with two solvation shells needed to explain its strikingly different X-ray absorption near edge structure (XANES) spectrum. Final solvation models were as follows: iodide, 8 water molecules at 3.60 ± 0.13 Å and bromide, 8 water molecules at 3.40 ± 0.14 Å, while chloride solvation included 7 water molecules at 3.15 ± 0.10 Å, andmore » a second shell of 7 water molecules at 4.14 ± 0.30 Å. Each of the three derived solvation shells is approximately uniformly disposed about the halides, with no global asymmetry. Time-dependent density functional theory calculations simulating the chloride XANES spectra following from alternative solvation spheres revealed surprising sensitivity of the electronic state to 6-, 7-, or 8-coordination, implying a strongly bounded phase space for the correct structure during an MXAN fit. MXAN analysis further showed that the asymmetric solvation predicted from molecular dynamics simulations using halide polarization can play no significant part in bulk solvation. Classical molecular dynamics used to explore chloride solvation found a 7-water solvation shell at 3.12 (−0.04/+0.3) Å, supporting the experimental result. These experiments provide the first fully three-dimensional structures presenting to atomic resolution the aqueous solvation spheres of the larger halide ions.« less

Iodate in calcite and vaterite: Insights from synchrotron X-ray absorption spectroscopy and first-principles calculations

NASA Astrophysics Data System (ADS)

Podder, J.; Lin, J.; Sun, W.; Botis, S. M.; Tse, J.; Chen, N.; Hu, Y.; Li, D.; Seaman, J.; Pan, Y.

2017-02-01

Calcium carbonates such as calcite are the dominant hosts of inorganic iodine in nature and are potentially important for the retention and removal of radioactive iodine isotopes (129I and 131I) in contaminated water. However, little is known about the structural environment of iodine in carbonates. In this study, iodate (IO3-) doped calcite and vaterite have been synthesized using the gel-diffusion method at three NaIO3 concentrations (0.002; 0.004; 0.008 M) and a pH value of 9.0, under ambient temperature and pressure. Inductively coupled plasma mass spectrometry (ICP-MS) analyses show that iodine is preferentially incorporated into calcite over vaterite. Synchrotron iodine K-edge X-ray absorption near-edge structure (XANES) spectra confirm that IO3- is the dominant iodine species in synthetic calcite and vaterite. Analyses of iodine K-edge extended X-ray absorption fine structure (EXAFS) data, complemented by periodic first-principles calculations at the density functional theory (DFT) levels, demonstrate that the I5+ ion of the IO3- group in calcite and vaterite is bonded by three and two additional O atoms (i.e., coordination numbers = 6 and 5), respectively, and is incorporated via the charged coupled substitution I5+ + Na+ ↔ C4+ + Ca2+, with the Na+ cation at a nearest Ca2+ site being the most energetically favorable configuration.

XMM-Newton studies of the supernova remnant G350.0-2.0

NASA Astrophysics Data System (ADS)

Karpova, A.; Shternin, P.; Zyuzin, D.; Danilenko, A.; Shibanov, Yu.

2016-11-01

We report the results of XMM-Newton observations of the Galactic mixed-morphology supernova remnant G350.0-2.0. Diffuse thermal X-ray emission fills the north-western part of the remnant surrounded by radio shell-like structures. We did not detect any X-ray counterpart of the latter structures, but found several bright blobs within the diffuse emission. The X-ray spectrum of the most part of the remnant can be described by a collisionally ionized plasma model VAPEC with solar abundances and a temperature of ≈0.8 keV. The solar abundances of plasma indicate that the X-ray emission comes from the shocked interstellar material. The overabundance of Fe was found in some of the bright blobs. We also analysed the brightest point-like X-ray source 1RXS J172653.4-382157 projected on the extended emission. Its spectrum is well described by the two-temperature optically thin thermal plasma model MEKAL typical for cataclysmic variable stars. The cataclysmic variable source nature is supported by the presence of a faint (g ≈ 21) optical source with non-stellar spectral energy distribution at the X-ray position of 1RXS J172653.4-382157. It was detected with the XMM-Newton optical/UV monitor in the U filter and was also found in the archival Hα and optical/near-infrared broad-band sky survey images. On the other hand, the X-ray spectrum is also described by the power law plus thermal component model typical for a rotation powered pulsar. Therefore, the pulsar interpretation of the source cannot be excluded. For this source, we derived the upper limit for the pulsed fraction of 27 per cent.

Mechanical design of a precision linear flexural stage for 3D x-ray diffraction microscope at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Shu, D.; Liu, W.; Kearney, S.; Anton, J.; Tischler, J. Z.

2015-09-01

The 3-D X-ray diffraction microscope is a new nondestructive tool for the three-dimensional characterization of mesoscopic materials structure. A flexural-pivot-based precision linear stage has been designed to perform a wire scan as a differential aperture for the 3-D diffraction microscope at the Advanced Photon Source, Argonne National Laboratory. The mechanical design and finite element analyses of the flexural stage, as well as its initial mechanical test results with laser interferometer are described in this paper.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

High spin state driven magnetism and thermoelectricity in Mn doped topological insulator Bi2Se3

NASA Astrophysics Data System (ADS)

Maurya, V. K.; Dong, C. L.; Chen, C. L.; Asokan, K.; Patnaik, S.

2018-06-01

We report on the synthesis, and structural - magnetic characterizations of Mn doped Bi2Se3 towards achieving a magnetically doped topological insulator. High quality single crystals of MnxBi2-xSe3 (x = 0, 0.03, 0.05, 0.1) are grown and analysed by X-ray diffraction (XRD), Low Energy Electron Diffraction (LEED), Scanning electron microscopy (SEM), and X-ray absorption near-edge structure spectroscopy (XANES). Magnetic properties of these samples under ZFC-FC protocol and isothermal magnetization confirm ferromagnetic correlation above x = 0.03 value. XANES measurements confirm that the dopant Mn is in Mn2+ state. This is further reconfirmed to be in high spin state by fitting magnetic data with Brillouin function for J = 5/2. Both Hall and Seebeck measurements indicate a sign change of charge carriers above x = 0.03 value of Mn doping. We propose Mn doped Bi2Se3 to be a potential candidate for electromagnetic and thermoelectric device applications involving topological surface states.

Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II) Complex with a Tridentate Ligand 4′-Chloro-2,2′:6′,2′′-Terpyridine

PubMed Central

Saghatforoush, L. A.; Valencia, L.; Chalabian, F.; Ghammamy, Sh.

2011-01-01

A new Cd(II) complex with the ligand 4′-chloro-2,2′6′,2′′-terpyridine (Cltpy), [Cd(Cltpy)(I)2], has been synthesized and characterized by CHN elemental analysis, 1H-NMR, 13C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy) N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II) complex are tested against different bacteria. PMID:21738495

Probing high-redshift clusters with HST/ACS gravitational weak-lensing and Chandra x-ray observations

NASA Astrophysics Data System (ADS)

Jee, Myungkook James

2006-06-01

Clusters of galaxies, the largest gravitationally bound objects in the Universe, are useful tracers of cosmic evolution, and particularly detailed studies of still-forming clusters at high-redshifts can considerably enhance our understanding of the structure formation. We use two powerful methods that have become recently available for the study of these distant clusters: spaced- based gravitational weak-lensing and high-resolution X-ray observations. Detailed analyses of five high-redshift (0.8 < z < 1.3) clusters are presented based on the deep Advanced Camera for Surveys (ACS) and Chandra X-ray images. We show that, when the instrumental characteristics are properly understood, the newly installed ACS on the Hubble Space Telescope (HST) can detect subtle shape distortions of background galaxies down to the limiting magnitudes of the observations, which enables the mapping of the cluster dark matter in unprecedented high-resolution. The cluster masses derived from this HST /ACS weak-lensing study have been compared with those from the re-analyses of the archival Chandra X-ray data. We find that there are interesting offsets between the cluster galaxy, intracluster medium (ICM), and dark matter centroids, and possible scenarios are discussed. If the offset is confirmed to be uniquitous in other clusters, the explanation may necessitate major refinements in our current understanding of the nature of dark matter, as well as the cluster galaxy dynamics. CL0848+4452, the highest-redshift ( z = 1.27) cluster yet detected in weak-lensing, has a significant discrepancy between the weak- lensing and X-ray masses. If this trend is found to be severe and common also for other X-ray weak clusters at redshifts beyond the unity, the conventional X-ray determination of cluster mass functions, often inferred from their immediate X-ray properties such as the X-ray luminosity and temperature via the so-called mass-luminosity (M-L) and mass-temperature (M-T) relations, will become highly unstable in this redshift regime. Therefore, the relatively unbiased weak-lensing measurements of the cluster mass properties can be used to adequately calibrate the scaling relations in future high-redshift cluster investigations.

XMM-Newton spectroscopy of the accreting magnetar candidate 4U0114+65

NASA Astrophysics Data System (ADS)

Sanjurjo-Ferrrín, G.; Torrejón, J. M.; Postnov, K.; Oskinova, L.; Rodes-Roca, J. J.; Bernabeu, G.

2017-10-01

Aims: 4U0114+65 is one of the slowest known X-ray pulsars. We present an analysis of a pointed observation by the XMM-Newton X-ray telescope in order to study the nature of the X-ray pulsations and the accretion process, and to diagnose the physical properties of the donor's stellar wind. Methods: We analysed the energy-resolved light curve and the time-resolved X-ray spectra provided by the EPIC cameras on board XMM-Newton. We also analysed the first high-resolution spectrum of this source provided by the Reflection Grating Spectrometer. Results: An X-ray pulse of 9350 ± 160 s was measured. Comparison with previous measurements confirms the secular spin up of this source. We successfully fit the pulse-phase-resolved spectra with Comptonisation models. These models imply a very small (r 3 km) and hot (kT 2 - 3 keV) emitting region and therefore point to a hot spot over the neutron star (NS) surface as the most reliable explanation for the X-ray pulse. The long NS spin period, the spin-up rate, and persistent X-ray emission can be explained within the theory of quasi-spherical settling accretion, which may indicate that the magnetic field is in the magnetar range. Thus, 4U 0114+65 could be a wind-accreting magnetar. We also observed two episodes of low luminosity. The first was only observed in the low-energy light curve and can be explained as an absorption by a large over-dense structure in the wind of the B1 supergiant donor. The second episode, which was deeper and affected all energies, may be due to temporal cessation of accretion onto one magnetic pole caused by non-spherical matter capture from the structured stellar wind. The light curve displays two types of dips that are clearly seen during the high-flux intervals. The short dips, with durations of tens of seconds, are produced through absorption by wind clumps. The long dips, in turn, seem to be associated with the rarefied interclump medium. From the analysis of the X-ray spectra, we found evidence of emission lines in the X-ray photoionised wind of the B1Ia donor. The Fe Kα line was found to be highly variable and much weaker than in other X-ray binaries with supergiant donors. The degree of wind clumping, measured through the covering fraction, was found to be much lower than in supergiant donor stars with earlier spectral types. Conclusions: The XMM-Newton spectroscopy provided further support for the magnetar nature of the neutron star in 4U0114+65. The light curve presents dips that can be associated with clumps and the interclump medium in the stellar wind of the mass donor.

Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

PubMed

Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

2011-01-01

Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

X-Ray Absorption Near Edge Structure And Extended X-Ray Absorption Fine Structure Analysis of Standards And Biological Samples Containing Mixed Oxidation States of Chromium(III) And Chromium(VI)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Parsons, J.G.; Dokken, K.; Peralta-Videa, J.R.

For the first time a method has been developed for the extended X-ray absorption fine structure (EXAFS) data analyses of biological samples containing multiple oxidation states of chromium. In this study, the first shell coordination and interatomic distances based on the data analysis of known standards of potassium chromate (Cr(VI)) and chromium nitrate hexahydrate (Cr(III)) were investigated. The standards examined were mixtures of the following molar ratios of Cr(VI):Cr(III), 0:1, 0.25:0.75, 0.5:0.5, 0.75:0.25, and 1:0. It was determined from the calibration data that the fitting error associated with linear combination X-ray absorption near edge structure (LC-XANES) fittings was approximately {+-}10%more » of the total fitting. The peak height of the Cr(VI) pre-edge feature after normalization of the X-ray absorption (XAS) spectra was used to prepare a calibration curve. The EXAFS fittings of the standards were also investigated and fittings to lechuguilla biomass samples laden with different ratios of Cr(III) and Cr(VI) were performed as well. An excellent agreement between the XANES data and the data presented in the EXAFS spectra was observed. The EXFAS data also presented mean coordination numbers directly related to the ratios of the different chromium oxidation states in the sample. The chromium oxygen interactions had two different bond lengths at approximately 1.68 and 1.98 {angstrom} for the Cr(VI) and Cr(III) in the sample, respectively.« less

A little adjustment of synthetic strategy led to a new highly repeated heteropolyblue: Structure, characterizations and photocatalytic properties

NASA Astrophysics Data System (ADS)

Chen, Wu-Hua; Zhang, Zhu-Sen; Zhao, Jin-Hua; Qiu, Ze-Hai; Yuan, Qiu-Lan; Huang, Tian-Fu; Lin, Xue-Yu; Hu, Zhi-Biao

2017-06-01

Hydrothermal synthesis is known as the most efficient method to prepare novel structural polyoxometalate (POM)-based materials, but controlled synthesis of a structure-directing POM is always challenging task. The experimental repeatability is usually one of the key topics. To explore a reliable hydrothermal synthesis approach for new POMs will be a meaningful work. Our previous work, which we have hydrothermally synthesized the first Cr-complexes-capped Keggin-type POM, [Hdma]3[H2phen]{[Cr(phen)]2[MoV8MoVI4O36(PO4)]}·nH2O (n ≈ 2) (Chen et al., polyhedron, 2015, 85, 117), afford us some commendable synthetic experiences, arouse us some introspections as well for its tricky preparation conditions and low experimental repeatability. Based on the aforementioned work, a new high-repetition-rate and more steady heteropolyblue, [H3O]0.5(Hdma)2.5(dma)0.25{[Cr(phen)]2[MoV6MoVI6O8(PO4)]}·2H2O (1) (dma = dimethylamine (C2H7N), phen = 1,10-phenanthroline (C12H8N2)), has been successfully obtained by virtue of reasonably adjusting synthetic strategy. The adjustment of synthetic strategy includes controlling ratio of reactants and aging time, reasonably using redoxes and stepwise self-assembly plans. Compound 1 is the second POM with Keggin-type polyanion capped by Cr-complexes. Experiments demonstrate that compound 1 has good catalytic activity in the both degradation reactions of rhodamine B (RHB) and methyl orange (MO) under ultraviolet (UV)-light and oxidant H2O2 conditions. Detailed structural characterizations include single-crystal X-ray diffraction (XRD) analyses, energy-dispersive X-ray spectrometry (EDS) analyses, elemental analyses, cerate oxidimetry, powder XRD, fourier transform infrared (FT-IR) spectroscopy, ultraviolet-visible-near-infrared (UV-Vis-NIR) solid diffuse reflection spectrum and X-ray photoelectron spectroscopy (XPS) analyses. The electrochemical property (cyclic voltammetry (CV)) of compound 1 has also been studied.

Model-based Approaches for the Determination of Lipid Bilayer Structure from Small-Angle Neutron and X-ray Scattering Data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Heberle, Frederick A; Pan, Jianjun; Standaert, Robert F

2012-01-01

Some of our recent work has resulted in the detailed structures of fully hydrated, fluid phase phosphatidylcholine (PC) and phosphatidylglycerol (PG) bilayers. These structures were obtained from the joint refinement of small-angle neutron and X-ray data using the scattering density profile (SDP) models developed by Ku erka et al. (Ku erka et al. 2012; Ku erka et al. 2008). In this review, we first discuss models for the standalone analysis of neutron or X-ray scattering data from bilayers, and assess the strengths and weaknesses inherent in these models. In particular, it is recognized that standalone data do not contain enoughmore » information to fully resolve the structure of inherently disordered fluid bilayers, and therefore may not provide a robust determination of bilayer structural parameters, including the much sought after area per lipid. We then discuss the development of matter density-based models (including the SDP model) that allow for the joint refinement of different contrast neutron and X-ray data sets, as well as the implementation of local volume conservation in the unit cell (i.e., ideal packing). Such models provide natural definitions of bilayer thicknesses (most importantly the hydrophobic and Luzzati thicknesses) in terms of Gibbs dividing surfaces, and thus allow for the robust determination of lipid areas through equivalent slab relationships between bilayer thickness and lipid volume. In the final section of this review, we discuss some of the significant findings/features pertaining to structures of PC and PG bilayers as determined from SDP model analyses.« less

Modelling the atomic structure of Al92U8 metallic glass.

PubMed

Michalik, S; Bednarcik, J; Jóvári, P; Honkimäki, V; Webb, A; Franz, H; Fazakas, E; Varga, L K

2010-10-13

The local atomic structure of the glassy Al(92)U(8) alloy was modelled by the reverse Monte Carlo (RMC) method, fitting x-ray diffraction (XRD) and extended x-ray absorption fine structure (EXAFS) signals. The final structural model was analysed by means of partial pair correlation functions, coordination number distributions and Voronoi tessellation. In our study we found that the most probable atomic separations between Al-Al and U-Al pairs in the glassy Al(92)U(8) alloy are 2.7 Å and 3.1 Å with coordination numbers 11.7 and 17.1, respectively. The Voronoi analysis did not support evidence of the existence of well-defined building blocks directly embedded in the amorphous matrix. The dense-random-packing model seems to be adequate for describing the connection between solvent and solute atoms.

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

X-ray analyses of thermally grown and reactively sputtered tantalum oxide films on NiTi alloy

NASA Astrophysics Data System (ADS)

McNamara, Karrina; Tofail, Syed A. M.; Conroy, Derek; Butler, James; Gandhi, Abbasi A.; Redington, Wynette

2012-08-01

Sputter deposition of tantalum (Ta) on the surface of NiTi alloy is expected to improve the alloy's corrosion resistance and biocompatibility. Tantalum is a well-known biomaterial which is not affected by body fluids and is not irritating to human tissue. Here we compare the oxidation chemistry crystal structure evolution of tantalum oxide films grown on NiTi by reactive O2 sputtering and by thermal oxidation of sputter deposited Ta films. The effect of sputtering parameters and post-sputtering treatments on the morphology, oxidation state and crystal structure of the tantalum oxide layer have been investigated by field-emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The study has found that it may be better to avoid oxidation at and above 600 °C. The study establishes that reactive sputtering in presence of low oxygen mixture yields thicker film with better control of the film quality except that the surface oxidation state of Ta is slightly lower.

Effect of Electron Beam Irradiation on Structural and Optical Properties of Cu-Doped In2O3 Films Prepared by RF Magnetron Sputtering

NASA Astrophysics Data System (ADS)

Krishnan, R. Reshmi; Sanjeev, Ganesh; Prabhu, Radhakrishna; Pillai, V. P. Mahadevan

2018-02-01

Undoped and Cu-doped In2O3 films were prepared by radiofrequency magnetron sputtering technique. The effects of Cu doping and high-energy electron beam irradiation on the structural and optical properties of as-prepared films were investigated using techniques such as x-ray diffraction, x-ray photoelectron spectroscopy (XPS), lateral scanning electron microscopic image analysis, energy-dispersive x-ray (EDX) spectroscopy, micro-Raman, and ultraviolet-visible (UV-vis) spectroscopy. Moderate doping of Cu in In2O3 enhanced the intensity of (222) peak, indicating alignment of crystalline grains along <111>. Electron beam irradiation promoted orientation of crystalline grains along <111> in undoped and moderately Cu-doped films. EDX spectroscopic and XPS analyses revealed incorporation of Cu2+ ions in the lattice. The transmittance of Cu-doped films decreased with e-beam irradiation. Systematic reduction of the bandgap energy with increase in Cu doping concentration was seen in unirradiated and electron-beam-irradiated films.

Myoanatomy of the velvet worm leg revealed by laboratory-based nanofocus X-ray source tomography.

PubMed

Müller, Mark; de Sena Oliveira, Ivo; Allner, Sebastian; Ferstl, Simone; Bidola, Pidassa; Mechlem, Korbinian; Fehringer, Andreas; Hehn, Lorenz; Dierolf, Martin; Achterhold, Klaus; Gleich, Bernhard; Hammel, Jörg U; Jahn, Henry; Mayer, Georg; Pfeiffer, Franz

2017-11-21

X-ray computed tomography (CT) is a powerful noninvasive technique for investigating the inner structure of objects and organisms. However, the resolution of laboratory CT systems is typically limited to the micrometer range. In this paper, we present a table-top nanoCT system in conjunction with standard processing tools that is able to routinely reach resolutions down to 100 nm without using X-ray optics. We demonstrate its potential for biological investigations by imaging a walking appendage of Euperipatoides rowelli , a representative of Onychophora-an invertebrate group pivotal for understanding animal evolution. Comparative analyses proved that the nanoCT can depict the external morphology of the limb with an image quality similar to scanning electron microscopy, while simultaneously visualizing internal muscular structures at higher resolutions than confocal laser scanning microscopy. The obtained nanoCT data revealed hitherto unknown aspects of the onychophoran limb musculature, enabling the 3D reconstruction of individual muscle fibers, which was previously impossible using any laboratory-based imaging technique.

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

The electronic structure of lithium metagallate.

PubMed

Johnson, N W; McLeod, J A; Moewes, A

2011-11-09

Herein we present a study of the electronic structure of lithium metagallate (LiGaO(2)), a material of interest in the field of optoelectronics. We use soft x-ray spectroscopy to probe the electronic structure of both the valence and conduction bands and compare our measurements to ab initio density functional theory calculations. We use several different exchange-correlation functionals, but find that no single theoretical approach used herein accurately quantifies both the band gap and the Ga 3d(10) states in LiGaO(2). We derive a band gap of 5.6 eV, and characterize electron hybridization in both the valence and conduction bands. Our study of the x-ray spectra may prove useful in analysing spectra from more complicated LiGaO(2) heterostructures. © 2011 IOP Publishing Ltd

X-ray Point Source Populations in Spiral and Elliptical Galaxies

NASA Astrophysics Data System (ADS)

Colbert, E.; Heckman, T.; Weaver, K.; Ptak, A.; Strickland, D.

2001-12-01

In the years of the Einstein and ASCA satellites, it was known that the total hard X-ray luminosity from non-AGN galaxies was fairly well correlated with the total blue luminosity. However, the origin of this hard component was not well understood. Some possibilities that were considered included X-ray binaries, extended upscattered far-infrared light via the inverse-Compton process, extended hot 107 K gas (especially in ellipitical galaxies), or even an active nucleus. Now, for the first time, we know from Chandra images that a significant amount of the total hard X-ray emission comes from individual X-ray point sources. We present here spatial and spectral analyses of Chandra data for X-ray point sources in a sample of ~40 galaxies, including both spiral galaxies (starbursts and non-starbursts) and elliptical galaxies. We shall discuss the relationship between the X-ray point source population and the properties of the host galaxies. We show that the slopes of the point-source X-ray luminosity functions are different for different host galaxy types and discuss possible reasons why. We also present detailed X-ray spectral analyses of several of the most luminous X-ray point sources (i.e., IXOs, a.k.a. ULXs), and discuss various scenarios for the origin of the X-ray point sources.

A hot X-ray filament associated with A3017 galaxy cluster

NASA Astrophysics Data System (ADS)

Parekh, V.; Durret, F.; Padmanabh, P.; Pandge, M. B.

2017-09-01

Recent simulations and observations have shown large-scale filaments in the cosmic web connecting nodes, with accreting materials (baryonic and dark matter) flowing through them. Current high-sensitivity observations also show that the propagation of shocks through filaments can heat them up and make filaments visible between two or more galaxy clusters or around massive clusters, based on optical and/or X-ray observations. We are reporting here the special case of the cluster A3017 associated with a hot filament. The temperature of the filament is 3.4^{-0.77}_{+1.30} keV and its length is ∼1 Mpc. We have analysed its archival Chandra data and report various properties. We also analysed GMRT 235/610 MHz radio data. Radio observations have revealed symmetric two-sided lobes that fill cavities in the A3017 cluster core region, associated with central active galactic nucleus. In the radio map, we also noticed a peculiar linear vertical radio structure in the X-ray filament region which might be associated with a cosmic filament shock. This radio structure could be a radio phoenix or old plasma where an old relativistic population is re-accelerated by shock propagation. Finally, we put an upper limit on the radio luminosity of the filament region.

XMM-Newton X-ray and HST weak gravitational lensing study of the extremely X-ray luminous galaxy cluster Cl J120958.9+495352 ( z = 0.902)

DOE PAGES

Tholken, Sophia; Schrabback, Tim; Reiprich, Thomas H.; ...

2018-03-05

Here, observations of relaxed, massive, and distant clusters can provide important tests of standard cosmological models, for example by using the gas mass fraction. To perform this test, the dynamical state of the cluster and its gas properties have to be investigated. X-ray analyses provide one of the best opportunities to access this information and to determine important properties such as temperature profiles, gas mass, and the total X-ray hydrostatic mass. For the last of these, weak gravitational lensing analyses are complementary independent probes that are essential in order to test whether X-ray masses could be biased.

XMM-Newton X-ray and HST weak gravitational lensing study of the extremely X-ray luminous galaxy cluster Cl J120958.9+495352 ( z = 0.902)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tholken, Sophia; Schrabback, Tim; Reiprich, Thomas H.

Here, observations of relaxed, massive, and distant clusters can provide important tests of standard cosmological models, for example by using the gas mass fraction. To perform this test, the dynamical state of the cluster and its gas properties have to be investigated. X-ray analyses provide one of the best opportunities to access this information and to determine important properties such as temperature profiles, gas mass, and the total X-ray hydrostatic mass. For the last of these, weak gravitational lensing analyses are complementary independent probes that are essential in order to test whether X-ray masses could be biased.

The solar atmosphere and the structure of active regions. [aircraft accidents, weather

NASA Technical Reports Server (NTRS)

Sturrock, P. A.

1975-01-01

Numerical analyses of solar activities are presented. The effect of these activities on aircraft and weather conditions was studied. Topics considered are: (1) solar flares; (2) solar X-rays; and (3) solar magnetic fields (charts are shown).

An epistemology on the nature of polymers.

PubMed

Laridjani, Mortéza; Leboucher, Pierre

2014-01-01

Liquids have neither a periodic structure nor the completely random character of gases therefore the detailed study of their x-ray scattering diagram encounters many difficulties. The idea of periodic regularity in molecules of liquid polymers has been an attractive proposition for the simple interpretation of liquid polymer x-ray diagrams. The categorisation of polymer substances as being between a crystal phase with a perfect order and an amorphous disordered state is an over simplification of the complex reality. For obtaining structural information, during the early stages of the application of x-ray diffraction, a near crystalline model of the molecular arrangements in liquids was utilised. However, the results from these investigations led to just an approximation of the crystalline state. Our studies have analysed the real image of Fourier space of liquid polymers, for the first time, using anomalous diffractometry. The findings show the precise atomic structure of liquid polymers when transformed, by cooling, to solid polymers. We demonstrate that there is an intermediate ordered structure, characterised by the real full image of Fourier space. This prominent state of matter, an intermediate ordered structure, is defined by a regular unit cell with a five-fold symmetry. These structural atomic studies contribute to a more detailed understanding of the properties of polymers than the traditional studies of the degree of crystallinity.

An Epistemology on the Nature of Polymers

PubMed Central

Laridjani, Mortéza; Leboucher, Pierre

2014-01-01

Liquids have neither a periodic structure nor the completely random character of gases therefore the detailed study of their x-ray scattering diagram encounters many difficulties. The idea of periodic regularity in molecules of liquid polymers has been an attractive proposition for the simple interpretation of liquid polymer x-ray diagrams. The categorisation of polymer substances as being between a crystal phase with a perfect order and an amorphous disordered state is an over simplification of the complex reality. For obtaining structural information, during the early stages of the application of x-ray diffraction, a near crystalline model of the molecular arrangements in liquids was utilised. However, the results from these investigations led to just an approximation of the crystalline state. Our studies have analysed the real image of Fourier space of liquid polymers, for the first time, using anomalous diffractometry. The findings show the precise atomic structure of liquid polymers when transformed, by cooling, to solid polymers. We demonstrate that there is an intermediate ordered structure, characterised by the real full image of Fourier space. This prominent state of matter, an intermediate ordered structure, is defined by a regular unit cell with a five-fold symmetry. These structural atomic studies contribute to a more detailed understanding of the properties of polymers than the traditional studies of the degree of crystallinity. PMID:25329440

Crystal structure, spectral property, antimicrobial activity and DFT calculation of N-(coumarin-3-yl)-N‧-(2-amino-5-phenyl-1,3,4-thiadiazol-2-yl) urea

NASA Astrophysics Data System (ADS)

Zhang, Hong-Song; Zhang, Kong-Yan; Chen, Li-Chuan; Li, Yao-Xin; Chai, Lan-Qin

2017-10-01

N-(coumarin-3-yl)-N‧-(2-amino-5-phenyl-1,3,4-thiadiazol-2-yl) urea was synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR, UV-Vis and emission spectroscopy, as well as by single-crystal X-ray diffraction. X-ray crystallographic analyses have indicated that the crystal structure consists of two dimethyl sulfoxide (DMSO) solvent molecules and the structural geometry of DMSO is a trigonal pyramid in shape. In the crystal structure, a self-assembling two-dimensional (2-D) layer supramolecular architecture is formed through intermolecular hydrogen bonds, Cdbnd O···π (thiadiazole ring) and π···π stacking interactions. The geometry of the compound has been optimized by the DFT method and the results are compared with the X-ray diffraction data. The electronic transitions and spectral features of the compound were carried out by using DFT/B3LYP method. In addition, the antimicrobial activity was also studied, and the highest occupied molecular orbital (HOMO), lowest unoccupied molecular orbital (LUMO), and HOMO-LUMO gap were also calculated.

X-ray computed tomography of wood-adhesive bondlines: Attenuation and phase-contrast effects

DOE PAGES

Paris, Jesse L.; Kamke, Frederick A.; Xiao, Xianghui

2015-07-29

Microscale X-ray computed tomography (XCT) is discussed as a technique for identifying 3D adhesive distribution in wood-adhesive bondlines. Visualization and material segmentation of the adhesives from the surrounding cellular structures require sufficient gray-scale contrast in the reconstructed XCT data. Commercial wood-adhesive polymers have similar chemical characteristics and density to wood cell wall polymers and therefore do not provide good XCT attenuation contrast in their native form. Here, three different adhesive types, namely phenol formaldehyde, polymeric diphenylmethane diisocyanate, and a hybrid polyvinyl acetate, are tagged with iodine such that they yield sufficient X-ray attenuation contrast. However, phase-contrast effects at material edgesmore » complicate image quality and segmentation in XCT data reconstructed with conventional filtered backprojection absorption contrast algorithms. A quantitative phase retrieval algorithm, which isolates and removes the phase-contrast effect, was demonstrated. The paper discusses and illustrates the balance between material X-ray attenuation and phase-contrast effects in all quantitative XCT analyses of wood-adhesive bondlines.« less

X-ray computed tomography of wood-adhesive bondlines: Attenuation and phase-contrast effects

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paris, Jesse L.; Kamke, Frederick A.; Xiao, Xianghui

Microscale X-ray computed tomography (XCT) is discussed as a technique for identifying 3D adhesive distribution in wood-adhesive bondlines. Visualization and material segmentation of the adhesives from the surrounding cellular structures require sufficient gray-scale contrast in the reconstructed XCT data. Commercial wood-adhesive polymers have similar chemical characteristics and density to wood cell wall polymers and therefore do not provide good XCT attenuation contrast in their native form. Here, three different adhesive types, namely phenol formaldehyde, polymeric diphenylmethane diisocyanate, and a hybrid polyvinyl acetate, are tagged with iodine such that they yield sufficient X-ray attenuation contrast. However, phase-contrast effects at material edgesmore » complicate image quality and segmentation in XCT data reconstructed with conventional filtered backprojection absorption contrast algorithms. A quantitative phase retrieval algorithm, which isolates and removes the phase-contrast effect, was demonstrated. The paper discusses and illustrates the balance between material X-ray attenuation and phase-contrast effects in all quantitative XCT analyses of wood-adhesive bondlines.« less

X-ray beamsplitter

DOEpatents

Ceglio, N.M.; Stearns, D.G.; Hawryluk, A.M.; Barbee, T.W. Jr.

1987-08-07

An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5--50 pairs of alternate Mo/Si layers with a period of 20--250 A. The support membrane is 10--200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window. 6 figs.

X-ray beamsplitter

DOEpatents

Ceglio, Natale M.; Stearns, Daniel S.; Hawryluk, Andrew M.; Barbee, Jr., Troy W.

1989-01-01

An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5-50 pairs of alternate Mo/Si layers with a period of 20-250 A. The support membrane is 10-200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window.

Syntheses, structures and properties of two new coordination polymers based on D-camphoric acid and 2-phenyl-4,6-diamino-1,3,5-triazine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lun, Huijie; Yang, Jinghe; Jin, Linyu

2015-05-15

By hydrothermal method, two new coordination polymers [Co(ca)(phdat)]{sub n} (1), [Ni(ca)(phdat).0.125H{sub 2}O]{sub n} (2) (H{sub 2}ca=D-camphoric acid, phdat=2-phenyl-4,6-diamino-1,3,5-triazine) have been achieved and structurally characterized by IR, elemental analyses, X-ray single-crystal diffraction and TGA. The X-ray single-crystal diffraction reveals that compounds 1 and 2 are isostructural, both of which exhibit two-dimensional layered network built up from paddle-wheel Co{sub 2}(CO{sub 2}){sub 4}/Ni{sub 2}(CO{sub 2}){sub 4} SBUs by ca{sup 2−} ligand. In the existence of π…π stacking interactions between triazine rings and phenyl rings, the 3D networks are constructed with the hanging phdat filled between the neighboring layers. Furthermore, compounds 1–2 exhibit antiferromagneticmore » behavior and compound 2 displays a good activity for methanol oxidation. - Graphical abstract: Two new coordination compounds 1–2 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses, magnetic and electrochemical measurement. - Highlights: • This paper reports two new coordination polymers based on D-camphoric acid. • Both the compounds feather two-dimensional layered networks built up from paddle-wheel SBUs. • The magnetism and electrochemical property are investigated.« less

Textural, Structural and Biological Evaluation of Hydroxyapatite Doped with Zinc at Low Concentrations

PubMed Central

Predoi, Daniela; Iconaru, Simona Liliana; Deniaud, Aurélien; Chevallet, Mireille; Michaud-Soret, Isabelle; Buton, Nicolas; Prodan, Alina Mihaela

2017-01-01

The present work was focused on the synthesis and characterization of hydroxyapatite doped with low concentrations of zinc (Zn:HAp) (0.01 < xZn < 0.05). The incorporation of low concentrations of Zn2+ ions in the hydroxyapatite (HAp) structure was achieved by co-precipitation method. The physico-chemical properties of the samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), zeta-potential, and DLS and N2-BET measurements. The results obtained by XRD and FTIR studies demonstrated that doping hydroxyapatite with low concentrations of zinc leads to the formation of a hexagonal structure with lattice parameters characteristic to hydroxyapatite. The XRD studies have also shown that the crystallite size and lattice parameters of the unit cell depend on the substitutions of Ca2+ with Zn2+ in the apatitic structure. Moreover, the FTIR analysis revealed that the water content increases with the increase of zinc concentration. Furthermore, the Energy Dispersive X-ray Analysis (EDAX) and XPS analyses showed that the elements Ca, P, O, and Zn were found in all the Zn:HAp samples suggesting that the synthesized materials were zinc doped hydroxyapatite, Ca10−xZnx(PO4)6(OH), with 0.01 ≤ xZn ≤ 0.05. Antimicrobial assays on Staphylococcus aureus and Escherichia coli bacterial strains and HepG2 cell viability assay were carried out. PMID:28772589

Electronic structure, optical and magnetic studies of PLD-grown (Mn, P)-doped ZnO nanocolumns at room temperature

NASA Astrophysics Data System (ADS)

Phan, The-Long; Ho, T. A.; Dang, N. T.; Nguyen, Manh Cuong; Dao, Van-Duong

2017-07-01

We prepared well-aligned Zn1-x Mn x O:yP nanocolumns (x  =  0-0.02, and y  =  0 and 1 mol%) on SiO2/Si(0 0 1) substrates by using pulsed laser deposition (PLD) and then investigated their electronic structure and optical and magnetic properties at room temperature. The analyses of x-ray photoelectron and x-ray absorption fine structure spectra revealed Mn2+ and/or P ions existing in nanocolumns, where Mn2+ ions are situated in the Zn2+ site of the ZnO-wurtzite structure. Although the incorporation of Mn2+ and/or P ions did not form secondary phases, as confirmed by x-ray and electron diffraction patterns, more lattice defects were created, and consequently changed the band-gap energy as well as the electron-phonon interactions in the nanocolumns. Magnetization versus magnetic-field measurements revealed that all the samples exhibited FM order. In particular, the (Mn, P) co-doping with x  =  0.02 and y  =  1 remarkably enhanced the magnetic moment up to 2.92 µ B/Mn. Based on the results obtained from analyzing the electronic structures, UV-Vis absorption and resonant Raman scattering spectra, and theoretical calculations, we believe that the enhancement of the FM order in (Mn, P)-doped ZnO nanocolumns is due to exchange interactions taking place between vacancy-mediated Mn2+ ions.

Screening and structural elucidation of the zwitterionic cocrystal o-picolinic acid with p-nitro aniline

NASA Astrophysics Data System (ADS)

Mekala, R.; Jagdish, P.; Mathammal, R.; Sangeetha, K.

2017-04-01

The cocrystal was screened by solvent drop grinding method and the crystals were grown by slow evaporation method at ambient conditions. The cocrystal formation of o-picolinic acid with p-nitro aniline was initially analysed by powder X-ray diffraction. Further the structural properties of the grown crystal were confirmed by the single X-ray diffraction which indicates that the cocrystal were connected by the strong N+sbnd H-⋯O hydrogen bond interaction. The cell parameters of the grown crystal were a = 14.2144(5) Å, b = 5.7558(2) Å, c = 16.0539(6) Å. The functional groups were identified using Fourier transform infrared and Raman spectral analysis. The excitation and emission state of the sample was analysed by the UV-Visible and Fluorescence studies. The red emission was observed from the Fluorescence studies. NMR studies revealed the chemical shift of the cocrystal. Thermal stability and its melting behaviour were studied by TGA and DSC analytical techniques. Electrical behaviour was studied using the dielectric studies. The intermolecular charge transfer within the molecule were analysed using HOMO- LUMO plots.

Optimizing use of the structural chemical analyser (variable pressure FESEM-EDX Raman spectroscopy) on micro-size complex historical paintings characterization.

PubMed

Guerra, I; Cardell, C

2015-10-01

The novel Structural Chemical Analyser (hyphenated Raman spectroscopy and scanning electron microscopy equipped with an X-ray detector) is gaining popularity since it allows 3-D morphological studies and elemental, molecular, structural and electronic analyses of a single complex micro-sized sample without transfer between instruments. However, its full potential remains unexploited in painting heritage where simultaneous identification of inorganic and organic materials in paintings is critically yet unresolved. Despite benefits and drawbacks shown in literature, new challenges have to be faced analysing multifaceted paint specimens. SEM-Structural Chemical Analyser systems differ since they are fabricated ad hoc by request. As configuration influences the procedure to optimize analyses, likewise analytical protocols have to be designed ad hoc. This paper deals with the optimization of the analytical procedure of a Variable Pressure Field Emission scanning electron microscopy equipped with an X-ray detector Raman spectroscopy system to analyse historical paint samples. We address essential parameters, technical challenges and limitations raised from analysing paint stratigraphies, archaeological samples and loose pigments. We show that accurate data interpretation requires comprehensive knowledge of factors affecting Raman spectra. We tackled: (i) the in-FESEM-Raman spectroscopy analytical sequence, (ii) correlations between FESEM and Structural Chemical Analyser/laser analytical position, (iii) Raman signal intensity under different VP-FESEM vacuum modes, (iv) carbon deposition on samples under FESEM low-vacuum mode, (v) crystal nature and morphology, (vi) depth of focus and (vii) surface-enhanced Raman scattering effect. We recommend careful planning of analysis strategies prior to research which, although time consuming, guarantees reliable results. The ultimate goal of this paper is to help to guide future users of a FESEM-Structural Chemical Analyser system in order to increase applications. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Complete titanium substitution by boron in a tetragonal prism: exploring the complex boride series Ti(3-x)Ru(5-y)Ir(y)B(2+x) (0 ≤ x ≤ 1 and 1 < y < 3) by experiment and theory.

PubMed

Fokwa, Boniface P T; Hermus, Martin

2011-04-18

Polycrystalline samples and single crystals of four members of the new complex boride series Ti(3-x)Ru(5-y)Ir(y)B(2+x) (0 ≤ x ≤ 1 and 1 < y < 3) were synthesized by arc-melting the elements in a water-cooled copper crucible under an argon atmosphere. The new silvery phases were structurally characterized by powder and single-crystal X-ray diffraction as well as energy- and wavelength-dispersive X-ray spectroscopy analyses. They crystallize with the tetragonal Ti(3)Co(5)B(2) structure type in space group P4/mbm (No. 127). Tetragonal prisms of Ru/Ir atoms are filled with titanium in the boron-poorest phase (Ti(3)Ru(2.9)Ir(2.1)B(2)). Gradual substitution of titanium by boron then results in the successive filling of this site by a Ti/B mixture en route to the complete boron occupation, leading to the boron-richest phase (Ti(2)Ru(2.8)Ir(2.2)B(3)). Furthermore, both ruthenium and iridium share two sites in these structures, but a clear Ru/Ir site preference is found. First-principles density functional theory calculations (Vienna ab initio simulation package) on appropriate structural models (using a supercell approach) have provided more evidence on the stability of the boron-richest and -poorest phases, and the calculated lattice parameters corroborate very well with the experimentally found ones. Linear muffin-tin orbital atomic sphere approximation calculations further supported these findings through crystal orbital Hamilton population bonding analyses, which also show that the Ru/Ir-B and Ru/Ir-Ti heteroatomic interactions are mainly responsible for the structural stability of these compounds. Furthermore, some stable and unstable phases of this complex series could be predicted using the rigid-band model. According to the density of states analyses, all phases should be metallic conductors, as was expected from these metal-rich borides.

Comparative Analysis of Microbial Communities in Iron-Dominated Flocculent Mats in Deep-Sea Hydrothermal Environments.

PubMed

Makita, Hiroko; Kikuchi, Sakiko; Mitsunobu, Satoshi; Takaki, Yoshihiro; Yamanaka, Toshiro; Toki, Tomohiro; Noguchi, Takuroh; Nakamura, Kentaro; Abe, Mariko; Hirai, Miho; Yamamoto, Masahiro; Uematsu, Katsuyuki; Miyazaki, Junichi; Nunoura, Takuro; Takahashi, Yoshio; Takai, Ken

2016-10-01

It has been suggested that iron is one of the most important energy sources for photosynthesis-independent microbial ecosystems in the ocean crust. Iron-metabolizing chemolithoautotrophs play a key role as primary producers, but little is known about their distribution and diversity and their ecological role as submarine iron-metabolizing chemolithotrophs, particularly the iron oxidizers. In this study, we investigated the microbial communities in several iron-dominated flocculent mats found in deep-sea hydrothermal fields in the Mariana Volcanic Arc and Trough and the Okinawa Trough by culture-independent molecular techniques and X-ray mineralogical analyses. The abundance and composition of the 16S rRNA gene phylotypes demonstrated the ubiquity of zetaproteobacterial phylotypes in iron-dominated mat communities affected by hydrothermal fluid input. Electron microscopy with energy-dispersive X-ray microanalysis and X-ray absorption fine structure (XAFS) analysis revealed the chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species and the potential contribution of Zetaproteobacteria to the in situ generation. These results suggest that putative iron-oxidizing chemolithoautotrophs play a significant ecological role in producing iron-dominated flocculent mats and that they are important for iron and carbon cycles in deep-sea low-temperature hydrothermal environments. We report novel aspects of microbiology from iron-dominated flocculent mats in various deep-sea environments. In this study, we examined the relationship between Zetaproteobacteria and iron oxides across several hydrothermally influenced sites in the deep sea. We analyzed iron-dominated mats using culture-independent molecular techniques and X-ray mineralogical analyses. The scanning electron microscopy-energy-dispersive X-ray spectroscopy SEM-EDS analysis and X-ray absorption fine structure (XAFS) analysis revealed chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species as well as the potential contribution of the zetaproteobacterial population to the in situ production. These key findings provide important information for understanding the mechanisms of both geomicrobiological iron cycling and the formation of iron-dominated mats in deep-sea hydrothermal fields. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula

NASA Technical Reports Server (NTRS)

Weisskopf, Martin C.; Hester, J. Jeff; Tennant, Allyn F.; Elsner, Ronald F.; Schulz, Norbert S.; Marshall, Herman L.; Karovska, Margarita; Nichols, Joy S.; Swartz, Douglas A.; Kolodziejczak, Jeffery J.

2000-01-01

The Chandra X-Ray Observatory observed the Crab Nebula and pulsar during orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) readout by the Advanced Charge Coupled Devices (CCD) Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray inner ring within the X-ray torus, the suggestion of a hollow-tube structure for the torus, and X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the nebula.

Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula.

PubMed

Weisskopf; Hester; Tennant; Elsner; Schulz; Marshall; Karovska; Nichols; Swartz; Kolodziejczak; O'Dell

2000-06-20

The Chandra X-Ray Observatory observed the Crab Nebula and pulsar during orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) readout by the Advanced CCD Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray inner ring within the X-ray torus, the suggestion of a hollow-tube structure for the torus, and X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the nebula.

Research in Solar Physics: Analysis of Skylab/ATM S-056 X-Ray Data

NASA Technical Reports Server (NTRS)

Henze, W., Jr.

1977-01-01

Data obtained by the X-ray event analyzer are described as well as methods used for film calibration. Topics discussed include analyses of the 15 June 1973 flare, oscillations in the solar soft X-ray flux, and deconvolution of X-ray images of the 5 September 1973 flare.

Synthesis, spectral and antifungal analysis of diaryldithiophosphates of mono- and dibutyltin(IV): x-ray structure of [{(3,5-CH3)2C6H3O)2PS2}2Sn(nBu)2].

PubMed

Syed, Atiya; Khajuria, Ruchi; Kumar, Sandeep; Jassal, Amanpreet Kaur; Hundal, Maninder S; Pandey, Sushil K

2014-01-01

Diaryldithiophosphate complexes of mono- and dibutyltin(IV) corresponding to [(ArO)(2)PS(2)(n)Sn(nBu)xCl(4-x-n)] (Ar = o-CH(3)C(6)H(4), m-CH(3)C(6)H(4), p-CH(3)C(6)H(4), 4-Cl-3-CH(3)C(6)H(3), (3,5-CH(3))(2)C(6)H(3); n = 1, 2 for x = 1 and n = 2 for x = 2) were successfully isolated and characterized by elemental analyses, IR, multinuclear NMR ((1)H, (13)C, (31)P and (119)Sn) spectroscopy and X-ray analysis. The thermal properties of the complex [(3,5-CH(3))(2)C(6)H(3)O(2)PS(2)](2)Sn(nBu)(2) (12) have been examined by combined DTA/ DTG thermal analyses. Single crystal X-ray analysis of [(3,5-CH(3))(2)C(6)H(3)O(2)PS(2)](2)S(n)(nBu)(2) (12) revealed that two diaryldithiophosphate ions are coordinated to tin atom in an anisobidentate fashion through the sulfur atoms of each dithiophosphate moiety leading to distorted skew-trapezoidal bipyramidal geometry. The antifungal activity depicts that these complexes are active against fungus Penicillium chrysogenium.

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

A glimpse of structural biology through X-ray crystallography.

PubMed

Shi, Yigong

2014-11-20

Since determination of the myoglobin structure in 1957, X-ray crystallography, as the anchoring tool of structural biology, has played an instrumental role in deciphering the secrets of life. Knowledge gained through X-ray crystallography has fundamentally advanced our views on cellular processes and greatly facilitated development of modern medicine. In this brief narrative, I describe my personal understanding of the evolution of structural biology through X-ray crystallography-using as examples mechanistic understanding of protein kinases and integral membrane proteins-and comment on the impact of technological development and outlook of X-ray crystallography.

Background radiation in inelastic X-ray scattering and X-ray emission spectroscopy. A study for Johann-type spectrometers

NASA Astrophysics Data System (ADS)

Paredes Mellone, O. A.; Bianco, L. M.; Ceppi, S. A.; Goncalves Honnicke, M.; Stutz, G. E.

2018-06-01

A study of the background radiation in inelastic X-ray scattering (IXS) and X-ray emission spectroscopy (XES) based on an analytical model is presented. The calculation model considers spurious radiation originated from elastic and inelastic scattering processes along the beam paths of a Johann-type spectrometer. The dependence of the background radiation intensity on the medium of the beam paths (air and helium), analysed energy and radius of the Rowland circle was studied. The present study shows that both for IXS and XES experiments the background radiation is dominated by spurious radiation owing to scattering processes along the sample-analyser beam path. For IXS experiments the spectral distribution of the main component of the background radiation shows a weak linear dependence on the energy for the most cases. In the case of XES, a strong non-linear behaviour of the background radiation intensity was predicted for energy analysis very close to the backdiffraction condition, with a rapid increase in intensity as the analyser Bragg angle approaches π / 2. The contribution of the analyser-detector beam path is significantly weaker and resembles the spectral distribution of the measured spectra. Present results show that for usual experimental conditions no appreciable structures are introduced by the background radiation into the measured spectra, both in IXS and XES experiments. The usefulness of properly calculating the background profile is demonstrated in a background subtraction procedure for a real experimental situation. The calculation model was able to simulate with high accuracy the energy dependence of the background radiation intensity measured in a particular XES experiment with air beam paths.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

NASA Astrophysics Data System (ADS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

A Novel Coordination Polymer Based on Trinuclear Cobalt Building Blocks Cluster: Synthesis, Crystal Structure, and Properties

NASA Astrophysics Data System (ADS)

Lu, J. F.; Tang, Z. H.; Shi, J.; Ge, H. G.; Jiang, M.; Song, J.; Jin, L. X.

2017-12-01

The title compound {[Co3(μ3-OH)(μ2-H2O)2(H2O)5(BTC)2] · 6H2O} n (H3BTC is a 1,3,5-benzenetricarboxylic acid) was prepared and characterized by single crystal and powder X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric and elemental analyses. The single crystal X-ray diffraction reveals that the title compound consists of 1D infinite zigzag chains which were constructed by trinuclear cobalt cluster and BTC3- ligand. Neighbouring above-mentioned 1D infinite zigzag chains are further linked by intermolecular hydrogen bonding to form a 3D supermolecular structure. In addition, the luminescent properties of the title compound were investigated.

Interfacial mixing in as-deposited Si/Ni/Si layers analyzed by x-ray and polarized neutron reflectometry

NASA Astrophysics Data System (ADS)

Bhattacharya, Debarati; Basu, Saibal; Singh, Surendra; Roy, Sumalay; Dev, Bhupendra Nath

2012-12-01

Interdiffusion occurring across the interfaces in a Si/Ni/Si layered system during deposition at room temperature was probed using x-ray reflectivity (XRR) and polarized neutron reflectivity (PNR). Exploiting the complementarity of these techniques, both structural and magnetic characterization with nanometer depth resolution could be achieved. Suitable model fitting of the reflectivity profiles identified the formation of Ni-Si mixed alloy layers at the Si/Ni and Ni/Si interfaces. The physical parameters of the layered structure, including quantitative assessment of the stoichiometry of interfacial alloys, were obtained from the analyses of XRR and PNR patterns. In addition, PNR provided magnetic moment density profile as a function of depth in the stratified medium.

X-ray emission from high temperature plasmas

NASA Technical Reports Server (NTRS)

Harries, W. L.

1974-01-01

X-rays from a 25-hJ plasma focus apparatus were observed with pinhole cameras. The cameras consist of 0.4 mm diameter pinholes in 2 cm thick lead housing enclosing an X-ray intensifying screen at the image plane. Pictures recorded through thin aluminum foils or plastic sheets for X-ray energies sub gamma smaller than 15 keV show distributed X-ray emissions from the focussed plasma and from the anode surface. However, when thick absorbers are used, radial filamentary structure in the X-ray emission from the anode surface is revealed. Occasionally larger structures are observed in addition to the filaments. Possible mechanisms for the filamentary structure are discussed.

Controlled cobalt doping in the spinel structure of magnetosome magnetite: new evidences from element- and site-specific X-ray magnetic circular dichroism analyses

PubMed Central

Menguy, Nicolas; Arrio, Marie-Anne; Sainctavit, Philippe; Juhin, Amélie; Wang, Yinzhao; Chen, Haitao; Bunau, Oana; Otero, Edwige; Ohresser, Philippe; Pan, Yongxin

2016-01-01

The biomineralization of magnetite nanocrystals (called magnetosomes) by magnetotactic bacteria (MTB) has attracted intense interest in biology, geology and materials science due to the precise morphology of the particles, the chain-like assembly and their unique magnetic properties. Great efforts have been recently made in producing transition metal-doped magnetosomes with modified magnetic properties for a range of applications. Despite some successful outcomes, the coordination chemistry and magnetism of such metal-doped magnetosomes still remain largely unknown. Here, we present new evidences from X-ray magnetic circular dichroism (XMCD) for element- and site-specific magnetic analyses that cobalt is incorporated in the spinel structure of the magnetosomes within Magnetospirillum magneticum AMB-1 through the replacement of Fe2+ ions by Co2+ ions in octahedral (Oh) sites of magnetite. Both XMCD at Fe and Co L2,3 edges, and energy-dispersive X-ray spectroscopy on transmission electron microscopy analyses reveal a heterogeneous distribution of cobalt occurring either in different particles or inside individual particles. Compared with non-doped one, cobalt-doped magnetosome sample has lower Verwey transition temperature and larger magnetic coercivity, related to the amount of doped cobalt. This study also demonstrates that the addition of trace cobalt in the growth medium can significantly improve both the cell growth and the magnetosome formation within M. magneticum AMB-1. Together with the cobalt occupancy within the spinel structure of magnetosomes, this study indicates that MTB may provide a promising biomimetic system for producing chains of metal-doped single-domain magnetite with an appropriate tuning of the magnetic properties for technological and biomedical applications. PMID:27512138

Controlled cobalt doping in the spinel structure of magnetosome magnetite: new evidences from element- and site-specific X-ray magnetic circular dichroism analyses.

PubMed

Li, Jinhua; Menguy, Nicolas; Arrio, Marie-Anne; Sainctavit, Philippe; Juhin, Amélie; Wang, Yinzhao; Chen, Haitao; Bunau, Oana; Otero, Edwige; Ohresser, Philippe; Pan, Yongxin

2016-08-01

The biomineralization of magnetite nanocrystals (called magnetosomes) by magnetotactic bacteria (MTB) has attracted intense interest in biology, geology and materials science due to the precise morphology of the particles, the chain-like assembly and their unique magnetic properties. Great efforts have been recently made in producing transition metal-doped magnetosomes with modified magnetic properties for a range of applications. Despite some successful outcomes, the coordination chemistry and magnetism of such metal-doped magnetosomes still remain largely unknown. Here, we present new evidences from X-ray magnetic circular dichroism (XMCD) for element- and site-specific magnetic analyses that cobalt is incorporated in the spinel structure of the magnetosomes within Magnetospirillum magneticum AMB-1 through the replacement of Fe(2+) ions by Co(2+) ions in octahedral (Oh) sites of magnetite. Both XMCD at Fe and Co L2,3 edges, and energy-dispersive X-ray spectroscopy on transmission electron microscopy analyses reveal a heterogeneous distribution of cobalt occurring either in different particles or inside individual particles. Compared with non-doped one, cobalt-doped magnetosome sample has lower Verwey transition temperature and larger magnetic coercivity, related to the amount of doped cobalt. This study also demonstrates that the addition of trace cobalt in the growth medium can significantly improve both the cell growth and the magnetosome formation within M. magneticum AMB-1. Together with the cobalt occupancy within the spinel structure of magnetosomes, this study indicates that MTB may provide a promising biomimetic system for producing chains of metal-doped single-domain magnetite with an appropriate tuning of the magnetic properties for technological and biomedical applications. © 2016 The Author(s).

Growth, structural, optical, thermal and mechanical properties of ammonium pentaborate single crystal.

PubMed

Balakrishnan, T; Bhagavannarayana, G; Ramamurthi, K

2008-11-15

Nonlinear optical single crystals of ammonium pentaborate (APB) were grown by the slow cooling method from aqueous solution. Grown crystal was characterized by powder X-ray diffraction (PXRD) and FT-IR spectral analysis. Perfection of the grown crystal was evaluated by high-resolution X-ray diffractometry (HRXRD). The effect of nylon threading on the perfection of the grown bigger crystal was also studied by HRXRD. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties were investigated by TG-DTA and DSC analyses. Its mechanical hardness was estimated by Vickers microhardness tester.

Surface and interface analysis of poly-hydroxyethylmethacrylate-coated anodic aluminium oxide membranes

NASA Astrophysics Data System (ADS)

Ali, Nurshahidah; Duan, Xiaofei; Jiang, Zhong-Tao; Goh, Bee Min; Lamb, Robert; Tadich, Anton; Poinern, Gérrard Eddy Jai; Fawcett, Derek; Chapman, Peter; Singh, Pritam

2014-01-01

The surface and interface of poly (2-hydroxyethylmethacrylate) (PHEMA) and anodic aluminium oxide (AAO) membranes were comprehensively investigated using Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy. It was found that 1s→π* (Cdbnd O) and 1s→σ* (Csbnd O) transitions were dominant on the surface of both bulk PHEMA polymer and PHEMA-surface coated AAO (AAO-PHEMA) composite. Findings from NEXAFS, Fourier-Transform Infrared (FTIR) and X-ray Photoelectron Spectroscopy (XPS) analyses suggest the possibility of chemical interaction between carbon from the ester group of polymer and AAO membrane.

Self-standing crystalline TiO2 nanotubes/CNTs heterojunction membrane: synthesis and characterization.

PubMed

Hesabi, Zohreh R; Allam, Nageh K; Dahmen, Klaus; Garmestani, Hamid; A El-Sayed, Mostafa

2011-04-01

In the present study, we report for the first time synthesis of TiO(2) nanotubes/CNTs heterojunction membrane. Chemical vapor deposition (CVD) of CNTs at 650 °C in a mixture of H(2)/He atmosphere led to in situ detachment of the anodically fabricated TiO(2) nanotube layers from the Ti substrate underneath. Morphological and structural evolution of TiO(2) nanotubes after CNTs deposition were investigated by field- emission scanning electron microscopy (FESEM), glancing angle X-ray diffraction (GAXRD), and X-ray photoelectron spectroscopy (XPS) analyses. © 2011 American Chemical Society

Effect of Molybdenum Incorporation on the Structure and Magnetic Properties of Cobalt Ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Orozco, C.; Melendez, A.; Manadhar, S.

Here, we report on the effect of molybdenum (Mo) incorporation on the crystal structure, surface morphology, Mo chemical valence state, and magnetic properties of cobalt ferrite (CoFe 2O 4, referred to CFO). Molybdenum incorporated cobalt ferrite (CoFe 2–xMo xO 4, referred to CFMO) ceramics were prepared by the conventional solid-state reaction method by varying the Mo concentration in the range of x = 0.0–0.3. X-ray diffraction studies indicate that the CFMO materials crystallize in inverse spinel cubic phase. Molybdenum incorporation induced lattice parameter increase from 8.322 to 8.343 Å coupled with a significant increase in density from 5.4 to 5.7more » g/cm 3 was evident in structural analyses. Scanning electron microscopy imaging analyses indicate that the Mo incorporation induces agglomeration of particles leading to larger particle size with increasing x(Mo) values. Detailed X-ray photoelectron spectroscopic (XPS) analyses indicate the increasing Mo content with increasing x from 0.0 to 0.3. XPS confirms that the chemistry of Mo is complex in these CFMO compounds; Mo ions exist in the lower oxidation state (Mo 4+) for higher x while in a mixed chemical valence state (Mo 4+, Mo 5+, Mo 6+) for lower x values. From the temperature-dependent magnetization, the samples show ferrimagnetic behavior including the pristine CFO. From the isothermal magnetization measurements, we find almost 2-fold decrease in coercive field ( H c) from 2143 to 1145 Oe with the increase in Mo doping up to 30%. This doping-dependent H c is consistently observed at all the temperatures measured (4, 100, 200, and 300 K). Furthermore, the saturation magnetization estimated at 4 K and at 1.5 T (from M–H loops) goes through a peak at 92 emu/g (at 15% Mo doping) from 81 emu/g (pristine CFO), and starts decreasing to 79 emu/g (at 30% Mo doping). The results demonstrate that the crystal structure, microstructure, and magnetic properties can be tuned by controlling the Mo-content in the CFMO materials.« less

Effect of Molybdenum Incorporation on the Structure and Magnetic Properties of Cobalt Ferrite

DOE PAGES

Orozco, C.; Melendez, A.; Manadhar, S.; ...

2017-09-26

Here, we report on the effect of molybdenum (Mo) incorporation on the crystal structure, surface morphology, Mo chemical valence state, and magnetic properties of cobalt ferrite (CoFe 2O 4, referred to CFO). Molybdenum incorporated cobalt ferrite (CoFe 2–xMo xO 4, referred to CFMO) ceramics were prepared by the conventional solid-state reaction method by varying the Mo concentration in the range of x = 0.0–0.3. X-ray diffraction studies indicate that the CFMO materials crystallize in inverse spinel cubic phase. Molybdenum incorporation induced lattice parameter increase from 8.322 to 8.343 Å coupled with a significant increase in density from 5.4 to 5.7more » g/cm 3 was evident in structural analyses. Scanning electron microscopy imaging analyses indicate that the Mo incorporation induces agglomeration of particles leading to larger particle size with increasing x(Mo) values. Detailed X-ray photoelectron spectroscopic (XPS) analyses indicate the increasing Mo content with increasing x from 0.0 to 0.3. XPS confirms that the chemistry of Mo is complex in these CFMO compounds; Mo ions exist in the lower oxidation state (Mo 4+) for higher x while in a mixed chemical valence state (Mo 4+, Mo 5+, Mo 6+) for lower x values. From the temperature-dependent magnetization, the samples show ferrimagnetic behavior including the pristine CFO. From the isothermal magnetization measurements, we find almost 2-fold decrease in coercive field ( H c) from 2143 to 1145 Oe with the increase in Mo doping up to 30%. This doping-dependent H c is consistently observed at all the temperatures measured (4, 100, 200, and 300 K). Furthermore, the saturation magnetization estimated at 4 K and at 1.5 T (from M–H loops) goes through a peak at 92 emu/g (at 15% Mo doping) from 81 emu/g (pristine CFO), and starts decreasing to 79 emu/g (at 30% Mo doping). The results demonstrate that the crystal structure, microstructure, and magnetic properties can be tuned by controlling the Mo-content in the CFMO materials.« less

A top-down approach to crystal engineering of a racemic Δ2-isoxazoline.

PubMed

Lombardo, Giuseppe M; Rescifina, Antonio; Chiacchio, Ugo; Bacchi, Alessia; Punzo, Francesco

2014-02-01

The crystal structure of racemic dimethyl (4RS,5RS)-3-(4-nitrophenyl)-4,5-dihydroisoxazole-4,5-dicarboxylate, C13H12N2O7, has been determined by single-crystal X-ray diffraction. By analysing the degree of growth of the morphologically important crystal faces, a ranking of the most relevant non-covalent interactions determining the crystal structure can be inferred. The morphological information is considered with an approach opposite to the conventional one: instead of searching inside the structure for the potential key interactions and using them to calculate the crystal habit, the observed crystal morphology is used to define the preferential lines of growth of the crystal, and then this information is interpreted by means of density functional theory (DFT) calculations. Comparison with the X-ray structure confirms the validity of the strategy, thus suggesting this top-down approach to be a useful tool for crystal engineering.

Structural correlation of the chalcogenide Ge40Se60 glass

NASA Astrophysics Data System (ADS)

Moharram, A. H.

2017-01-01

Binary Ge40Se60 glass was prepared using the melt-quench technique. The total structure factors, S( K), are obtained using the X-ray diffraction in the wave vector interval 0.28 ≤ K ≤ 6.5 Å-1. The appearance of the first sharp diffraction peak (FSDP) in the structure factor indicates the presence of the intermediate range order. Radial distribution functions, RDF( r), have been obtained using either the conventional (Fourier) transformation or the Monte Carlo simulation of the experimental X-ray data. The short range order parameters deduced from the Monte Carlo total correlation, T( r), functions are better than those obtained from the conventional (Fourier) T( r) data. Gaussian analyses of the total correlation function show that Ge2(Se1/2)6 molecular units are the basic structural units for the investigated Ge40Se60 glass.

Hard X-Ray Emission from Partially Occulted Solar Flares: RHESSI Observations in Two Solar Cycles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Effenberger, Frederic; Costa, Fatima Rubio da; Petrosian, Vahé

2017-02-01

Flares close to the solar limb, where the footpoints are occulted, can reveal the spectrum and structure of the coronal looptop source in X-rays. We aim at studying the properties of the corresponding energetic electrons near their acceleration site, without footpoint contamination. To this end, a statistical study of partially occulted flares observed with Reuven Ramaty High-Energy Solar Spectroscopic Imager is presented here, covering a large part of solar cycles 23 and 24. We perform detailed spectra, imaging, and light curve analyses for 116 flares and include contextual observations from SDO and STEREO when available, providing further insights into flaremore » emission that were previously not accessible. We find that most spectra are fitted well with a thermal component plus a broken power-law, non-thermal component. A thin-target kappa distribution model gives satisfactory fits after the addition of a thermal component. X-ray imaging reveals small spatial separation between the thermal and non-thermal components, except for a few flares with a richer coronal source structure. A comprehensive light curve analysis shows a very good correlation between the derivative of the soft X-ray flux (from GOES ) and the hard X-rays for a substantial number of flares, indicative of the Neupert effect. The results confirm that non-thermal particles are accelerated in the corona and estimated timescales support the validity of a thin-target scenario with similar magnitudes of thermal and non-thermal energy fluxes.« less

Local geometric and electronic structures and origin of magnetism in Co-doped BaTiO3 multiferroics

NASA Astrophysics Data System (ADS)

Phan, The-Long; Thang, P. D.; Ho, T. A.; Manh, T. V.; Thanh, Tran Dang; Lam, V. D.; Dang, N. T.; Yu, S. C.

2015-05-01

We have prepared polycrystalline samples BaTi1-xCoxO3 (x = 0-0.1) by solid-state reaction. X-ray diffraction and Raman-scattering studies reveal the phase separation in crystal structure as changing Co-doping content (x). The samples with x = 0-0.01 are single phase in a tetragonal structure. At higher doping contents (x > 0.01), there is the formation and development of a secondary hexagonal phase. Magnetization measurements at room temperature indicate a coexistence of paramagnetic and weak-ferromagnetic behaviors in BaTi1-xCoxO3 samples with x > 0, while pure BaTiO3 is diamagnetic. Both these properties increase with increasing x. Analyses of X-ray absorption spectra recorded from BaTi1-xCoxO3 for the Co and Ti K-edges indicate the presence of Co2+ and Co3+ ions. They locate in the Ti4+ site of the tetragonal and hexagonal BaTiO3 structures. Particularly, there is a shift of oxidation state from Co2+ to Co3+ when Co-doping content increases. We believe that the paramagnetic nature in BaTi1-xCoxO3 samples is due to isolated Co2+ and Co3+ centers. The addition of Co3+ ions enhances the paramagnetic behavior. Meanwhile, the origin of ferromagnetism is due to lattice defects, which is less influenced by the changes caused by the variation in concentration of Co2+ and Co3+ ions.

X-ray absorption spectroscopy and X-ray photoelectron spectroscopy studies of CaSO 4:Dy thermoluminescent phosphors

NASA Astrophysics Data System (ADS)

Bakshi, A. K.; Jha, S. N.; Olivi, L.; Phase, D. M.; Kher, R. K.; Bhattacharyya, D.

2007-11-01

Extended X-ray absorption fine structure (EXAFS) measurements have been carried out on CaSO4:Dy phosphor samples at the Dy L3 edge with synchrotron radiation. Measurements were carried out on a set of samples which were subjected to post-preparation annealing at different temperatures and for different cycles. The EXAFS data have been analysed to find the Dy-S and Dy-O bond lengths in the neighbourhood of the Dy atoms in a CaSO4 matrix. The observations from EXAFS measurements were verified with XANES and XPS techniques. On the basis of these measurements, efforts were made to explain the loss of thermoluminescence sensitivity of CaSO4:Dy phosphors after repeated cycles of annealing at 400 °C in air for 1 h.

Method and apparatus for molecular imaging using x-rays at resonance wavelengths

DOEpatents

Chapline, G.F. Jr.

Holographic x-ray images are produced representing the molecular structure of a microscopic object, such as a living cell, by directing a beam of coherent x-rays upon the object to produce scattering of the x-rays by the object, producing interference on a recording medium between the scattered x-rays from the object and unscattered coherent x-rays and thereby producing holograms on the recording surface, and establishing the wavelength of the coherent x-rays to correspond with a molecular resonance of a constituent of such object and thereby greatly improving the contrast, sensitivity and resolution of the holograms as representations of molecular structures involving such constituent. For example, the coherent x-rays may be adjusted to the molecular resonant absorption line of nitrogen at about 401.3 eV to produce holographic images featuring molecular structures involving nitrogen.

Direct detection of x-rays for protein crystallography employing a thick, large area CCD

DOEpatents

Atac, Muzaffer; McKay, Timothy

1999-01-01

An apparatus and method for directly determining the crystalline structure of a protein crystal. The crystal is irradiated by a finely collimated x-ray beam. The interaction of the x-ray beam with the crystal produces scattered x-rays. These scattered x-rays are detected by means of a large area, thick CCD which is capable of measuring a significant number of scattered x-rays which impact its surface. The CCD is capable of detecting the position of impact of the scattered x-ray on the surface of the CCD and the quantity of scattered x-rays which impact the same cell or pixel. This data is then processed in real-time and the processed data is outputted to produce a image of the structure of the crystal. If this crystal is a protein the molecular structure of the protein can be determined from the data received.

Method and apparatus for molecular imaging using X-rays at resonance wavelengths

DOEpatents

Chapline, Jr., George F.

1985-01-01

Holographic X-ray images are produced representing the molecular structure of a microscopic object, such as a living cell, by directing a beam of coherent X-rays upon the object to produce scattering of the X-rays by the object, producing interference on a recording medium between the scattered X-rays from the object and unscattered coherent X-rays and thereby producing holograms on the recording surface, and establishing the wavelength of the coherent X-rays to correspond with a molecular resonance of a constituent of such object and thereby greatly improving the contrast, sensitivity and resolution of the holograms as representations of molecular structures involving such constituent. For example, the coherent X-rays may be adjusted to the molecular resonant absorption line of nitrogen at about 401.3 eV to produce holographic images featuring molecular structures involving nitrogen.

Local structure in LaMnO3 and CaMnO3 perovskites: A quantitative structural refinement of Mn K -edge XANES data

NASA Astrophysics Data System (ADS)

Monesi, C.; Meneghini, C.; Bardelli, F.; Benfatto, M.; Mobilio, S.; Manju, U.; Sarma, D. D.

2005-11-01

Hole-doped perovskites such as La1-xCaxMnO3 present special magnetic and magnetotransport properties, and it is commonly accepted that the local atomic structure around Mn ions plays a crucial role in determining these peculiar features. Therefore experimental techniques directly probing the local atomic structure, like x-ray absorption spectroscopy (XAS), have been widely exploited to deeply understand the physics of these compounds. Quantitative XAS analysis usually concerns the extended region [extended x-ray absorption fine structure (EXAFS)] of the absorption spectra. The near-edge region [x-ray absorption near-edge spectroscopy (XANES)] of XAS spectra can provide detailed complementary information on the electronic structure and local atomic topology around the absorber. However, the complexity of the XANES analysis usually prevents a quantitative understanding of the data. This work exploits the recently developed MXAN code to achieve a quantitative structural refinement of the Mn K -edge XANES of LaMnO3 and CaMnO3 compounds; they are the end compounds of the doped manganite series LaxCa1-xMnO3 . The results derived from the EXAFS and XANES analyses are in good agreement, demonstrating that a quantitative picture of the local structure can be obtained from XANES in these crystalline compounds. Moreover, the quantitative XANES analysis provides topological information not directly achievable from EXAFS data analysis. This work demonstrates that combining the analysis of extended and near-edge regions of Mn K -edge XAS spectra could provide a complete and accurate description of Mn local atomic environment in these compounds.

Studies on synthesis, growth, structural, thermal, linear and nonlinear optical properties of organic picolinium maleate single crystals.

PubMed

Pandi, P; Peramaiyan, G; Sudhahar, S; Chakkaravarthi, G; Mohan Kumar, R; Bhagavannarayana, G; Jayavel, R

2012-12-01

Picolinium maleate (PM), an organic material has been synthesised and single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal X-ray diffraction analysis. PM crystal belongs to the monoclinic crystallographic system with space group P2(1)/c. The crystalline perfection of the grown crystals was analyzed by high-resolution X-ray diffraction rocking curve measurements. The presence of functional groups in PM was identified by FTIR and FT-NMR spectral analyses. Thermal behaviour and stability of picolinium maleate were studied by TGA/DTA analyses. UV-Vis spectral studies reveal that PM crystals are transparent in the wavelength region 327-1100 nm. The laser damage threshold value of PM crystal was found to be 4.3 GW/cm(2) using Nd:YAG laser. The Kurtz and Perry powder second harmonic generation technique confirms the nonlinear optical property of the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Design and synthesis of two luminescent Zn(II)-based coordination polymers with different structures regulated by different solvent system

NASA Astrophysics Data System (ADS)

Wu, Wei-Ping; Wen, Gui-Lin; Liao, Yi; Wang, Jun; Lu, Lu; Wu, Yu; Xie, Bin

2016-08-01

Two new coordination polymers (CPs) [Zn(HL)(H2O)]n (1) and [Zn3(L)2(H2O)2]n·(H2O)n (2), based on a multifunctional ligand combined carboxylate groups and a nitrogen donor group 5-(6-carboxypyridin-2-yl)isophthalic acid (H3L), have been synthesized under different solvent media and fully characterized by powder X-ray diffraction (PXRD), infrared (IR) spectra, elemental analyses (EA) and thermogravimetric analyses (TGA). Single-crystal X-ray diffraction analysis reveals that 1 shows 1D dimeric chain structure, while 2 gives a 3D dense packing framework. Topology analysis illustrates that 2 can be simplified as a 3-nodal net (4, 5, 6-connected net) with the point symbol of {44·62}{46·64}2{48·66·8}. In addition, solid state luminescent properties of two complexes have also been studied in detail, which may act as the potential optical materials.

Trinuclear organooxotin assemblies from solvothermal synthesis reaction: Crystal structure, hydrogen bonding and π π stacking interaction

NASA Astrophysics Data System (ADS)

Ma, Chunlin; Sun, Junshan; Zhang, Rufen

2007-05-01

Two new trinuclear mono-organooxotin(IV) complexes with 2,3,4,5-tetrafluorobenzoic acid and sodium perchlorate of the types: [(SnR) 3(OH)(2,3,4,5-F 4C 6HCO 2) 4 · ClO 4] · [O 2CC 6HF 4](R = PhCH 2, 1; o- F-PhCH 2 for 2), have been solvothermally synthesized and structurally characterized by elemental, IR, 1H, 13C and 119Sn NMR and X-ray crystallography diffraction analyses. Complex 2 is also characterized by X-ray crystallography diffraction analyses. In complex 2, four carboxyl groups and a perchlorate bridged three tin atoms in a cyclohexane chair arrangement and form the basic framework. A hydroxyl group comprises the oxygen components of the stannoxane ring system. In these complexes, weak but significant intramolecular hydrogen bonding and π-π stacking interaction are also shown. These contacts lead to aggregation and supramolecular assembly of complexes 1 and 2 into 1D or 2D framework.

The analysis of scalp irritation by coacervates produced in hair shampoo via FTIR with focal plane array detector, X-ray photoelectron microscopy and HaCaT cells.

PubMed

Jung, I K; Park, S C; Kim, S H; Kim, J H; Cha, N R; Bae, W R; Kim, H N; Cho, S A; Yoo, J W; Kim, B M; Lee, J H

2017-04-01

Coacervates are inevitably formed on scalp on using hair washing products. Our goal was to analyse the coacervates in detail to identify the part responsible for scalp stimulation. Shampoo that increases coacervate formation was applied to in vitro skin and was washed. The residue was then analysed using Fourier transform infrared spectroscopy-focal plane array (FTIR-FPA) and X-ray photoelectron microscopy (XPS). And HaCaT cells were used for irritant test of coacervate. Through this research, it was confirmed that the coacervate was a macromolecule structurally similar to a cationic polymer and contains an anionic surfactant. Its anionic surfactant was structurally semi-stable so that it released onto scalp when it absorbs moisture. Coacervate releases sulphate bonding into the matrix when it is exposed to water. Thus, the scalp stimulation would be expected. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Characterisation of the rare cadmium chromate pigment in a 19th century tube colour by Raman, FTIR, X-ray and EPR

NASA Astrophysics Data System (ADS)

Christiansen, Marie Bitsch; Sørensen, Mikkel Agerbæk; Sanyova, Jana; Bendix, Jesper; Simonsen, Kim Pilkjær

2017-03-01

In an investigation of the artists' materials used by P. S. Krøyer the contents of the tube colours found in Krøyer's painting cabinet were examined. In most cases, the results of the pigment analyses were as expected based on our knowledge of artists' colours used in the late 1800s and early 1900s. However, in one of the tube colours labelled "Jaune de Cadmium Citron" (cadmium lemon yellow) an extremely rare cadmium chromate pigment was found. The pigment was analysed and characterised by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), single-crystal X-ray crystallography, and electron paramagnetic resonance (EPR) spectroscopy. Cadmium chromate was synthesised by precipitation from an aqueous solution of cadmium nitrate and potassium chromate, and the resulting yellow crystals proved identical to the pigment found in the tube colour "Jaune de Cadmium Citron". The structure determined by single-crystal X-ray diffraction identified the pigment as 2CdCrO4·KOH·H2O or more accurately as KCd2(CrO4)2(H3O2) illustrating the μ-H3O2- species. The yellow colour of the paint sample taken from the tube had a greenish hue, which became even more prominent upon storage and drying. EPR analysis of the sample showed the presence of paramagnetic degradation products containing Cr(III) and Cr(V).

Characterisation of the rare cadmium chromate pigment in a 19th century tube colour by Raman, FTIR, X-ray and EPR.

PubMed

Christiansen, Marie Bitsch; Sørensen, Mikkel Agerbæk; Sanyova, Jana; Bendix, Jesper; Simonsen, Kim Pilkjær

2017-03-15

In an investigation of the artists' materials used by P. S. Krøyer the contents of the tube colours found in Krøyer's painting cabinet were examined. In most cases, the results of the pigment analyses were as expected based on our knowledge of artists' colours used in the late 1800s and early 1900s. However, in one of the tube colours labelled "Jaune de Cadmium Citron" (cadmium lemon yellow) an extremely rare cadmium chromate pigment was found. The pigment was analysed and characterised by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), single-crystal X-ray crystallography, and electron paramagnetic resonance (EPR) spectroscopy. Cadmium chromate was synthesised by precipitation from an aqueous solution of cadmium nitrate and potassium chromate, and the resulting yellow crystals proved identical to the pigment found in the tube colour "Jaune de Cadmium Citron". The structure determined by single-crystal X-ray diffraction identified the pigment as 2CdCrO 4 ·KOH·H 2 O or more accurately as KCd 2 (CrO 4 ) 2 (H 3 O 2 ) illustrating the μ-H 3 O 2 - species. The yellow colour of the paint sample taken from the tube had a greenish hue, which became even more prominent upon storage and drying. EPR analysis of the sample showed the presence of paramagnetic degradation products containing Cr(III) and Cr(V). Copyright © 2016 Elsevier B.V. All rights reserved.

Detection of uranium and chemical state analysis of individual radioactive microparticles emitted from the Fukushima nuclear accident using multiple synchrotron radiation X-ray analyses.

PubMed

Abe, Yoshinari; Iizawa, Yushin; Terada, Yasuko; Adachi, Kouji; Igarashi, Yasuhito; Nakai, Izumi

2014-09-02

Synchrotron radiation (SR) X-ray microbeam analyses revealed the detailed chemical nature of radioactive aerosol microparticles emitted during the Fukushima Daiichi Nuclear Power Plant (FDNPP) accident, resulting in better understanding of what occurred in the plant during the early stages of the accident. Three spherical microparticles (∼2 μm, diameter) containing radioactive Cs were found in aerosol samples collected on March 14th and 15th, 2011, in Tsukuba, 172 km southwest of the FDNPP. SR-μ-X-ray fluorescence analysis detected the following 10 heavy elements in all three particles: Fe, Zn, Rb, Zr, Mo, Sn, Sb, Te, Cs, and Ba. In addition, U was found for the first time in two of the particles, further confirmed by U L-edge X-ray absorption near-edge structure (XANES) spectra, implying that U fuel and its fission products were contained in these particles along with radioactive Cs. These results strongly suggest that the FDNPP was damaged sufficiently to emit U fuel and fission products outside the containment vessel as aerosol particles. SR-μ-XANES spectra of Fe, Zn, Mo, and Sn K-edges for the individual particles revealed that they were present at high oxidation states, i.e., Fe(3+), Zn(2+), Mo(6+), and Sn(4+) in the glass matrix, confirmed by SR-μ-X-ray diffraction analysis. These radioactive materials in a glassy state may remain in the environment longer than those emitted as water-soluble radioactive Cs aerosol particles.

High-pressure studies with x-rays using diamond anvil cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Guoyin; Mao, Ho Kwang

2016-11-22

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. Thesemore » HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.« less

High-pressure studies with x-rays using diamond anvil cells

NASA Astrophysics Data System (ADS)

Shen, Guoyin; Mao, Ho Kwang

2017-01-01

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.

Morphological evolution of X-ray flare structures from the rise through the decay phase. [Skylab study of solar flares

NASA Technical Reports Server (NTRS)

Kahler, S. W.; Krieger, A. S.; Vaiana, G. S.

1975-01-01

The morphological evolution of 12 solar X-ray subflares from onset through the decay phase has been studied using photographic X-ray images obtained from Skylab. The spatial configurations are found to vary widely from flare to flare, but they appear to be composed of two basic kinds of structures. The first, termed 'X-ray kernels', are brightest during the rise phase; the second, looplike structures, appear during the maximum and decay phases of the event. The X-ray kernels are small pointlike structures which may be related to the nonthermal phases of flares.

Thin soil layer of green roof systems studied by X-Ray CT

NASA Astrophysics Data System (ADS)

Šácha, Jan; Jelínková, Vladimíra; Dohnal, Michal

2016-04-01

The popular non-invasive visualization technique of X-ray computed tomography (CT) has been used for 3D examination of thin soil layer of vegetated roof systems. The two categories of anthropogenic soils, usually used for green roof systems, were scanned during the first months after green roof system construction. First was represented by stripped topsoil with admixed crushed bricks and was well graded in terms of particle size distribution. The other category represented a commercial lightweight technogenic substrate. The undisturbed soil samples of total volume of 62.8 ccm were studied be means of X-ray Computed Tomography using X-ray Inspection System GE Phoenix Nanomex 180T with resulting spatial resolution about 57 μm in all directions. For both soil categories visible macroporosity, connectivity (described by the Euler characteristic), dimensionless connectivity and critical cross section of pore network were determined. Moreover, the temporal structural changes of studied soils were discussed together with heat and water regime of the green roof system. The analysis of CT images of anthropogenic soils was problematic due to the different X-ray attenuation of individual constituents. The correct determination of the threshold image intensity differentiating the soil constituents from the air phase had substantial importance for soil pore network analyses. However, X-ray CT derived macroporosity profiles reveal significant temporal changes notably in the soil comprised the stripped topsoil with admixed crushed bricks. The results implies that the technogenic substrate is structurally more stable over time compared to the stripped topsoil. The research was realized as a part of the University Centre for Energy Efficient Buildings supported by the EU and with financial support from the Czech Science Foundation under project number 14-10455P.

Effects of soft X-ray radiation damage on paraffin-embedded rat tissues supported on ultralene: a chemical perspective.

PubMed

Bedolla, Diana E; Mantuano, Andrea; Pickler, Arissa; Mota, Carla Lemos; Braz, Delson; Salata, Camila; Almeida, Carlos Eduardo; Birarda, Giovanni; Vaccari, Lisa; Barroso, Regina Cély; Gianoncelli, Alessandra

2018-05-01

Radiation damage is an important aspect to be considered when analysing biological samples with X-ray techniques as it can induce chemical and structural changes in the specimens. This work aims to provide new insights into the soft X-ray induced radiation damage of the complete sample, including not only the biological tissue itself but also the substrate and embedding medium, and the tissue fixation procedure. Sample preparation and handling involves an unavoidable interaction with the sample matrix and could play an important role in the radiation-damage mechanism. To understand the influence of sample preparation and handling on radiation damage, the effects of soft X-ray exposure at different doses on ultralene, paraffin and on paraffin-embedded rat tissues were studied using Fourier-transform infrared (FTIR) microspectroscopy and X-ray microscopy. Tissues were preserved with three different commonly used fixatives: formalin, glutaraldehyde and Karnovsky. FTIR results showed that ultralene and paraffin undergo a dose-dependent degradation of their vibrational profiles, consistent with radiation-induced oxidative damage. In addition, formalin fixative has been shown to improve the preservation of the secondary structure of proteins in tissues compared with both glutaraldehyde and Karnovsky fixation. However, conclusive considerations cannot be drawn on the optimal fixation protocol because of the interference introduced by both substrate and embedding medium in the spectral regions specific to tissue lipids, nucleic acids and carbohydrates. Notably, despite the detected alterations affecting the chemical architecture of the sample as a whole, composed of tissue, substrate and embedding medium, the structural morphology of the tissues at the micrometre scale is essentially preserved even at the highest exposure dose.

Investigating the origins of nanostructural variations in differential ethnic hair types using X-ray scattering techniques.

PubMed

Wade, M; Tucker, I; Cunningham, P; Skinner, R; Bell, F; Lyons, T; Patten, K; Gonzalez, L; Wess, T

2013-10-01

Human hair is a major determinant of visual ethnic differentiation. Although hair types are celebrated as part of our ethnic diversity, the approach to hair care has made the assumption that hair types are structurally and chemically similar. Although this is clearly not the case at the macroscopic level, the intervention of many hair treatments is at the nanoscopic and molecular levels. The purpose of the work presented here is to identify the main nanoscopic and molecular hierarchical differences across five different ethnic hair types from hair fibres taken exclusively from the scalp. These are Afro (subdivided into elastic 'rubber' and softer non-elastic 'soft'), Chinese, European and Mullato (mixed race). Small angle X-Ray scattering (SAXS) is a technique capable of resolving nanostructural variations in complex materials. Individual hair fibres from different ethnic hair types were used to investigate structural features found in common and also specific to each type. Simultaneous wide angle X-Ray scattering (WAXS) was used to analyse the submolecular level structure of the fibrous keratin present. The data sets from both techniques were analysed with principal component analysis (PCA) to identify underlying variables. Principal component analysis of both SAXS and WAXS data was shown to discriminate the scattering signal between different hair types. The X-ray scattering results show a common underlying keratin intermediate filament (KIF) structure. However, distinct differences were observed in the preferential orientation and intensity signal from the lipid component of the hair. In addition, differences were observed in the intensity distribution of the very low-angle sample-dependent diffuse scatter surrounding the 'beamstop.' The results indicate that the fibrous keratin scaffold remains consistent between ethnic hair types. The hierarchies made by these may be modulated by variation in the content of keratin-associated proteins (KAPs) and lipids that alter the interfacial structures and lead to macroscopic differences in hair morphology. © 2013 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Cybastacines A and B: Antibiotic Sesterterpenes from a Nostoc sp. Cyanobacterium.

PubMed

Cabanillas, Alfredo H; Tena Pérez, Víctor; Maderuelo Corral, Santiago; Rosero Valencia, Diego Fernando; Martel Quintana, Antera; Ortega Doménech, Montserrat; Rumbero Sánchez, Ángel

2018-02-23

Cybastacines A (1) and B (2) were discovered as a novel pentacyclic sesterterpenoid-alkaloid skeleton structure, with a guanidinium group. These molecules were isolated from a Nostoc sp. cyanobacterium collected in the Canary Islands. Their structures were elucidated primarily by a combination of spectroscopic analyses and X-ray diffraction. These compounds showed antibiotic activities against several clinically relevant bacterial strains.

Synchrotron applications in wood preservation and deterioration

Treesearch

Barbara L. Illman

2003-01-01

Several non-intrusive synchrotron techniques are being used to detect and study wood decay. The techniques use high intensity synchrotron-generated X-rays to determine the atomic structure of materials with imaging, diffraction, and absorption. Some of the techniques are X-ray absorption near edge structure (XANES), X-ray fluorescence spectroscopy (XFS), X-ray...

Structure and substructure analysis of DAFT/FADA galaxy clusters in the [0.4-0.9] redshift range

NASA Astrophysics Data System (ADS)

Guennou, L.; Adami, C.; Durret, F.; Lima Neto, G. B.; Ulmer, M. P.; Clowe, D.; LeBrun, V.; Martinet, N.; Allam, S.; Annis, J.; Basa, S.; Benoist, C.; Biviano, A.; Cappi, A.; Cypriano, E. S.; Gavazzi, R.; Halliday, C.; Ilbert, O.; Jullo, E.; Just, D.; Limousin, M.; Márquez, I.; Mazure, A.; Murphy, K. J.; Plana, H.; Rostagni, F.; Russeil, D.; Schirmer, M.; Slezak, E.; Tucker, D.; Zaritsky, D.; Ziegler, B.

2014-01-01

Context. The DAFT/FADA survey is based on the study of ~90 rich (masses found in the literature >2 × 1014 M⊙) and moderately distant clusters (redshifts 0.4 < z < 0.9), all with HST imaging data available. This survey has two main objectives: to constrain dark energy (DE) using weak lensing tomography on galaxy clusters and to build a database (deep multi-band imaging allowing photometric redshift estimates, spectroscopic data, X-ray data) of rich distant clusters to study their properties. Aims: We analyse the structures of all the clusters in the DAFT/FADA survey for which XMM-Newton and/or a sufficient number of galaxy redshifts in the cluster range are available, with the aim of detecting substructures and evidence for merging events. These properties are discussed in the framework of standard cold dark matter (ΛCDM) cosmology. Methods: In X-rays, we analysed the XMM-Newton data available, fit a β-model, and subtracted it to identify residuals. We used Chandra data, when available, to identify point sources. In the optical, we applied a Serna & Gerbal (SG) analysis to clusters with at least 15 spectroscopic galaxy redshifts available in the cluster range. We discuss the substructure detection efficiencies of both methods. Results: XMM-Newton data were available for 32 clusters, for which we derive the X-ray luminosity and a global X-ray temperature for 25 of them. For 23 clusters we were able to fit the X-ray emissivity with a β-model and subtract it to detect substructures in the X-ray gas. A dynamical analysis based on the SG method was applied to the clusters having at least 15 spectroscopic galaxy redshifts in the cluster range: 18 X-ray clusters and 11 clusters with no X-ray data. The choice of a minimum number of 15 redshifts implies that only major substructures will be detected. Ten substructures were detected both in X-rays and by the SG method. Most of the substructures detected both in X-rays and with the SG method are probably at their first cluster pericentre approach and are relatively recent infalls. We also find hints of a decreasing X-ray gas density profile core radius with redshift. Conclusions: The percentage of mass included in substructures was found to be roughly constant with redshift values of 5-15%, in agreement both with the general CDM framework and with the results of numerical simulations. Galaxies in substructures show the same general behaviour as regular cluster galaxies; however, in substructures, there is a deficiency of both late type and old stellar population galaxies. Late type galaxies with recent bursts of star formation seem to be missing in the substructures close to the bottom of the host cluster potential well. However, our sample would need to be increased to allow a more robust analysis. Tables 1, 2, 4 and Appendices A-C are available in electronic form at http://www.aanda.org

Trace element distribution in the rat cerebellum

NASA Astrophysics Data System (ADS)

Kwiatek, W. M.; Long, G. J.; Pounds, J. G.; Reuhl, K. R.; Hanson, A. L.; Jones, K. W.

1990-04-01

Spatial distributions and concentrations of trace elements (TE) in the brain are important because TE perform catalytic and structural functions in enzymes which regulate brain function and development. We have investigated the distributions of TE in rat cerebellum. Structures were sectioned and analyzed by the Synchrotron Radiation Induced X-ray Emission (SRIXE) method using the NSLS X-26 white-light microprobe facility. Advantages important for TE analysis of biological specimens with X-ray microscopy include short time of measurement, high brightness and flux, good spatial resolution, multielemental detection, good sensitivity, and nondestructive irradiation. Trace elements were measured in thin rat brain sections of 20 μm thickness. The analyses were performed on sample volumes as small as 0.2 nl with Minimum Detectable Limits (MDL) of 50 ppb wet weight for Fe, 100 ppb wet weight for Cu, and Zn, and 1 ppm wet weight for Pb. The distribution of TE in the molecular cell layer, granule cell layer and fiber tract of rat cerebella was investigated. Both point analyses and two-dimensional semiquantitative mapping of the TE distribution in a section were used. All analyzed elements were observed in each structure of the cerebellum except mercury which was not observed in granule cell layer or fiber tract. This approach permits an exacting correlation of the TE distribution in complex structure with the diet, toxic elements, and functional status of the animal.

X-ray spectra and electron structure of A15 compounds of transition metals

NASA Astrophysics Data System (ADS)

Kurmaev, E. Z.; Iarmoshenko, Iu. M.

1988-01-01

Results of an X-ray emission spectroscopy study of the electron structure of A15 compounds are reported. In particular, attention is given to the X-ray spectra of A15 compounds of the A3B type with transition and nontransition elements, effect of alloying on the formation of the electron structure of ternary phases, and effect of atomic ordering in the X-ray spectra of A15 compounds with changes in heat treament and concentration. The X-ray spectra of A15 compounds irradiated by fast neutrons are also examined.

X-ray absorption spectroscopy: EXAFS (Extended X-ray Absorption Fine Structure) and XANES (X-ray Absorption Near Edge Structure)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alp, E.E.; Mini, S.M.; Ramanathan, M.

1990-04-01

The x-ray absorption spectroscopy (XAS) had been an essential tool to gather spectroscopic information about atomic energy level structure in the early decades of this century. It has also played an important role in the discovery and systematization of rare-earth elements. The discovery of synchrotron radiation in 1952, and later the availability of broadly tunable synchrotron based x-ray sources have revitalized this technique since the 1970's. The correct interpretation of the oscillatory structure in the x-ray absorption cross-section above the absorption edge by Sayers et. al. has transformed XAS from a spectroscopic tool to a structural technique. EXAFS (Extended X-raymore » Absorption Fine Structure) yields information about the interatomic distances, near neighbor coordination numbers, and lattice dynamics. An excellent description of the principles and data analysis techniques of EXAFS is given by Teo. XANES (X-ray Absorption Near Edge Structure), on the other hand, gives information about the valence state, energy bandwidth and bond angles. Today, there are about 50 experimental stations in various synchrotrons around the world dedicated to collecting x-ray absorption data from the bulk and surfaces of solids and liquids. In this chapter, we will give the basic principles of XAS, explain the information content of essentially two different aspects of the absorption process leading to EXAFS and XANES, and discuss the source and samples limitations.« less

Synchrotron powder X-ray diffraction and structural analysis of Eu0.5La0.5FBiS2-x Se x

NASA Astrophysics Data System (ADS)

Nagasaka, K.; Jinno, G.; Miura, O.; Miura, A.; Moriyoshi, C.; Kuroiwa, Y.; Mizuguchi, Y.

2017-07-01

Eu0.5La0.5FBiS2-x Se x is a new BiS2-based superconductor system. In Eu0.5La0.5FBiS2-x Se x , electron carriers are doped to the BiS2 layer by the substitution of Eu by La. Bulk superconductivity in this system is induced by increasing the in-plane chemical pressure, which is controlled by the Se concentration (x). In this study, we have analysed the crystal structure of Eu0.5La0.5FBiS2-x Se x using synchrotron powder diffraction and the Rietveld refinement. The precise determination of the structural parameters and thermal factors suggest that the emergence of bulk superconductivity in Eu0.5La0.5FBiS2-x Se x is achieved by the enhanced in-plane chemical pressure and the decrease in in-plane disorder.

Energy dispersive X-ray analyses of organelles of NaCI-treated maize root cells

NASA Astrophysics Data System (ADS)

Stelzer, Ralf

1984-04-01

NaCl sensitive plants of Zea mays cv. ADOUR were grown in nutrient solutions with or without NaCl. Frozen, hydrated root-tip tissues were investigated by means of an ETEC scanning electron microscope fitted with a KEVEX energy dispersive X-ray analyser. Morphological details of the gently etched but non-coated surface of the cross fractured specimen were easy to identify and to analyse using an electron beam with a low intensity at 10 kV. X-ray data obtained from cell compartments and organelles as nuclei, nucleoli and mitochondria within individual cells establish typical X-ray spectra. Comparisons of these spectra support the hypothesis that Na + ions are predominantly localized in vacuoles and also to a lesser extent in the cytoplasm, e.g. in small vesicles, but not in other cell organelles. Furthermore the analysed cell compartments show differences in the distribution of Mg, P, S, Cl, K and Ca effected by the addition of NaCl to the growth medium. The X-ray data are discussed in relation to the physiological meaning of a NaCl induced redistribution of elements within individual maize root cells.

X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

NASA Astrophysics Data System (ADS)

Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

2009-06-01

Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

Probing solid catalysts under operating conditions: electrons or X-rays?

PubMed

Thomas, John Meurig; Hernandez-Garrido, Juan-Carlos

2009-01-01

Seeing is believing: In light of recent advances, the pros and cons of using electrons and X-rays for in situ studies of catalysts are analyzed: by using X-rays the structure of bound reactants at steady state are obtained from extended X-ray adsorption fine structure spectroscopy (EXAFS) data (see graph), thereby affording mechanistic insights.

Transformation and Precipitation Reactions by Metal Active Gas Pulsed Welded Joints from X2CrNiMoN22-5-3 Duplex Stainless Steels

PubMed Central

Utu, Ion-Dragos; Mitelea, Ion; Urlan, Sorin Dumitru; Crăciunescu, Corneliu Marius

2016-01-01

The high alloying degree of Duplex stainless steels makes them susceptible to the formation of intermetallic phases during their exposure to high temperatures. Precipitation of these phases can lead to a decreasing of the corrosion resistance and sometimes of the toughness. Starting from the advantages of the synergic Metal Active Gas (MAG) pulsed welding process, this paper analyses the structure formation particularities of homogeneous welded joints from Duplex stainless steel. The effect of linear welding energy on the structure morphology of the welded joints was revealed by macro- and micrographic examinations, X-ray energy dispersion analyses, measurements of ferrite proportion and X-ray diffraction analysis. The results obtained showed that the transformation of ferrite into austenite is associated with the chromium, nickel, molybdenum and nitrogen distribution between these two phases and their redistribution degree is closely linked to the overall heat cycle of the welding process. The adequate control of the energy inserted in the welded components provides an optimal balance between the two microstructural constituents (Austenite and Ferrite) and avoids the formation of undesirable intermetallic phases. PMID:28773727

Transformation and Precipitation Reactions by Metal Active Gas Pulsed Welded Joints from X2CrNiMoN22-5-3 Duplex Stainless Steels.

PubMed

Utu, Ion-Dragos; Mitelea, Ion; Urlan, Sorin Dumitru; Crăciunescu, Corneliu Marius

2016-07-21

The high alloying degree of Duplex stainless steels makes them susceptible to the formation of intermetallic phases during their exposure to high temperatures. Precipitation of these phases can lead to a decreasing of the corrosion resistance and sometimes of the toughness. Starting from the advantages of the synergic Metal Active Gas (MAG) pulsed welding process, this paper analyses the structure formation particularities of homogeneous welded joints from Duplex stainless steel. The effect of linear welding energy on the structure morphology of the welded joints was revealed by macro- and micrographic examinations, X-ray energy dispersion analyses, measurements of ferrite proportion and X-ray diffraction analysis. The results obtained showed that the transformation of ferrite into austenite is associated with the chromium, nickel, molybdenum and nitrogen distribution between these two phases and their redistribution degree is closely linked to the overall heat cycle of the welding process. The adequate control of the energy inserted in the welded components provides an optimal balance between the two microstructural constituents (Austenite and Ferrite) and avoids the formation of undesirable intermetallic phases.

First-principles calculations of K-shell X-ray absorption spectra for warm dense nitrogen

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zi; Zhang, Shen; Kang, Wei

2016-05-15

X-ray absorption spectrum is a powerful tool for atomic structure detection on warm dense matter. Here, we perform first-principles molecular dynamics and X-ray absorption spectrum calculations on warm dense nitrogen along a Hugoniot curve. From the molecular dynamics trajectory, the detailed atomic structures are examined for each thermodynamical condition. The K-shell X-ray absorption spectrum is calculated, and its changes with temperature and pressure along the Hugoniot curve are discussed. The warm dense nitrogen systems may contain isolated nitrogen atoms, N{sub 2} molecules, and nitrogen clusters, which show quite different contributions to the total X-ray spectrum due to their different electronmore » density of states. The changes of X-ray spectrum along the Hugoniot curve are caused by the different nitrogen structures induced by the temperature and the pressure. Some clear signatures on X-ray spectrum for different thermodynamical conditions are pointed out, which may provide useful data for future X-ray experiments.« less

Local structure and X-ray magnetic circular dichroism of Au in Au-Co nanoalloys

NASA Astrophysics Data System (ADS)

Maurizio, C.; Michieli, N.; Kalinic, B.; Mattarello, V.; Bello, V.; Wilhelm, F.; Ollefs, K.; Mattei, G.

2018-03-01

Coupling a plasmonic metal with a magnetic one in thin films and nanostructures is very interesting for the emerging field of magnetoplasmonics. In particular, coupling through alloying is a promising strategy to induce a magnetic moment on the plasmonic metal atoms, in a way that is intimately related to the local structure of the (metastable) alloy material. In this framework, Au:Co bimetallic films have been produced via magnetron co-sputtering deposition. X-ray absorption spectroscopy (XAS) at both Au- and Co-edges clearly indicates the formation of a full-metallic layer composed for the major part of a binary AuxCo1-x alloy, with x = 0.7-0.8. XAS and transmission electron microscopy analyses suggest the presence of a minor fraction of segregated metals. X-ray magnetic circular dichroism (XMCD) analysis at Au L2,3 edges detected a net magnetic moment of Au atoms (μ = 0.06 μB), significantly larger (≈3.5 times) that the one for Au-capped Co nanoclusters and comparable to the one for a Co-rich Au/Co multilayer, despite the 4 times larger concentration of Co with respect to the present case. This Au-Co magnetic coupling is favored by a high degree of mixing of the two metals in the alloy.

Transmission X-ray microscopy for full-field nano-imaging of biomaterials

PubMed Central

ANDREWS, JOY C; MEIRER, FLORIAN; LIU, YIJIN; MESTER, ZOLTAN; PIANETTA, PIERO

2010-01-01

Imaging of cellular structure and extended tissue in biological materials requires nanometer resolution and good sample penetration, which can be provided by current full-field transmission X-ray microscopic techniques in the soft and hard X-ray regions. The various capabilities of full-field transmission X-ray microscopy (TXM) include 3D tomography, Zernike phase contrast, quantification of absorption, and chemical identification via X-ray fluorescence and X-ray absorption near edge structure (XANES) imaging. These techniques are discussed and compared in light of results from imaging of biological materials including microorganisms, bone and mineralized tissue and plants, with a focus on hard X-ray TXM at ≤ 40 nm resolution. PMID:20734414

X-ray Fluorescence Holography: Principles, Apparatus, and Applications

NASA Astrophysics Data System (ADS)

Hayashi, Kouichi; Korecki, Pawel

2018-06-01

X-ray fluorescence holography (XFH) is an atomic structure determination technique that combines the capabilities of X-ray diffraction and X-ray fluorescence spectroscopy. It provides a unique means of gaining fully three-dimensional information about the local atomic structure and lattice site positions of selected elements inside compound samples. In this work, we discuss experimental and theoretical aspects that are essential for the efficient recording and analysis of X-ray fluorescence holograms and review the most recent advances in XFH. We describe experiments performed with brilliant synchrotron radiation as well as with tabletop setups that employ conventional X-ray tubes.

Review of the applications of x-ray refraction and the x-ray waveguide phenomenon to estimation of film structures.

PubMed

Hayashi, Kouichi

2010-12-01

Based on our previous work, I review the applications of x-ray refraction and the x-ray waveguide phenomenon to organic and inorganic thin films in the present paper. Under grazing incidence conditions, observations of refracted x-rays and guided x-rays due to the x-ray waveguide phenomenon provide information about thin film structures, and thus have potential as alternative methods to x-ray reflectivity. To date, we have measured the spectra of the refracted x-rays and guided x-rays from end faces of thin films using white incident x-ray beams, and utilized them for the determination of film density and thickness. Some of this work is summarized in the present paper. At the end of this paper, I describe our recent achievement in this field, namely the in situ measurement of guided x-rays during the film degradation process due to strong synchrotron radiation damage. Moreover, I discuss the perspective of the present technique from the viewpoint of micro-characterization and real-time estimation of thin films.

Thermal effects of laser marking on microstructure and corrosion properties of stainless steel.

PubMed

Švantner, M; Kučera, M; Smazalová, E; Houdková, Š; Čerstvý, R

2016-12-01

Laser marking is an advanced technique used for modification of surface optical properties. This paper presents research on the influence of laser marking on the corrosion properties of stainless steel. Processes during the laser beam-surface interaction cause structure and color changes and can also be responsible for reduction of corrosion resistance of the surface. Corrosion tests, roughness, microscopic, energy dispersive x-ray, grazing incidence x-ray diffraction, and ferrite content analyses were carried out. It was found that increasing heat input is the most crucial parameter regarding the degradation of corrosion resistance of stainless steel. Other relevant parameters include the pulse length and pulse frequency. The authors found a correlation between laser processing parameters, grazing incidence x-ray measurement, ferrite content, and corrosion resistance of the affected surface. Possibilities and limitations of laser marking of stainless steel in the context of the reduction of its corrosion resistance are discussed.

Reverse engineering the ancient ceramic technology based on X-ray fluorescence spectromicroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sciau, Philippe; Leon, Yoanna; Goudeau, Philippe

2011-07-06

We present results of X-ray fluorescence (XRF) microprobe analyses of ancient ceramic cross-sections aiming at deciphering the different firing protocols used for their production. Micro-focused XRF elemental mapping, Fe chemical mapping and Fe K-edge X-ray absorption near edge structure spectroscopy were performed on pre-sigillata ceramics from southern Gaul, and terra Sigillata vessels from Italy and southern Gaul. Pieces from the different workshops and regions showed significant difference in the starting clay material, clay conditioning and kiln firing condition. By contrast, sherds from the same workshop exhibited more subtle differences and possible misfirings. Understanding the precise firing conditions and protocols wouldmore » allow recreation of kilns for various productions. Furthermore, evolution and modification of kiln design would shed some light on how ancient potters devised solutions to diverse technological problems they encountered.« less

Atmospheric electron x-ray spectrometer

NASA Technical Reports Server (NTRS)

Feldman, Jason E. (Inventor); George, Thomas (Inventor); Wilcox, Jaroslava Z. (Inventor)

2002-01-01

The present invention comprises an apparatus for performing in-situ elemental analyses of surfaces. The invention comprises an atmospheric electron x-ray spectrometer with an electron column which generates, accelerates, and focuses electrons in a column which is isolated from ambient pressure by a:thin, electron transparent membrane. After passing through the membrane, the electrons impinge on the sample in atmosphere to generate characteristic x-rays. An x-ray detector, shaping amplifier, and multi-channel analyzer are used for x-ray detection and signal analysis. By comparing the resultant data to known x-ray spectral signatures, the elemental composition of the surface can be determined.

Investigating the Defect Structures in Transparent Conducting Oxides Using X-ray and Neutron Scattering Techniques

PubMed Central

González, Gabriela B.

2012-01-01

Transparent conducting oxide (TCO) materials are implemented into a wide variety of commercial devices because they possess a unique combination of high optical transparency and high electrical conductivity. Created during the processing of the TCOs, defects within the atomic-scale structure are responsible for their desirable optical and electrical properties. Therefore, studying the defect structure is essential to a better understanding of the behavior of transparent conductors. X-ray and neutron scattering techniques are powerful tools to investigate the atomic lattice structural defects in these materials. This review paper presents some of the current developments in the study of structural defects in n-type TCOs using x-ray diffraction (XRD), neutron diffraction, extended x-ray absorption fine structure (EXAFS), pair distribution functions (PDFs), and x-ray fluorescence (XRF). PMID:28817010

Hemoglobin redux: combining neutron and X-ray diffraction with mass spectrometry to analyse the quaternary state of oxidized hemoglobins

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mueser, Timothy C., E-mail: timothy.mueser@utoledo.edu; Griffith, Wendell P.; Kovalevsky, Andrey Y.

2010-11-01

X-ray and neutron diffraction studies of cyanomethemoglobin are being used to evaluate the structural waters within the dimer–dimer interface involved in quaternary-state transitions. Improvements in neutron diffraction instrumentation are affording the opportunity to re-examine the structures of vertebrate hemoglobins and to interrogate proton and solvent position changes between the different quaternary states of the protein. For hemoglobins of unknown primary sequence, structural studies of cyanomethemoglobin (CNmetHb) are being used to help to resolve sequence ambiguity in the mass spectra. These studies have also provided additional structural evidence for the involvement of oxidized hemoglobin in the process of erythrocyte senescence. X-raymore » crystal studies of Tibetan snow leopard CNmetHb have shown that this protein crystallizes in the B state, a structure with a more open dyad, which possibly has relevance to RBC band 3 protein binding and erythrocyte senescence. R-state equine CNmetHb crystal studies elaborate the solvent differences in the switch and hinge region compared with a human deoxyhemoglobin T-state neutron structure. Lastly, comparison of histidine protonation between the T and R state should enumerate the Bohr-effect protons.« less

X-ray structure investigation of some substituted indoles, and the x-ray crystal of 1,1'-bishomocubane

DOE Office of Scientific and Technical Information (OSTI.GOV)

Quarles, William G.

1970-05-01

The crystal structures of 5-methoxytryptamine, melatonin, and the p-bromobenzoate of 1,1'-bishomocubane have been solved by x-ray diffraction methods. A computer program for the trial and error solution of crystal structures is also described here.

X-Ray Reprocessing in Active Galactic Nuclei

NASA Technical Reports Server (NTRS)

Begelman, Mitchell C.

2004-01-01

This is the final report for research entitled "X-ray reprocessing in active galactic nuclei," into X-ray absorption and emission in various classes of active galaxy via X-ray spectral signatures. The fundamental goal of the research was to use these signatures as probes of the central engine structure and circumnuclear environment of active galactic nuclei. The most important accomplishment supported by this grant involved the detailed analysis and interpretation of the XMM data for the bright Seyfert 1 galaxy MCG-6-30-15. This work was performed by Drs. Christopher Reynolds and Mitchell Begelman in collaboration with Dr. Jorn Wilms (University of Tubingen, Germany; PI of the XMM observation) and other European scientists. With XMM we obtained medium resolution X-ray spectra of unprecedented quality for this Seyfert galaxy. Modeling the X-ray spectrum within the framework of accretion disk reflection models produced the first evidence for energy extraction from the spin of a black hole. Specifically, we found that the extreme gravitational redshifts required to explain the X-ray spectrum suggests that the bulk of the energy dissipation is concentrated very close to the black hole, in contrast with the expectations of any pure accretion disk model. In a second paper we addressed the low- energy spectral complexity and used RXTE specta to pin down the high-energy spectral index, thus firming up our initial interpretation. Additionally, we carried out detailed spectral and variability analyses of a number of Seyfert and radio galaxies (e.g., NGC 5548 and 3C 111) and developed general techniques that will be useful in performing X-ray reverberation mapping of accretion disks in AGN, once adequate data becomes available. A list of papers supported by this research is included.

Worldwide Protein Data Bank validation information: usage and trends.

PubMed

Smart, Oliver S; Horský, Vladimír; Gore, Swanand; Svobodová Vařeková, Radka; Bendová, Veronika; Kleywegt, Gerard J; Velankar, Sameer

2018-03-01

Realising the importance of assessing the quality of the biomolecular structures deposited in the Protein Data Bank (PDB), the Worldwide Protein Data Bank (wwPDB) partners established Validation Task Forces to obtain advice on the methods and standards to be used to validate structures determined by X-ray crystallography, nuclear magnetic resonance spectroscopy and three-dimensional electron cryo-microscopy. The resulting wwPDB validation pipeline is an integral part of the wwPDB OneDep deposition, biocuration and validation system. The wwPDB Validation Service webserver (https://validate.wwpdb.org) can be used to perform checks prior to deposition. Here, it is shown how validation metrics can be combined to produce an overall score that allows the ranking of macromolecular structures and domains in search results. The ValTrends DB database provides users with a convenient way to access and analyse validation information and other properties of X-ray crystal structures in the PDB, including investigating trends in and correlations between different structure properties and validation metrics.

Worldwide Protein Data Bank validation information: usage and trends

PubMed Central

Horský, Vladimír; Gore, Swanand; Svobodová Vařeková, Radka; Bendová, Veronika

2018-01-01

Realising the importance of assessing the quality of the biomolecular structures deposited in the Protein Data Bank (PDB), the Worldwide Protein Data Bank (wwPDB) partners established Validation Task Forces to obtain advice on the methods and standards to be used to validate structures determined by X-ray crystallography, nuclear magnetic resonance spectroscopy and three-dimensional electron cryo-microscopy. The resulting wwPDB validation pipeline is an integral part of the wwPDB OneDep deposition, biocuration and validation system. The wwPDB Validation Service webserver (https://validate.wwpdb.org) can be used to perform checks prior to deposition. Here, it is shown how validation metrics can be combined to produce an overall score that allows the ranking of macromolecular structures and domains in search results. The ValTrendsDB database provides users with a convenient way to access and analyse validation information and other properties of X-ray crystal structures in the PDB, including investigating trends in and correlations between different structure properties and validation metrics. PMID:29533231

Structural diversity of silver (I) azine complexes - Effect of substituents and counter anions

NASA Astrophysics Data System (ADS)

Patra, Goutam Kumar; Mukherjee, Anindita; Mitra, Partha; Adarsh, N. N.

2011-08-01

Three new Ag(I) complexes, 1, 2, and 3 of two azine ligands diacetyl dihydrazone ( L1) and benzil dihydrazone ( L2) have been synthesized and characterized by single crystal X-ray diffraction studies (for 2 and 3), X-ray powder diffraction studies( 1 and 2), elemental analyses, IR and UV-VIS spectroscopy and TGA analysis. They represent one-dimensional polymeric assemblies and discrete dinuclear Ag(I) complex depending on functionality of the ligands and the counter anions. Tetrahedral as well as square pyramidal coordination motifs of the silver (I) ions have been observed in the supramolecular designing of such hybrid organic-inorganic materials.

X-ray diffraction studies of enkephalins. Crystal structure of [(4'-bromo) Phe4,Leu5]enkephalin.

PubMed Central

Ishida, T; Kenmotsu, M; Mino, Y; Inoue, M; Fujiwara, T; Tomita, K; Kimura, T; Sakakibara, S

1984-01-01

In order to investigate the structure-activity relationship of [Leu5]- and [Met5]enkephalins, [(4'-bromo)Phe4, Leu5]-, [(4'-bromo)Phe4, Met5]- and [Met5] enkephalins were synthesized and crystallized. The crystal structure of [(4'-bromo) Phe4, Leu5]- enkephalin was determined by X-ray diffraction method using the heavy atom method and refined to R = 0.092 by the least-squares method. The molecule in this crystal took essentially the same type I' beta-turn conformation found in [Leu5]enkephalin [Smith & Griffin (1978) Science 199, 1214-1216). On the other hand, the preliminary three-dimensional Patterson analyses showed that the most probable conformations of [(4'-bromo)Phe4,Met5]- and [Met5]enkephalins are both the dimeric extended forms. Based on these insights, the biologically active conformation of enkephalin was discussed in relation to the mu- and delta-receptors. PMID:6721829

Effects of Piezoelectric Potential of ZnO on Resistive Switching Characteristics of Flexible ZnO/TiO2 Heterojunction Cells

NASA Astrophysics Data System (ADS)

Li, Hongxia; Zhou, You; Du, Gang; Huang, Yanwei; Ji, Zhenguo

2018-03-01

Flexible resistance random access memory (ReRAM) devices with a heterojunction structure of PET/ITO/ZnO/TiO2/Au were fabricated on polyethylene terephthalate/indium tin oxide (PET/ITO) substrates by different physical and chemical preparation methods. X-ray diffraction, scanning electron microscopy and atomic force microscopy were carried out to investigate the crystal structure, surface topography and cross-sectional structure of the prepared films. X-ray photoelectron spectroscopy was also used to identify the chemical state of Ti, O and Zn elements. Theoretical and experimental analyses were conducted to identify the effect of piezoelectric potential of ZnO on resistive switching characteristics of flexible ZnO/TiO2 heterojunction cells. The results showed a pathway to enhance the performance of ReRAM devices by engineering the interface barrier, which is also feasible for other electronics, optoelectronics and photovoltaic devices.

A new series of lanthanide coordination polymers with 2,2‧-bipyridine and glutaric acid: Synthesis, crystal structures and properties of [Ln(bipy)(glut)(NO3)

NASA Astrophysics Data System (ADS)

Wang, Chunguang; Xing, Yongheng; Li, Zhangpeng; Li, Jing; Zeng, Xiaoqing; Ge, Maofa; Niu, Shuyun

2009-08-01

A series of new lanthanide coordination polymers, with the formula [Ln(bipy)(glut)(NO 3)] (Ln = Eu ( 1), Tb ( 2), Sm ( 3), Pr ( 4); bipy = 2,2'-bipyridine; H 2glut = glutaric acid), have been synthesized under the hydrothermal condition and characterized by elemental analysis, IR spectroscopy, powder X-ray diffraction, and single-crystal X-ray diffraction. Structural analyses reveal that all four complexes are isostructural and crystallized in monoclinic system, P2 1/ c space group. For these complexes, the Ln 3+ are all linked through glutaric acid ligands to form 1D chain-like polymeric structures, and bipy and NO3- are coordinated on two sides of the chains. The thermogravimetric analysis of 1 and photoluminescent properties of 1 and 2 are discussed in detail.

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix.

PubMed

Di Luccio, Tiziana; Laera, Anna Maria; Tapfer, Leander; Kempter, Susanne; Kraus, Robert; Nickel, Bert

2006-06-29

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.

Resonant soft X-ray scattering on protein solutions

NASA Astrophysics Data System (ADS)

Ye, Dan; Le, Thinh; Wang, Cheng; Zwart, Peter; Gomez, Esther; Gomez, Enrique

Protein structure is crucial for biological function, such that characterizing protein folding and packing is important for the design of therapeutics and enzymes. We propose resonant soft X-ray scattering (RSOXS) as an approach to study proteins and other biological assemblies in solution. Calculations of the scattering contrast suggest that soft X-ray scattering is more sensitive than hard X-ray scattering, because of contrast generated at the absorption edges of constituent elements such as carbon, nitrogen and oxygen. We have examined the structure of bovine serum albumin (BSA) in solution by RSOXS. We find that by varying incident X-ray energies, we are able to achieve higher scattering contrast near the absorption edge. From our RSOXS scattering result we are able to reconstruct the structure of BSA in 3D. These RSOXS results also agree with hard X-ray experiments, including crystallographic data. Our study demonstrates the potential of RSOXS for studying protein structure in solution.

Epitaxial growth and properties of YBa2Cu3O(x)-Pb(Zr(0.6)Ti(0.4))O3-YBa2Cu3O(x) trilayer structure by laser ablation

NASA Astrophysics Data System (ADS)

Boikov, Iu. A.; Esaian, S. K.; Ivanov, Z. G.; Brorsson, G.; Claeson, T.; Lee, J.; Safari, A.

1992-08-01

YBa2Cu3O(x)Pb(Zr(0.6)Ti(0.4))O3-YBa2Cu3O(x) multilayer structure has been grown on SrTiO3 and Al2O3 substrates using laser ablation. The deposition conditions for the growth of trilayers and their properties are studied in this investigation. Scanning electron microscope images and X-ray diffraction analyses indicate that all the constituent films in the trilayer grow epitaxially on SrTiO3 and were highly oriented on Al2O3. Transport measurements on these multilayers show that top YBa2Cu3O(x) films have good superconducting properties.

X-ray crystallography over the past decade for novel drug discovery - where are we heading next?

PubMed

Zheng, Heping; Handing, Katarzyna B; Zimmerman, Matthew D; Shabalin, Ivan G; Almo, Steven C; Minor, Wladek

2015-01-01

Macromolecular X-ray crystallography has been the primary methodology for determining the three-dimensional structures of proteins, nucleic acids and viruses. Structural information has paved the way for structure-guided drug discovery and laid the foundations for structural bioinformatics. However, X-ray crystallography still has a few fundamental limitations, some of which may be overcome and complemented using emerging methods and technologies in other areas of structural biology. This review describes how structural knowledge gained from X-ray crystallography has been used to advance other biophysical methods for structure determination (and vice versa). This article also covers current practices for integrating data generated by other biochemical and biophysical methods with those obtained from X-ray crystallography. Finally, the authors articulate their vision about how a combination of structural and biochemical/biophysical methods may improve our understanding of biological processes and interactions. X-ray crystallography has been, and will continue to serve as, the central source of experimental structural biology data used in the discovery of new drugs. However, other structural biology techniques are useful not only to overcome the major limitation of X-ray crystallography, but also to provide complementary structural data that is useful in drug discovery. The use of recent advancements in biochemical, spectroscopy and bioinformatics methods may revolutionize drug discovery, albeit only when these data are combined and analyzed with effective data management systems. Accurate and complete data management is crucial for developing experimental procedures that are robust and reproducible.

Covalency in Metal-Oxygen Multiple Bonds Evaluated Using Oxygen K-edge Spectroscopy and Electronic Structure Theory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Minasian, Stefan G.; Keith, Jason M.; Batista, Enrique R.

Advancing theories of how metal oxygen bonding influences metal oxo properties can expose new avenues for innovation in materials science, catalysis, and biochemistry. Historically, spectroscopic analyses of the transition metal peroxyanions, MO4x-, have formed the basis for new M O bonding theories. Herein, relative changes in M O orbital mixing in MO42- (M = Cr, Mo, W) and MO41- (M = Mn, Tc, Re) are evaluated for the first time by non-resonant inelastic X-ray scattering, X-ray absorption spectroscopy using fluorescence and transmission (via a scanning transmission X-ray microscope), and linear-response density functional theory. The results suggest that moving from Groupmore » 6 to Group 7 or down the triads increases M O e () mixing. Meanwhile, t2 mixing ( + ) remains relatively constant within the same Group. These unexpected changes in frontier orbital energy and composition are evaluated in terms of periodic trends in d orbital energy and radial extension.« less

X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy of tetragonal Mn72Ge28 epitaxial thin film

NASA Astrophysics Data System (ADS)

Kim, Jinhyeok; Mizuguchi, Masaki; Inami, Nobuhito; Ueno, Tetsuro; Ueda, Shigenori; Takanashi, Koki

2018-04-01

An epitaxially grown Mn72Ge28 film with a tetragonal crystal structure was fabricated. It was clarified that the film had a perpendicular magnetization and a high perpendicular magnetic anisotropy energy of 14.3 Merg/cm3. The electronic structure was investigated by X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy. The obtained X-ray magnetic circular dichroism spectrum revealed that the Mn orbital magnetic moment governed the magnetocrystalline anisotropy of the Mn72Ge28 film. A doublet structure was observed for the Mn 2p3/2 peak of hard X-ray photoelectron spectrum, indicating the spin exchange interaction between the 2p core-hole and 3d valence electrons.

Enhanced Imaging of Corrosion in Aircraft Structures with Reverse Geometry X-ray(registered tm)

NASA Technical Reports Server (NTRS)

Winfree, William P.; Cmar-Mascis, Noreen A.; Parker, F. Raymond

2000-01-01

The application of Reverse Geometry X-ray to the detection and characterization of corrosion in aircraft structures is presented. Reverse Geometry X-ray is a unique system that utilizes an electronically scanned x-ray source and a discrete detector for real time radiographic imaging of a structure. The scanned source system has several advantages when compared to conventional radiography. First, the discrete x-ray detector can be miniaturized and easily positioned inside a complex structure (such as an aircraft wing) enabling images of each surface of the structure to be obtained separately. Second, using a measurement configuration with multiple detectors enables the simultaneous acquisition of data from several different perspectives without moving the structure or the measurement system. This provides a means for locating the position of flaws and enhances separation of features at the surface from features inside the structure. Data is presented on aircraft specimens with corrosion in the lap joint. Advanced laminographic imaging techniques utilizing data from multiple detectors are demonstrated to be capable of separating surface features from corrosion in the lap joint and locating the corrosion in multilayer structures. Results of this technique are compared to computed tomography cross sections obtained from a microfocus x-ray tomography system. A method is presented for calibration of the detectors of the Reverse Geometry X-ray system to enable quantification of the corrosion to within 2%.

X-ray backscatter imaging of nuclear materials

DOEpatents

Chapman, Jeffrey Allen; Gunning, John E; Hollenbach, Daniel F; Ott, Larry J; Shedlock, Daniel

2014-09-30

The energy of an X-ray beam and critical depth are selected to detect structural discontinuities in a material having an atomic number Z of 57 or greater. The critical depth is selected by adjusting the geometry of a collimator that blocks backscattered radiation so that backscattered X-ray originating from a depth less than the critical depth is not detected. Structures of Lanthanides and Actinides, including nuclear fuel rod materials, can be inspected for structural discontinuities such as gaps, cracks, and chipping employing the backscattered X-ray.

X-ray tomography as a powerful method for zinc-air battery research

NASA Astrophysics Data System (ADS)

Franke-Lang, Robert; Arlt, Tobias; Manke, Ingo; Kowal, Julia

2017-12-01

X-ray tomography is used to investigate material redistribution and effects of electrochemical reactions in a zinc-air battery in-situ. For this, a special battery set-up is developed which meets tomographic and electrochemical requirements. The prepared batteries are discharged and some of them have partially been charged. To analyse the three-dimensional structure of the zinc and air electrode a tomographic measurement is made in charge and discharge condition without disassembling the battery. X-ray tomography gives the opportunity to detect and analyse three different effects within the cell operation: tracking the morphology and transformation of zinc and air electrode, monitoring electrolyte decomposition and movement, finding electrical misbehaviour by parasitic reactions. Therefore, it is possible to identify the loss of capacity and major problems of cyclability. The electrolyte strongly reacts with the pure zinc that leads to gassing and a loss of electrolyte. The loss prevents a charge carrier exchange between the anode and the cathode and reduces the theoretical capacity. One of the chemical reaction produces hydroxylated zinc, namely zincate. The most crucial problems with cyclability are affected by zincate movement into the catalyst layer. This assumption is confirmed by finding pure zinc areas within the catalyst layer.

Electronic structure and soft-X-ray-induced photoreduction studies of iron-based magnetic polyoxometalates of type {(M)M5}12Fe(III)30 (M = Mo(VI), W(VI)).

PubMed

Kuepper, Karsten; Derks, Christine; Taubitz, Christian; Prinz, Manuel; Joly, Loïc; Kappler, Jean-Paul; Postnikov, Andrei; Yang, Wanli; Kuznetsova, Tatyana V; Wiedwald, Ulf; Ziemann, Paul; Neumann, Manfred

2013-06-14

Giant Keplerate-type molecules with a {Mo72Fe30} core show a number of very interesting properties, making them particularly promising for various applications. So far, only limited data on the electronic structure of these molecules from X-ray spectra and electronic structure calculations have been available. Here we present a combined electronic and magnetic structure study of three Keplerate-type nanospheres--two with a {Mo72Fe30} core and one with a {W72Fe30} core by means of X-ray absorption spectroscopy, X-ray magnetic circular dichroism (XMCD), SQUID magnetometry, and complementary theoretical approaches. Furthermore, we present detailed studies of the Fe(3+)-to-Fe(2+) photoreduction process, which is induced under soft X-ray radiation in these molecules. We observe that the photoreduction rate greatly depends on the ligand structure surrounding the Fe ions, with negatively charged ligands leading to a dramatically reduced photoreduction rate. This opens the possibility of tailoring such polyoxometalates by X-ray spectroscopic studies and also for potential applications in the field of X-ray induced photochemistry.

Transmission X-ray microscopy for full-field nano imaging of biomaterials.

PubMed

Andrews, Joy C; Meirer, Florian; Liu, Yijin; Mester, Zoltan; Pianetta, Piero

2011-07-01

Imaging of cellular structure and extended tissue in biological materials requires nanometer resolution and good sample penetration, which can be provided by current full-field transmission X-ray microscopic techniques in the soft and hard X-ray regions. The various capabilities of full-field transmission X-ray microscopy (TXM) include 3D tomography, Zernike phase contrast, quantification of absorption, and chemical identification via X-ray fluorescence and X-ray absorption near edge structure imaging. These techniques are discussed and compared in light of results from the imaging of biological materials including microorganisms, bone and mineralized tissue, and plants, with a focus on hard X-ray TXM at ≤ 40-nm resolution. Copyright © 2010 Wiley-Liss, Inc.

Resonant soft X-ray scattering for polymer materials

DOE PAGES

Liu, Feng; Brady, Michael A.; Wang, Cheng

2016-04-16

Resonant Soft X-ray Scattering (RSoXS) was developed within the last few years, and the first dedicated resonant soft X-ray scattering beamline for soft materials was constructed at the Advanced Light Source, LBNL. RSoXS combines soft X-ray spectroscopy with X-ray scattering and thus offers statistical information for 3D chemical morphology over a large length scale range from nanometers to micrometers. Using RSoXS to characterize multi-length scale soft materials with heterogeneous chemical structures, we have demonstrated that soft X-ray scattering is a unique complementary technique to conventional hard X-ray and neutron scattering. Its unique chemical sensitivity, large accessible size scale, molecular bondmore » orientation sensitivity with polarized X-rays, and high coherence have shown great potential for chemically specific structural characterization for many classes of materials.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gholipur, Reza, E-mail: gholipur.reza@gmail.com; Bahari, Ali, E-mail: a.bahari@umz.ac.ir

Highlights: • Glassy Ce{sub x}La{sub 1−x}O{sub y} nanostructure films were grown on Si(1 0 0) substrate using the sol–gel method. • G{sub p} = ωϵ{sub 0}ϵ′ tan(δ) was calculated at different temperatures. • Electrical and structural the Ce{sub x}La{sub 1−x}O{sub y} samples were studied. • The conductivity-temperature study shows that the compound obeys the Arrhenius law. - Abstract: The Ce{sub x}La{sub 1−x}O{sub y} samples are synthesized, characterized and their electrical properties are reported at different molar ratios in the frequency range of 10{sup −1}–10{sup +5} Hz. Ac conductivity and permittivity data are analyzed by using conductivity formalism. The values ofmore » capacitance and tan(δ) were recorded with respect to different frequencies and temperatures. X-ray diffraction (XRD) patterns of the films show that the films posses crystalline phases. Surface morphology of the films is analyzed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The energy dispersive X-ray (EDX) and X-ray photoelectron spectroscopy (XPS) analyses reveal that elemental composition is in right stoichiometry. Electrical characterizations of the Ce{sub x}La{sub 1−x}O{sub y} samples were done by capacitance–voltage (C–V) and current density–voltage (J–V) measurements of MOS structures. Investigation showed high value of k = 44.80 and low leakage current (∼1 × 10{sup −5} A/cm{sup 2}) of the Ce{sub 0.4}La{sub 0.6}O{sub y} film.« less

Sulfur Speciation in Biochars by Very High Resolution Benchtop Kα X-ray Emission Spectroscopy.

PubMed

Holden, William M; Seidler, Gerald T; Cheah, Singfoong

2018-05-30

The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33 S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given by benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Kα XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.

Sulfur Speciation in Biochars by Very High Resolution Benchtop Ka X-Ray Emission Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cheah, Singfoong; Holden, William M.; Seidler, Gerald T.

The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given bymore » benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Ka XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.« less

Observation of femtosecond X-ray interactions with matter using an X-ray–X-ray pump–probe scheme

PubMed Central

Inoue, Ichiro; Inubushi, Yuichi; Sato, Takahiro; Tono, Kensuke; Katayama, Tetsuo; Kameshima, Takashi; Ogawa, Kanade; Togashi, Tadashi; Owada, Shigeki; Amemiya, Yoshiyuki; Tanaka, Takashi; Hara, Toru

2016-01-01

Resolution in the X-ray structure determination of noncrystalline samples has been limited to several tens of nanometers, because deep X-ray irradiation required for enhanced resolution causes radiation damage to samples. However, theoretical studies predict that the femtosecond (fs) durations of X-ray free-electron laser (XFEL) pulses make it possible to record scattering signals before the initiation of X-ray damage processes; thus, an ultraintense X-ray beam can be used beyond the conventional limit of radiation dose. Here, we verify this scenario by directly observing femtosecond X-ray damage processes in diamond irradiated with extraordinarily intense (∼1019 W/cm2) XFEL pulses. An X-ray pump–probe diffraction scheme was developed in this study; tightly focused double–5-fs XFEL pulses with time separations ranging from sub-fs to 80 fs were used to excite (i.e., pump) the diamond and characterize (i.e., probe) the temporal changes of the crystalline structures through Bragg reflection. It was found that the pump and probe diffraction intensities remain almost constant for shorter time separations of the double pulse, whereas the probe diffraction intensities decreased after 20 fs following pump pulse irradiation due to the X-ray–induced atomic displacement. This result indicates that sub-10-fs XFEL pulses enable conductions of damageless structural determinations and supports the validity of the theoretical predictions of ultraintense X-ray–matter interactions. The X-ray pump–probe scheme demonstrated here would be effective for understanding ultraintense X-ray–matter interactions, which will greatly stimulate advanced XFEL applications, such as atomic structure determination of a single molecule and generation of exotic matters with high energy densities. PMID:26811449

Observation of the strain field near the Si(111) 7 x 7 surface with a new X-ray diffraction technique.

PubMed

Emoto, T; Akimoto, K; Ichimiya, A

1998-05-01

A new X-ray diffraction technique has been developed in order to measure the strain field near a solid surface under ultrahigh vacuum (UHV) conditions. The X-ray optics use an extremely asymmetric Bragg-case bulk reflection. The glancing angle of the X-rays can be set near the critical angle of total reflection by tuning the X-ray energy. Using this technique, rocking curves for Si surfaces with different surface structures, i.e. a native oxide surface, a slightly oxide surface and an Si(111) 7 x 7 surface, were measured. It was found that the widths of the rocking curves depend on the surface structures. This technique is efficient in distinguishing the strain field corresponding to each surface structure.

X-ray scanning of overhead aurorae from rockets

NASA Technical Reports Server (NTRS)

Barcus, J. R.; Goldberg, R. A.; Gesell, L. H.

1981-01-01

Two Nike Tomahawk rocket payloads were launched into energetic auroral events in September, 1976 to investigate the structure of these events, as well as their effects on the atmosphere. X-ray scintillation detectors with energy discrimination in four ranges were used to measure the deposition of bremsstrahlung produced X-rays within the stratosphere and mesosphere. Iterative computer techniques were used to reconstruct X-ray source maps at 100 km, taking atmospheric absorption effects into account. Payload 18.178 was launched on September 21st into an aurora having two distinct azimuthal regions of optical brightness. The X-ray scanner detected the same features, and overlays of the X-ray source maps on all-sky photographs showed spatial coincidence of the X-ray with optical features at the lower energies (below 40 keV). Payload 18.179 was launched September 23rd into an aurora with a more diffuse character. The optical structure did not coincide as well with the measured X-ray structure. There was also an indication of a two-component spectrum for each event, with the hard component originating in the more diffuse, optically faint regions.

Crystal structure, molecular docking, and biological activity of the zinc complexes with 2-thenoyltrifluoroacetone and N-donor heterocyclic ligands

NASA Astrophysics Data System (ADS)

Eshaghi Malekshah, Rahime; Salehi, Mehdi; Kubicki, Maciej; Khaleghian, Ali

2017-12-01

Two novel mononuclear complexes, [Zn (TTA) (bipy)Cl] (1) and [Zn (TTA) (phen)Cl] (2) (TTA = 4,4,4-Trifluoro-1-(2-furyl)-1,3-butanedione, phen = 1,10-phenanthroline and bipy 2, 2ʹ-bipyridine), were synthesized and fully characterized by elemental analyses, 1H NMR, UV-Vis, FTIR spectroscopy, and conductivity measurements. The crystal structures of these two mono-nuclear zinc (II) complexes were determined by X-ray single-crystal diffraction. The result of X-ray diffraction analyses revealed that both complexes have distorted tetragonal-pyramid structures. In MTT cytotoxicity studies, these Zn (II) complexes exhibited antitumor activity against MCF-7 and MKN-45 cell lines. It was also found that the proliferation rate of MCF-7 and MKN-45 cells decreased after treatment with the above-mentioned complexes. In addition, the apoptosis-inducing activity was assessed by AO/EB (Acridine Orange/Ethidium bromide) staining assay and found that they have the potential to act as effective metal-based anticancer drugs. Finally, the molecular docking studies showed that complex 2 strongly binds through minor groove with DNA by relative binding energy -7.33 kcal mol-1.

X-ray crystallography over the past decade for novel drug discovery – where are we heading next?

PubMed Central

Zheng, Heping; Handing, Katarzyna B; Zimmerman, Matthew D; Shabalin, Ivan G; Almo, Steven C; Minor, Wladek

2015-01-01

Introduction Macromolecular X-ray crystallography has been the primary methodology for determining the three-dimensional structures of proteins, nucleic acids and viruses. Structural information has paved the way for structure-guided drug discovery and laid the foundations for structural bioinformatics. However, X-ray crystallography still has a few fundamental limitations, some of which may be overcome and complemented using emerging methods and technologies in other areas of structural biology. Areas covered This review describes how structural knowledge gained from X-ray crystallography has been used to advance other biophysical methods for structure determination (and vice versa). This article also covers current practices for integrating data generated by other biochemical and biophysical methods with those obtained from X-ray crystallography. Finally, the authors articulate their vision about how a combination of structural and biochemical/biophysical methods may improve our understanding of biological processes and interactions. Expert opinion X-ray crystallography has been, and will continue to serve as, the central source of experimental structural biology data used in the discovery of new drugs. However, other structural biology techniques are useful not only to overcome the major limitation of X-ray crystallography, but also to provide complementary structural data that is useful in drug discovery. The use of recent advancements in biochemical, spectroscopy and bioinformatics methods may revolutionize drug discovery, albeit only when these data are combined and analyzed with effective data management systems. Accurate and complete data management is crucial for developing experimental procedures that are robust and reproducible. PMID:26177814

Cleaning up the Legacy of the Cold War: Plutonium Oxides and the Role of Synchrotron Radiation Research

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, David Lewis

2015-01-21

The deceptively simple binary formula of AnO 2 belies an incredibly complex structural nature, and propensity to form mixed-valent, nonstoichiometric phases of composition AnO 2±x. For plutonium, the very formation of PuO 2+x has challenged a long-established dogma, and raised fundamental questions for long-term storage and environmental migration. This presentation covers two aspects of Los Alamos synchrotron radiation studies of plutonium oxides: (1) the structural chemistry of laboratory-prepared AnO 2+x systems (An = U, Pu; 0 ≤ x ≤ 0.25) determined through a combination of x-ray absorption fine structure spectroscopy (XAFS) and x-ray scattering of laboratory prepared samples; and (2)more » the application of synchrotron radiation towards the decontamination and decommissioning of the Rocky Flats Environmental Technology Site. Making the case for particle transport mechanisms as the basis of plutonium and americium mobility, rather than aqueous sorption-desorption processes, established a successful scientific basis for the dominance of physical transport processes by wind and water. The scientific basis was successful because it was in agreement with general theory on insolubility of PuO 2 in oxidation state IV, results of ultrafiltration analyses of field water/sediment samples, XAFS analyses of soil, sediment, and concrete samples, and was also in general agreement with on-site monitoring data. This understanding allowed Site contractors to rapidly move to application of soil erosion and sediment transport models as the means of predicting plutonium and americium transport, which led to design and application of site-wide soil erosion control technology to help control downstream concentrations of plutonium and americium in streamflow.« less

Intricate Short-Range Ordering and Strongly Anisotropic Transport Properties of Li 1–x Sn 2+x As 2

DOE PAGES

Lee, Kathleen; Kaseman, Derrick; Sen, Sabyasachi; ...

2015-02-22

A new ternary compound, Li 1-xSn 2+xAs 2, 0.2 < x < 0.4, was synthesized via solid-state reaction of elements. The compound crystallizes in a layered structure in the Rmore » $$\\overline{3}m$$ space group (No. 166) with Sn-As layers separated by layers of jointly occupied Li/Sn. The Sn-As layers are comprised of Sn 3As 3 puckered hexagons in a chair conformation that share all edges. Li/Sn atoms in the interlayer space are surrounded by a regular As 6 octahedron. Thorough investigations by synchrotron x-ray and neutron powder diffraction indicate no long-range Li/Sn ordering. In contrast, local Sn/Li ordering was revealed by synergistic investigations via solid-state 6,7Li NMR spectroscopy, HR-TEM, and neutron and X-ray pair distribution function analyses. Due to their different chemical natures, Li and Sn atoms tend to segregate into Li-rich and Sn-rich regions creating substantial inhomogeneity on the nanoscale. Inhomogeneous local structure has high impact on the physical properties of the synthesized compounds: local Li/Sn ordering and multiple nanoscale interfaces result in unexpectedly low thermal conductivity and highly anisotropic resistivity in Li 1-xSn 2+xAs 2.« less

Eleven years of monitoring the Seyfert 1 Mrk 335 with Swift: Characterizing the X-ray and UV/optical variability

NASA Astrophysics Data System (ADS)

Gallo, L. C.; Blue, D. M.; Grupe, D.; Komossa, S.; Wilkins, D. R.

2018-05-01

The narrow-line Seyfert 1 galaxy (NLS1) Mrk 335 has been continuously monitored with Swift since May 2007 when it fell into a long-lasting, X-ray low-flux interval. Results from the nearly 11 years of monitoring are presented here. Structure functions are used to measure the UV-optical and X-ray power spectra. The X-ray structure function measured between 10 - 100 days is consistent with the flat, low-frequency part of the power spectrum measured previously in Mrk 335. The UV-optical structure functions of Mrk 335 are comparable with those of other Seyfert 1 galaxies and of Mrk 335 itself when it was in a normal bright state. There is no indication that the current X-ray low-flux state is attributed to changes in the accretion disc structure of Mrk 335. The characteristic timescales measured in the structure functions can be attributed to thermal (for the UV) and dynamic (for the optical) timescales in a standard accretion disc. The high-quality UVW2 (˜1800 Å in the source frame) structure function appears to have two breaks and two different slopes between 10 - 160 days. Correlations between the X-ray and other bands are not highly significant when considering the entire 11-year light curves, but more significant behaviour is present when considering segments of the light curves. A correlation between the X-ray and UVW2 in 2014 (Year-8) may be predominately caused by an giant X-ray flare that was interpreted as jet-like emission. In 2008 (Year-2), possible lags between the UVW2 emission and other UV-optical waveband may be consistent with reprocessing of X-ray or UV emission in the accretion disc.

DOE Office of Scientific and Technical Information (OSTI.GOV)

McCormac, Kathleen; Byrd, Ian; Brannen, Rodney

We prepared highly porous Si/TiO 2 composite nanofibres using a unique sulphur-templating method combined with electrospinning. The structure, morphology, surface area, phase and composition of these nanofibres were characterized using Raman spectroscopy, scanning electron microscopy, powder X-ray diffraction, surface area analyser and thermogravimetric analyser. The specific surface area of Si/TiO 2 porous NFs is as large as 387m 2g -1, whose silicon capacity can be maintained above 1580mAhg -1 in 180 cycles.

Hirshfeld surface analyses and crystal structures of supramolecular self-assembly thiourea derivatives directed by non-covalent interactions

NASA Astrophysics Data System (ADS)

Gumus, Ilkay; Solmaz, Ummuhan; Binzet, Gun; Keskin, Ebru; Arslan, Birdal; Arslan, Hakan

2018-04-01

The novel N-(bis(3,5-dimethoxybenzyl)carbamothioyl)-4-R-benzamide (R: H, Cl, CH3 and OCH3) compounds have been synthesized and characterized by FT-IR, 1H NMR and 13C NMR spectroscopy. Their crystal structures were also determined by single-crystal X-ray diffraction studies. Hirshfeld surfaces analysis and their associated two dimensional fingerprint plots of compounds were used as theoretical approach to assess driving force for crystal structure formation via the intermolecular interactions in the crystal lattices of synthesized compounds. The study of X-ray single crystal diffraction and Hirshfeld surfaces analysis of the prepared compounds shows that hydrogen bonding and other weaker interactions such as Nsbnd H⋯S, weak Csbnd H⋯S, Csbnd H⋯O, Csbnd H⋯N and Csbnd H···π intermolecular interactions and π-π stacking, among molecules of synthesized compounds participate in a cooperative way to stabilize the supramolecular structures.

Structural properties of ultrafine Ba-hexaferrite nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Makovec, Darko, E-mail: Darko.Makovec@ijs.si; Primc, Darinka; Sturm, Saso

2012-12-15

Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was studied using X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDXS), X-ray absorption fine structure (XAFS), and Moessbauer spectroscopy (MS), to be compared to the structure of larger nanoparticles and the bulk. The nanoparticles were synthesized with hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH{sup -}. The ultrafine nanoparticles were formed in a discoid shape, {approx}10 nm wide and only {approx}3 nm thick, comparable to the size of the hexagonal unit cell in the c-direction.more » The HRTEM image analysis confirmed the hexaferrite structure, whereas EDXS showed the composition matching the BaFe{sub 12}O{sub 19} formula. XAFS and MS analyses showed considerable disorder of the structure, most probably responsible for the low magnetization. - Graphical abstract: Left: HREM image of an ultrafine Ba-hexaferrite nanoparticle (inset: TEM image of the nanoparticles); Right: the experimental HRTEM image is compared with calculated image and corresponding atomic model. Highlights: Black-Right-Pointing-Pointer Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was compared to the structure of the bulk. Black-Right-Pointing-Pointer Thickness the discoid nanoparticles was comparable to the size of the hexagonal unit cell in the c-direction. Black-Right-Pointing-Pointer Considerable disorder of the nanoparticles' structure is most probably responsible for their low magnetization.« less

Fault-related structural permeability: Qualitative insights of the damage-zone from micro-CT analysis.

NASA Astrophysics Data System (ADS)

Gomila, Rodrigo; Arancibia, Gloria; Nehler, Mathias; Bracke, Rolf; Stöckhert, Ferdinand

2016-04-01

Fault zones and their related structural permeability play a leading role in the migration of fluids through the continental crust. A first approximation to understanding the structural permeability conditions, and the estimation of its hydraulic properties (i.e. palaeopermeability and fracture porosity conditions) of the fault-related fracture mesh is the 2D analysis of its veinlets, usually made in thin-section. Those estimations are based in the geometrical parameters of the veinlets, such as average fracture density, length and aperture, which can be statistically modelled assuming penny-shaped fractures of constant radius and aperture within an anisotropic fracture system. Thus, this model is related to fracture connectivity, its length and to the cube of the fracture apertures. In this way, the estimated values presents their own inaccuracies owing to the method used. Therefore, the study of the real spatial distribution of the veinlets of the fault-related fracture mesh (3D), feasible with the use of micro-CT analyses, is a first order factor to unravel both, the real structural permeability conditions of a fault-zone, together with the validation of previous estimations made in 2D analyses in thin-sections. This early contribution shows the preliminary results of a fault-related fracture mesh and its 3D spatial distribution in the damage zone of the Jorgillo Fault (JF), an ancient subvertical left-lateral strike-slip fault exposed in the Atacama Fault System in northern Chile. The JF is a ca. 20 km long NNW-striking strike-slip fault with sinistral displacement of ca. 4 km. The methodology consisted of the drilling of vertically oriented plugs of 5 mm in diameter located at different distances from the JF core - damage zone boundary. Each specimen was, then, scanned with an x-ray micro-CT scanner (ProCon X-Ray CTalpha) in order to assess the fracture mesh. X-rays were generated in a transmission target x-ray tube with acceleration voltages ranging from 90-120 kV and target currents from 40-60 μA. The focal spot size on the diamond/tungsten target was about 5 μm. The x-ray beam was filtered using a 1 mm Aluminum plate before passing the sample. 1200 x-ray images were taken during a full rotation of the sample using an amorphous silicon flat panel detector with 1516x1900 pixels. This resulted in a voxel resolution of about 8 μm in the 3D data reconstructed from the images. Future work will be aimed in the images segmentation of the fault-related fracture mesh followed by the estimation of its hydraulic properties at the time of fracture sealing. Acknowledgements: This work is a contribution to the CONICYT- BMBF International Scientific Collaborative Research Program Project PCCI130025/FKZ01DN14033 and the FONDAP-CONICYT Project 15090013.

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Small Angle X-ray Scattering for Nanoparticle Research

DOE PAGES

Li, Tao; Senesi, Andrew J.; Lee, Byeongdu

2016-04-07

X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and ångström length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle’s size, size distribution,more » shape, and organization into hierarchal structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well the combination of SAXS with other X-ray and non-X ray characterization tools. Furthermore, we conclude with an examination of several key areas of research where X-rays scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and in operando studies of catalysts and energy storage materials. Throughout this review we highlight the unique capabilities of X-ray scattering for structural characterization of materials in their native environment.« less

Small Angle X-ray Scattering for Nanoparticle Research

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Tao; Senesi, Andrew J.; Lee, Byeongdu

X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and ångström length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle’s size, size distribution,more » shape, and organization into hierarchal structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well the combination of SAXS with other X-ray and non-X ray characterization tools. Furthermore, we conclude with an examination of several key areas of research where X-rays scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and in operando studies of catalysts and energy storage materials. Throughout this review we highlight the unique capabilities of X-ray scattering for structural characterization of materials in their native environment.« less

Radio and X-ray structure of Centaurus A

NASA Technical Reports Server (NTRS)

Feigelson, E. D.

1982-01-01

Recent studies of the nearby radio galaxy Centaurus A with the Very Large Array and the Einstein X-Ray Observatory reveal complex radio and X-ray structures. A prominent one-sided jet comprised of resolved knots located 0.2-6 kpc from the nucleus is seen in both radio and X-rays. The X-ray emission is probably synchrotron, requiring in situ reacceleration up to about ten million. Inverse Compton emission is not a likely explanation though a thermal model in which the nucleus ejects dense 100,000 solar mass clouds cannot be excluded. An elongated X-ray region is also found near the 'middle' radio lobe and optical HII regions about 30 kpc NE of the nucleus. Conditions around the active nucleus, the absence of X-rays from the inner radio lobes, and X-ray evidence for a hot interstellar medium are briefly discussed

Structure of the Archaeoglobus fulgidus orphan ORF AF1382 determined by sulfur SAD from a moderately diffracting crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Jin-Yi; Fu, Zheng-Qing; Argonne National Laboratory, Argonne, Illinois

2012-09-01

The crystal structure of the 11.14 kDa orphan ORF 1382 from Archaeoglobus fulgidus (AF1382) has been determined by sulfur SAD phasing using data collected from a moderately diffracting crystal and 1.9 Å synchrotron X-rays. The crystal structure of the 11.14 kDa orphan ORF 1382 from Archaeoglobus fulgidus (AF1382) has been determined by sulfur SAD phasing using a moderately diffracting crystal and 1.9 Å wavelength synchrotron X-rays. AF1382 was selected as a structural genomics target by the Southeast Collaboratory for Structural Genomics (SECSG) since sequence analyses showed that it did not belong to the Pfam-A database and thus could represent amore » novel fold. The structure was determined by exploiting longer wavelength X-rays and data redundancy to increase the anomalous signal in the data. AF1382 is a 95-residue protein containing five S atoms associated with four methionine residues and a single cysteine residue that yields a calculated Bijvoet ratio (ΔF{sub anom}/F) of 1.39% for 1.9 Å wavelength X-rays. Coupled with an average Bijvoet redundancy of 25 (two 360° data sets), this produced an excellent electron-density map that allowed 69 of the 95 residues to be automatically fitted. The S-SAD model was then manually completed and refined (R = 23.2%, R{sub free} = 26.8%) to 2.3 Å resolution. High-resolution data were subsequently collected from a better diffracting crystal using 0.97 Å wavelength synchrotron X-rays and the S-SAD model was refined (R = 17.9%, R{sub free} = 21.4%) to 1.85 Å resolution. AF1382 has a winged-helix–turn–helix structure common to many DNA-binding proteins and most closely resembles the N-terminal domain (residues 1–82) of the Rio2 kinase from A. fulgidus, which has been shown to bind DNA, and a number of MarR-family transcriptional regulators, suggesting a similar DNA-binding function for AF1382. The analysis also points out the advantage gained from carrying out data reduction and structure determination on-site while the crystal is still available for further data collection.« less

VO2 Thermochromic Films on Quartz Glass Substrate Grown by RF-Plasma-Assisted Oxide Molecular Beam Epitaxy

PubMed Central

Zhang, Dong; Sun, Hong-Jun; Wang, Min-Huan; Miao, Li-Hua; Liu, Hong-Zhu; Zhang, Yu-Zhi; Bian, Ji-Ming

2017-01-01

Vanadium dioxide (VO2) thermochromic thin films with various thicknesses were grown on quartz glass substrates by radio frequency (RF)-plasma assisted oxide molecular beam epitaxy (O-MBE). The crystal structure, morphology and chemical stoichiometry were investigated systemically by X-ray diffraction (XRD), atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) analyses. An excellent reversible metal-to-insulator transition (MIT) characteristics accompanied by an abrupt change in both electrical resistivity and optical infrared (IR) transmittance was observed from the optimized sample. Remarkably, the transition temperature (TMIT) deduced from the resistivity-temperature curve was reasonably consistent with that obtained from the temperature-dependent IR transmittance. Based on Raman measurement and XPS analyses, the observations were interpreted in terms of residual stresses and chemical stoichiometry. This achievement will be of great benefit for practical application of VO2-based smart windows. PMID:28772673

Characterization of D-glucaric acid using NMR, x-ray crystal structure, and MM3 molecular modeling analyses

USDA-ARS?s Scientific Manuscript database

D-glucaric acid was characterized in solution by comparing NMR spectra from the isotopically unlabeled molecule with those from D-glucaric acid labeled with deuterium or carbon-13 atoms. The NMR studies provided unequivocal assignments for all carbon atoms and non-hydroxyl protons of the molecule. ...

Kaolinite flocculation induced by smectite addition - a transmission X-ray microscopic study.

PubMed

Zbik, Marek S; Song, Yen-Fang; Frost, Ray L

2010-09-01

The influence of smectite addition on kaolinite suspensions in water was investigated by transmission X-ray microscopy (TXM) and Scanning Electron Microscopy (SEM). Sedimentation test screening was also conducted. Micrographs were processed by the STatistic IMage Analysing (STIMAN) program and structural parameters were calculated. From the results of the sedimentation tests important influences of small smectite additions to about 3wt.% on kaolinite suspension flocculation has been found. In order to determine the reason for this smectite impact on kaolinite suspension, macroscopic behaviour micro-structural examination using Transmission X-ray Microscope (TXM) and SEM has been undertaken. TXM & SEM micrographs of freeze-dried kaolinite-smectite suspensions with up to 20% smectite showed a high degree of orientation of the fabric made of highly oriented particles and greatest density when 3wt.% of smectite was added to the 10wt.% dense kaolinite suspension. In contrast, suspensions containing pure kaolinite do not show such platelet mutual orientation but homogenous network of randomly oriented kaolinite platelets. This suggests that in kaolinite-smectite suspensions, smectite forms highly oriented basic framework into which kaolinite platelets may bond in face to face preferential contacts strengthening structure and allowing them to show plastic behaviour which is cause of platelets orientation. Copyright 2010 Elsevier Inc. All rights reserved.

Syntheses, structural characterization, and DPPH radical scavenging activity of cocrystals of caffeine with 1- and 2-naphthoxyacetic acids

NASA Astrophysics Data System (ADS)

Suresh Kumar, G. S.; Seethalakshmi, P. G.; Sumathi, D.; Bhuvanesh, N.; Kumaresan, S.

2013-03-01

Caffeine:1-naphthoxyacetic acid [(caf)(1-naa)] and caffeine:2-naphthoxyacetic acid [(caf)(2-naa)] cocrystals have been synthesized and single crystals were grown by slow evaporation technique. The structures of the grown crystals were elucidated using single crystal X-ray diffraction analysis. Both the cocrystals belong to the monoclinic crystallographic system with space group P21/c, Z = 4, and α = γ = 90°, whereas β = 111.4244(18)° for [(caf)(1-naa)] and β = 109.281(6)° for [(caf)(2-naa)]. The crystal packing is predominantly stabilized by hydrogen bonding and π-π stacking interactions. The presence of unionized -COOH functional group in both the cocrystals was identified by FTIR spectral analysis. Thermal behavior and stability of both the cocrystals were studied by TGA/DTA analyses. Solvent-free formation of these cocrystals was confirmed by powder X-ray diffraction analyses. The theoretical energy of cocrystals showed that the formers have higher energy than cocrystals 1 and 2. DPPH radical scavenging activity of cocrystals 1 and 2 is slightly greater than the formers.

Crystal growth, structural, optical, spectral and thermal studies of tris( L-phenylalanine) L-phenylalaninium nitrate: A new organic nonlinear optical material

NASA Astrophysics Data System (ADS)

Prakash, M.; Geetha, D.; Lydia Caroline, M.

2011-10-01

Tris( L-phenylalanine) L-phenylalaninium nitrate, C 9H 12NO 2+·NO 3-·3C 9H 11NO 2 (TPLPN), a new organic nonlinear optical material was grown from aqueous solution by slow evaporation solution growth at room temperature. The grown crystals were subjected to powder X-ray diffraction and single crystal X-ray diffraction studies to confirm the crystalline nature and crystal structure. The modes of vibration of different molecular groups present in TPLPN have been identified by FTIR spectral analysis. The presence of hydrogen and carbon in the grown crystal were confirmed by using proton and carbon nuclear magnetic resonance (NMR) spectral analyses. The optical transmission spectral study establishes good transmitting ability of the crystal in the entire visible region. The thermogravimetric (TG) and differential thermal analyses (DTA) were carried out to understand the thermal stability of the sample. The nonlinear optical property of the compound observed using Kurtz powder second harmonic generation test assets the suitability of the grown material for the frequency conversion of laser radiation of Nd:YAG.

Effect of Fe-substitution on the structure and magnetism of single crystals Mn2-xFexBO4

NASA Astrophysics Data System (ADS)

Platunov, M. S.; Kazak, N. V.; Knyazev, Yu. V.; Bezmaternykh, L. N.; Moshkina, E. M.; Trigub, A. L.; Veligzhanin, A. A.; Zubavichus, Y. V.; Solovyov, L. A.; Velikanov, D. A.; Ovchinnikov, S. G.

2017-10-01

Single crystalline Mn2-xFexBO4 with x = 0.3, 0.5, 0.7 grown by the flux method have been studied by means of X-ray diffraction and X-ray absorption spectroscopy at both Mn and Fe K edges. The compounds were found to crystallize in an orthorhombic warwickite structure (sp. gr. Pnam). The lattice parameters change linearly with x thus obeying the Vegard's law. The Fe3+ substitution for Mn3+ has been deduced from the X-ray absorption near-edge structure (XANES) spectra. Two energy positions of the absorption edges have been observed in Mn K-edge XANES spectra indicating the presence of manganese in two different oxidation states. Extended X-ray absorption fine structure (EXAFS) analysis has shown the reduction of local structural distortions upon Fe substitution. The magnetization data have revealed a spin-glass transition at TSG = 11, 14 and 18 K for x = 0.3, 0.5 and 0.7, respectively.

The origin of luminescence from di[4-(4-diphenylaminophenyl)phenyl]sulfone (DAPSF), a blue light emitter: an X-ray excited optical luminescence (XEOL) and X-ray absorption near edge structure (XANES) study.

PubMed

Zhang, Duo; Zhang, Hui; Zhang, Xiaohong; Sham, Tsun-Kong; Hu, Yongfeng; Sun, Xuhui

2016-03-07

The electronic structure and optical properties of di[4-(4-diphenylaminophenyl)phenyl]sulfone (denoted as DAPSF), a highly efficient fluorophor, have been investigated using X-ray excited optical luminescence (XEOL) and X-ray absorption near edge structure (XANES) spectroscopy at excitation energies across the C, N, O K-edges and the sulfur K-edge. The results indicate that the blue luminescence is mainly related to the sulfur functional group.

Opportunities and challenges for time-resolved studies of protein structural dynamics at X-ray free-electron lasers.

PubMed

Neutze, Richard

2014-07-17

X-ray free-electron lasers (XFELs) are revolutionary X-ray sources. Their time structure, providing X-ray pulses of a few tens of femtoseconds in duration; and their extreme peak brilliance, delivering approximately 10(12) X-ray photons per pulse and facilitating sub-micrometre focusing, distinguish XFEL sources from synchrotron radiation. In this opinion piece, I argue that these properties of XFEL radiation will facilitate new discoveries in life science. I reason that time-resolved serial femtosecond crystallography and time-resolved wide angle X-ray scattering are promising areas of scientific investigation that will be advanced by XFEL capabilities, allowing new scientific questions to be addressed that are not accessible using established methods at storage ring facilities. These questions include visualizing ultrafast protein structural dynamics on the femtosecond to picosecond time-scale, as well as time-resolved diffraction studies of non-cyclic reactions. I argue that these emerging opportunities will stimulate a renaissance of interest in time-resolved structural biochemistry.

Effect of Pressure on Valence and Structural Properties of YbFe 2 Ge 2 Heavy Fermion Compound—A Combined Inelastic X-ray Spectroscopy, X-ray Diffraction, and Theoretical Investigation

DOE PAGES

Kumar, Ravhi S.; Svane, Axel; Vaitheeswaran, Ganapathy; ...

2015-10-19

We measured the crystal structure and the Yb valence of the YbFe 2Ge 2 heavy fermion compound at room temperature and under high pressures using high-pressure powder X-ray diffraction and X-ray absorption spectroscopy via both partial fluorescence yield and resonant inelastic X-ray emission techniques. Moreover, the measurements are complemented by first-principles density functional theoretical calculations using the self-interaction corrected local spin density approximation investigating in particular the magnetic structure and the Yb valence. Finally, while the ThCr 2Si 2-type tetragonal (I4/mmm) structure is stable up to 53 GPa, the X-ray emission results show an increase of the Yb valence frommore » v = 2.72(2) at ambient pressure to v = 2.93(3) at ~9 GPa, where at low temperature a pressure-induced quantum critical state was reported.« less

Calibration of X-Ray diffractometer by the experimental comparison method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dudka, A. P., E-mail: dudka@ns.crys.ras.ru

2015-07-15

A software for calibrating an X-ray diffractometer with area detector has been developed. It is proposed to search for detector and goniometer calibration models whose parameters are reproduced in a series of measurements on a reference crystal. Reference (standard) crystals are prepared during the investigation; they should provide the agreement of structural models in repeated analyses. The technique developed has been used to calibrate Xcalibur Sapphire and Eos, Gemini Ruby (Agilent) and Apex x8 and Apex Duo (Bruker) diffractometers. The main conclusions are as follows: the calibration maps are stable for several years and can be used to improve structuralmore » results, verified CCD detectors exhibit significant inhomogeneity of the efficiency (response) function, and a Bruker goniometer introduces smaller distortions than an Agilent goniometer.« less

Direct Synthesis of Novel and Reactive Sulfide-modified Nano Iron through Nanoparticle Seeding for Improved Cadmium-Contaminated Water Treatment

PubMed Central

Su, Yiming; Adeleye, Adeyemi S.; Huang, Yuxiong; Zhou, Xuefei; Keller, Arturo A.; Zhang, Yalei

2016-01-01

Magnetic sulfide-modified nanoscale zerovalent iron (S-nZVI) is of great technical and scientific interest because of its promising application in groundwater remediation, although its synthesis is still a challenge. We develop a new nanoparticle seeding method to obtain a novel and reactive nanohybrid, which contains an Fe(0) core covered by a highly sulfidized layer under high extent of sulfidation. Syntheses monitoring experiments show that seeding accelerates the reduction rate from Fe2+ to Fe0 by 19%. X-ray adsorption near edge structure (XANES) spectroscopy and extended X-ray absorption fine structure analyses demonstrate the hexahedral Fe-Fe bond (2.45 and 2.83 Å) formation through breaking down of the 1.99 Å Fe-O bond both in crystalline and amorphous iron oxide. The XANES analysis also shows 24.2% (wt%) of FeS with bond length of 2.4 Å in final nanohybrid. Both X-ray diffraction and Mössbauer analyses further confirm that increased nanoparticle seeding results in formation of more Fe0 crystals. Nano-SiO2 seeding brings down the size of single Fe0 grain from 32.4 nm to 18.7 nm, enhances final Fe0 content from 5.9% to 55.6%, and increases magnetization from 4.7 to 65.5 emu/g. The synthesized nanohybrid has high cadmium removal capacity and holds promising prospects for treatment of metal-contaminated water. PMID:27095387

Direct Synthesis of Novel and Reactive Sulfide-modified Nano Iron through Nanoparticle Seeding for Improved Cadmium-Contaminated Water Treatment

NASA Astrophysics Data System (ADS)

Su, Yiming; Adeleye, Adeyemi S.; Huang, Yuxiong; Zhou, Xuefei; Keller, Arturo A.; Zhang, Yalei

2016-04-01

Magnetic sulfide-modified nanoscale zerovalent iron (S-nZVI) is of great technical and scientific interest because of its promising application in groundwater remediation, although its synthesis is still a challenge. We develop a new nanoparticle seeding method to obtain a novel and reactive nanohybrid, which contains an Fe(0) core covered by a highly sulfidized layer under high extent of sulfidation. Syntheses monitoring experiments show that seeding accelerates the reduction rate from Fe2+ to Fe0 by 19%. X-ray adsorption near edge structure (XANES) spectroscopy and extended X-ray absorption fine structure analyses demonstrate the hexahedral Fe-Fe bond (2.45 and 2.83 Å) formation through breaking down of the 1.99 Å Fe-O bond both in crystalline and amorphous iron oxide. The XANES analysis also shows 24.2% (wt%) of FeS with bond length of 2.4 Å in final nanohybrid. Both X-ray diffraction and Mössbauer analyses further confirm that increased nanoparticle seeding results in formation of more Fe0 crystals. Nano-SiO2 seeding brings down the size of single Fe0 grain from 32.4 nm to 18.7 nm, enhances final Fe0 content from 5.9% to 55.6%, and increases magnetization from 4.7 to 65.5 emu/g. The synthesized nanohybrid has high cadmium removal capacity and holds promising prospects for treatment of metal-contaminated water.

Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

DOE PAGES

Kern, Jan; Yachandra, Vittal K.; Yano, Junko

2015-09-02

We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kern, Jan; Yachandra, Vittal K.; Yano, Junko

We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

X-ray free electron laser: opportunities for drug discovery.

PubMed

Cheng, Robert K Y; Abela, Rafael; Hennig, Michael

2017-11-08

Past decades have shown the impact of structural information derived from complexes of drug candidates with their protein targets to facilitate the discovery of safe and effective medicines. Despite recent developments in single particle cryo-electron microscopy, X-ray crystallography has been the main method to derive structural information. The unique properties of X-ray free electron laser (XFEL) with unmet peak brilliance and beam focus allow X-ray diffraction data recording and successful structure determination from smaller and weaker diffracting crystals shortening timelines in crystal optimization. To further capitalize on the XFEL advantage, innovations in crystal sample delivery for the X-ray experiment, data collection and processing methods are required. This development was a key contributor to serial crystallography allowing structure determination at room temperature yielding physiologically more relevant structures. Adding the time resolution provided by the femtosecond X-ray pulse will enable monitoring and capturing of dynamic processes of ligand binding and associated conformational changes with great impact to the design of candidate drug compounds. © 2017 The Author(s). Published by Portland Press Limited on behalf of the Biochemical Society.

Oligomeric domain structure of human complement factor H by X-ray and neutron solution scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Perkins, S.J.; Nealis, A.S.; Sim, R.B.

1991-03-19

Factor H is a regulatory component of the complement system. It has a monomer M{sub r} of 150,000. Primary structure analysis shows that the polypeptide is divided into 20 homologous regions, each 60 amino acid residues long. These are independently folding domains and are termed short consensus repeats (SCRs) or complement control protein (CCP) repeats. High-flux synchrotron x-ray and neutron scatteriing studies were performed in order to define its solution structure in conditions close to physiological. The M{sub r} of factor H was determined as 250,000-320,000 to show that factor H is dimeric. The radius of gyration R{sub G} ofmore » native factor H by X-rays or by neutrons in 0% or 100% {sup 2}H{sub 2}O buffers is not measurable but is greater than 12.5 nm. Two cross-sectional radii of gyration R{sub XS-1} and R{sub XS-2} were determined as 3.0-3.1 and 1.8 nm, respectively. Analyses of the cross-sectional intensities show that factor H is composed of two distinct subunits. This model corresponds to an actual R{sub G} fo 21-23 nm. The separation between each SCR/CCP in factor H is close to 4 nm. In the solution structure of factor H, the SCR/CCP domains are in a highly extended conformation.« less

Chromium immobilization by extra- and intraradical fungal structures of arbuscular mycorrhizal symbioses.

PubMed

Wu, Songlin; Zhang, Xin; Sun, Yuqing; Wu, Zhaoxiang; Li, Tao; Hu, Yajun; Lv, Jitao; Li, Gang; Zhang, Zhensong; Zhang, Jing; Zheng, Lirong; Zhen, Xiangjun; Chen, Baodong

2016-10-05

Arbuscular mycorrhizal (AM) fungi can enhance plant Cr tolerance through immobilizing Cr in mycorrhizal roots. However, the detailed processes and mechanisms are unclear. The present study focused on cellular distribution and speciation of Cr in both extraradical mycelium (ERM) and mycorrhizal roots exposed to Cr(VI) by using field emission scanning electron microscopy equipped with energy dispersive X-ray spectrometer (FE-SEM-EDS), scanning transmission soft X-ray microscopy (STXM) and X-ray absorption fine structure (XAFS) spectroscopy techniques. We found that amounts of particles (possibly extracellular polymeric substances, EPS) were produced on the AM fungal surface upon Cr(VI) stress, which contributed greatly to Cr(VI) reduction and immobilization. With EDS of the surface of AM fungi exposed to various Cr(VI) levels, a positive correlation between Cr and P was revealed, suggesting that phosphate groups might act as counter ions of Cr(III), which was also confirmed by the XAFS analysis. Besides, STXM and XAFS analyses showed that Cr(VI) was reduced to Cr(III) in AM fungal structures (arbuscules, intraradical mycelium, etc.) and cell walls in mycorrhizal roots, and complexed possibly with carboxyl groups or histidine analogues. The present work provided evidence of Cr immobilization on fungal surface and in fungal structures in mycorrhizal roots at a cellular level, and thus unraveled the underlying mechanisms by which AM symbiosis immobilize Cr. Copyright © 2016 Elsevier B.V. All rights reserved.

Characterization of ceramic powders by an X-ray measuring method

NASA Technical Reports Server (NTRS)

Ziegler, B.

1983-01-01

X-ray line broadening analysis gives quantitative data on structural changes of ceramic powders after different processing steps. Various Al2O3 powders were investigated and the following points are discussed on the basis of these results: X-ray line broadening analysis, structural changes during grinding, structural changes during annealing, influence of structural properties on sintering behavior and application of line broadening analysis to quality control of powders.

X-ray Intermolecular Structure Factor (XISF): separation of intra- and intermolecular interactions from total X-ray scattering data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mou, Q.; Benmore, C. J.; Yarger, J. L.

2015-06-01

XISF is a MATLAB program developed to separate intermolecular structure factors from total X-ray scattering structure factors for molecular liquids and amorphous solids. The program is built on a trust-region-reflective optimization routine with the r.m.s. deviations of atoms physically constrained. XISF has been optimized for performance and can separate intermolecular structure factors of complex molecules.

X-ray Intermolecular Structure Factor ( XISF ): separation of intra- and intermolecular interactions from total X-ray scattering data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mou, Q.; Benmore, C. J.; Yarger, J. L.

2015-05-09

XISFis a MATLAB program developed to separate intermolecular structure factors from total X-ray scattering structure factors for molecular liquids and amorphous solids. The program is built on a trust-region-reflective optimization routine with the r.m.s. deviations of atoms physically constrained.XISFhas been optimized for performance and can separate intermolecular structure factors of complex molecules.

NAD+ administration significantly attenuates synchrotron radiation X-ray-induced DNA damage and structural alterations of rodent testes

PubMed Central

Sheng, Caibin; Chen, Heyu; Wang, Ban; Liu, Tengyuan; Hong, Yunyi; Shao, Jiaxiang; He, Xin; Ma, Yingxin; Nie, Hui; Liu, Na; Xia, Weiliang; Ying, Weihai

2012-01-01

Synchrotron radiation (SR) X-ray has great potential for its applications in medical imaging and cancer treatment. In order to apply SR X-ray in clinical settings, it is necessary to elucidate the mechanisms underlying the damaging effects of SR X-ray on normal tissues, and to search for the strategies to reduce the detrimental effects of SR X-ray on normal tissues. However, so far there has been little information on these topics. In this study we used the testes of rats as a model to characterize SR X-ray-induced tissue damage, and to test our hypothesis that NAD+ administration can prevent SR X-ray-induced injury of the testes. We first determined the effects of SR X-ray at the doses of 0, 0.5, 1.3, 4 and 40 Gy on the biochemical and structural properties of the testes one day after SR X-ray exposures. We found that 40 Gy of SR X-ray induced a massive increase in double-strand DNA damage, as assessed by both immunostaining and Western blot of phosphorylated H2AX levels, which was significantly decreased by intraperitoneally (i.p.) administered NAD+ at doses of 125 and 625 mg/kg. Forty Gy of SR X-ray can also induce marked increases in abnormal cell nuclei as well as significant decreases in the cell layers of the seminiferous tubules one day after SR X-ray exposures, which were also ameliorated by the NAD+ administration. In summary, our study has shown that SR X-ray can produce both molecular and structural alterations of the testes, which can be significantly attenuated by NAD+ administration. These results have provided not only the first evidence that SR X-ray-induced tissue damage can be ameliorated by certain approaches, but also a valuable basis for elucidating the mechanisms underlying SR X-ray-induced tissue injury. PMID:22518270

Synthesis and characterization of two new zinc(II) coordination polymers with bidentate flexible ligands: Formation of a 2D structure with (44.62)-sql topology

NASA Astrophysics Data System (ADS)

Lalegani, Arash; Khaledi Sardashti, Mohammad; Gajda, Roman; Woźniak, Krzysztof

2017-12-01

Zinc(II) coordination polymers [Zn(bip)2(NCS)2]n (1) and [Zn(μ-bbd)(N3)2]n (2) were synthesized by using the neutral flexible bidentate N-donor ligands 1,4-bis(3,5-dimethylpyrazolyl)butane (bbd) and 1,3-bis(imidazolyl)propane (bip), mono-anionic NCS- or N3-ligand and zinc(II) chloride salts. The results of the X-ray analyses demonstrate that in the structure of 1, the zinc(II) ion is located on an inversion center and exhibits an ZnN6 octahedral arrangement while, in the structure of 2, the zinc(II) ion adopts an ZnN4 tetrahedral geometry. In the polymer 1, the NCS groups are terminally N-bonded to the metal center and the each bip with anti-gauche conformation acts as bridging connecting four zinc(II) ions to form a two-dimensional network with a sql [point symbol (44.62)] topology while, in the polymer 1, the N3 groups are terminally bonded to the metal center and each bbd with anti-anti-anti conformation acts as bridging ligand connecting two zinc(II) ions to form a one-dimensional zig-zag chain. Coordination compounds 1 and 2 have been characterized by infrared spectroscopy, elemental analyses and single-crystal X-ray diffraction. Thermal analyses of polymers were also presented.

Discovery of novel inhibitors for DHODH via virtual screening and X-ray crystallographic structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

McLean, Larry R.; Zhang, Ying; Degnen, William

2010-10-28

Amino-benzoic acid derivatives 1-4 were found to be inhibitors for DHODH by virtual screening, biochemical, and X-ray crystallographic studies. X-ray structures showed that 1 and 2 bind to DHODH as predicted by virtual screening, but 3 and 4 were found to be structurally different from the corresponding compounds initially identified by virtual screening.

X-PEEM, XPS and ToF-SIMS characterisation of xanthate induced chalcopyrite flotation: Effect of pulp potential

NASA Astrophysics Data System (ADS)

Kalegowda, Yogesh; Chan, Yuet-Loy; Wei, Der-Hsin; Harmer, Sarah L.

2015-05-01

Synchrotron-based X-ray photoemission electron microscopy (X-PEEM), X-ray photo-electron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and ultraviolet visible spectroscopy were used to characterize the flotation behaviour of chalcopyrite with xanthate at different processing conditions. The flotation recovery of chalcopyrite decreased from 97% under oxidative conditions (Eh ~ 385 mV SHE, pH 4) to 41% at a reductive potential of - 100 mV SHE (at pH 9). X-PEEM images constructed from the metal L3 absorption edges were used to produce near-edge X-ray absorption fine structure (NEXAFS) spectra from regions of interest, allowing the variability in mineral surface chemistry of each mineral particle to be analysed, and the effect of pulp potential (Eh) on the flotation of chalcopyrite to be determined. XPS, ToF-SIMS and NEXAFS analyses of chalcopyrite particles at oxidative conditions show that the surface was mildly oxidised and covered with adsorbed molecular CuEX. The Cu 2p XPS and Cu L2,3 NEXAFS spectra were dominated by CuI species attributed to bulk chalcopyrite and adsorbed CuEX. At a reductive potential of - 100 mV SHE, an increase in concentration of CuI and FeIII oxides and hydroxides was observed. X-PEEM analysis was able to show the presence of a low percentage of CuII oxides (CuO or Cu(OH)2) with predominantly CuI oxide (Cu2O) which is not evident in Cu 2p XPS spectra.

The surface structure of silver-coated gold nanocrystals and its influence on shape control

DOE PAGES

Padmos, J. Daniel; Personick, Michelle L.; Tang, Qing; ...

2015-07-08

Understanding the surface structure of metal nanocrystals with specific facet indices is important due to its impact on controlling nanocrystal shape and functionality. However, this is particularly challenging for halide-adsorbed nanocrystals due to the difficulty in analysing interactions between metals and light halides (for example, chloride). Here we uncover the surface structures of chloride-adsorbed, silver-coated gold nanocrystals with {111}, {110}, {310} and {720} indexed facets by X-ray absorption spectroscopy and density functional theory modelling. The silver–chloride, silver–silver and silver–gold bonding structures are markedly different between the nanocrystal surfaces, and are sensitive to their formation mechanism and facet type. A uniquemore » approach of combining the density functional theory and experimental/simulated X-ray spectroscopy further verifies the surface structure models and identifies the previously indistinguishable valence state of silver atoms on the nanocrystal surfaces. Overall, this work elucidates the thus-far unknown chloride–metal nanocrystal surface structures and sheds light onto the halide-induced growth mechanism of anisotropic nanocrystals.« less

Reconstitution of SNARE proteins into solid-supported lipid bilayer stacks and X-ray structure analysis.

PubMed

Xu, Yihui; Kuhlmann, Jan; Brennich, Martha; Komorowski, Karlo; Jahn, Reinhard; Steinem, Claudia; Salditt, Tim

2018-02-01

SNAREs are known as an important family of proteins mediating vesicle fusion. For various biophysical studies, they have been reconstituted into supported single bilayers via proteoliposome adsorption and rupture. In this study we extended this method to the reconstitution of SNAREs into supported multilamellar lipid membranes, i.e. oriented multibilayer stacks, as an ideal model system for X-ray structure analysis (X-ray reflectivity and diffraction). The reconstitution was implemented through a pathway of proteomicelle, proteoliposome and multibilayer. To monitor the structural evolution in each step, we used small-angle X-ray scattering for the proteomicelles and proteoliposomes, followed by X-ray reflectivity and grazing-incidence small-angle scattering for the multibilayers. Results show that SNAREs can be successfully reconstituted into supported multibilayers, with high enough orientational alignment for the application of surface sensitive X-ray characterizations. Based on this protocol, we then investigated the effect of SNAREs on the structure and phase diagram of the lipid membranes. Beyond this application, this reconstitution protocol could also be useful for X-ray analysis of many further membrane proteins. Copyright © 2017 Elsevier B.V. All rights reserved.

Magnetic resonance imaging analyses of varved marine sedimentary records of the Gulf of California

NASA Astrophysics Data System (ADS)

Briskin, Madeleine; Robins, Jon; Riedel, William R.; Booker, Ron

1986-08-01

Nuclear Magnetic Resonance Imaging used for the first time to analyze marine sedimentary records of the Gulf of California is a remarkable improvement over the more conventional X-ray technique in the identification of organic rich layers. Analytical results indicate that NMRI differentiates clearly between organic rich (light) and organic poor (dark) deposits. It also provides a fine resolution of sedimentary structures, laminae and stratigraphic subtleties. It may be made to yield a three-dimensional stratigraphy; the procedure is nondestructive. The organic vs. inorganic resolution provided by NMRI technology complemented by X-ray when needed should facilitate future studies of paleoceanographic, paleoclimatic and biogeochemical cycles recorded in the vast deposits of marine clays.

Sonochemical syntheses of a new nano-sized porous lead(II) coordination polymer as precursor for preparation of lead(II) oxide nanoparticles

NASA Astrophysics Data System (ADS)

Ranjbar, Zohreh Rashidi; Morsali, Ali

2009-11-01

Nano-scale of a new Pb(II) coordination polymer, {[Pb(bpacb)(OAc)]·DMF} n ( 1); bpacbH = 3,5-bis[(4-pyridylamino)carbonyl]benzoic acid], were synthesized by a sonochemical method. The nano-material was characterized by scanning electron microscopy, X-ray powder diffraction (XRD), 1H, 13C NMR, IR spectroscopy and elemental analyses. Crystal structure of compound 1 was determined by X-ray crystallography. Calcination of the nano-sized compound 1 at 700 °C under air atmospheres yields PbO nanoparticles. Thermal stability of nano-sized and single crystalline samples of compound 1 were studied and compared with each other.

Powder X-ray diffraction laboratory, Reston, Virginia

USGS Publications Warehouse

Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

2014-01-01

The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

The syntheses, molecular structure analyses and DFT studies on new benzil monohydrazone based Schiff bases

NASA Astrophysics Data System (ADS)

Elmacı, Gökhan; Duyar, Halil; Aydıner, Burcu; Seferoğlu, Nurgül; Naziri, Mir Abolfazl; Şahin, Ertan; Seferoğlu, Zeynel

2018-06-01

Benzil monohydrazone based Schiff bases were synthesized and characterized by 1H NMR, 13C NMR, HRMS as well as by single crystal X-ray diffraction. The geometries of the compounds was optimized by the DFT method and the results were compared with the X-ray diffraction data. The HOMO and LUMO energy gap and also related parameters (electronic chemical potential (μ) and global hardness (η), global electrophilicity index (ω) and softness (s)) were obtained from ground state calculations. In addition, the thermal properties of the compounds were investigated by DTA-TGA. The results showed that the compounds have good thermal properties for practical applications as optic dye.

X-ray Binaries and the Galaxy Structure in Hard X-rays

NASA Astrophysics Data System (ADS)

Lutovinov, Alexander

The Galaxy structure in the hard X-ray energy band (¿20 keV) was studied using data of the INTEGRAL observatory. A deep and nearly uniform coverage of the galactic plane allowed to increase significantly the sensitivity of the survey and discover several dozens new galac-tic sources. The follow-up observations with XMM-Newton and CHANDRA observatories in X-rays and ground-based telescopes in optical and infrared wavebands gave us a possibility to determine optical counterparts and distances for number of new and already known faint sources. That, in turn, allowed us to build the spatial distribution of different classes of galactic X-ray binaries and obtain preliminary results of the structure of the further part of the Galaxy.

Ain't no Crab, PWN Got a Brand New Bag: Correlated Radio and X-ray Structures in Pulsar Wind Nebulae

NASA Astrophysics Data System (ADS)

Roberts, M. S. E.; Lyutikov, M.; Gaensler, B. M.; Brogan, C. L.; Tam, C. R.; Romani, R. W.

2005-04-01

The traditional view of radio pulsar wind nebulae (PWN), encouraged by the Crab nebula's X-ray and radio morphologies, is that they are a result of the integrated history of their pulsars' wind. The radio emission should therefore be largely unaffected by recent pulsar activity, and hence minimally correlated with structures in the X-ray nebulae. Observations of several PWN, both stationary and rapidly moving, now show clear morphological relationships between structures in the radio and X-ray with radio intensity variations on the order of unity. We present high-resolution X-ray and radio images of several PWN of both types and discuss the morphological relationships between the two wavebands.

Ethanol fixed brain imaging by phase-contrast X-ray technique

NASA Astrophysics Data System (ADS)

Takeda, Tohoru; Thet-Thet-Lwin; Kunii, Takuya; Sirai, Ryota; Ohizumi, Takahito; Maruyama, Hiroko; Hyodo, Kazuyuki; Yoneyama, Akio; Ueda, Kazuhiro

2013-03-01

The two-crystal phase-contrast X-ray imaging technique using an X-ray crystal interferometer can depict the fine structures of rat's brain such as cerebral cortex, white matter, and basal ganglia. Image quality and contrast by ethanol fixed brain showed significantly better than those by usually used formalin fixation at 35 keV X-ray energy. Image contrast of cortex by ethanol fixation was more than 3-times higher than that by formalin fixation. Thus, the technique of ethanol fixation might be better suited to image cerebral structural detail at 35 keV X-ray energy.

Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

NASA Astrophysics Data System (ADS)

Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

2016-03-01

Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization of the resin embedded (originally polycrystalline) silicate sample. We explore the astrophysical implications of this laboratory result as an upper limit to the effect of X-rays on the structure of cosmic silicates.

X-ray radiative transfer in protoplanetary disks. The role of dust and X-ray background fields

NASA Astrophysics Data System (ADS)

Rab, Ch.; Güdel, M.; Woitke, P.; Kamp, I.; Thi, W.-F.; Min, M.; Aresu, G.; Meijerink, R.

2018-01-01

Context. The X-ray luminosities of T Tauri stars are about two to four orders of magnitude higher than the luminosity of the contemporary Sun. As these stars are born in clusters, their disks are not only irradiated by their parent star but also by an X-ray background field produced by the cluster members. Aims: We aim to quantify the impact of X-ray background fields produced by young embedded clusters on the chemical structure of disks. Further, we want to investigate the importance of the dust for X-ray radiative transfer in disks. Methods: We present a new X-ray radiative transfer module for the radiation thermo-chemical disk code PRODIMO (PROtoplanetary DIsk MOdel), which includes X-ray scattering and absorption by both the gas and dust component. The X-ray dust opacities can be calculated for various dust compositions and dust-size distributions. For the X-ray radiative transfer we consider irradiation by the star and by X-ray background fields. To study the impact of X-rays on the chemical structure of disks we use the well established disk ionization tracers N2H+ and HCO+. Results: For evolved dust populations (e.g. grain growth), X-ray opacities are mostly dominated by the gas; only for photon energies E ≳ 5-10 keV do dust opacities become relevant. Consequently the local disk X-ray radiation field is only affected in dense regions close to the disk midplane. X-ray background fields can dominate the local X-ray disk ionization rate for disk radii r ≳ 20 au. However, the N2H+ and HCO+ column densities are only significantly affected in cases of low cosmic-ray ionization rates (≲10-19 s-1), or if the background flux is at least a factor of ten higher than the flux level of ≈10-5 erg cm-2 s-1 expected for clusters typical for the solar vicinity. Conclusions: Observable signatures of X-ray background fields in low-mass star-formation regions, like Taurus, are only expected for cluster members experiencing a strong X-ray background field (e.g. due to their location within the cluster). For the majority of the cluster members, the X-ray background field has relatively little impact on the disk chemical structure.

PREFACE: Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques

NASA Astrophysics Data System (ADS)

Sakurai, Kenji

2010-12-01

This special issue is devoted to describing recent applications of x-ray and neutron scattering techniques to the exploration of surfaces and buried interfaces of various functional materials. Unlike many other surface-sensitive methods, these techniques do not require ultra high vacuum, and therefore, a variety of real and complicated surfaces fall within the scope of analysis. It must be particularly emphasized that the techniques are capable of seeing even buried function interfaces as well as the surface. Furthermore, the information, which ranges from the atomic to mesoscopic scale, is highly quantitative and reproducible. The non-destructive nature of the techniques is another important advantage of using x-rays and neutrons, when compared with other atomic-scale analyses. This ensures that the same specimen can be measured by other techniques. Such features are fairly attractive when exploring multilayered materials with nanostructures (dots, tubes, wires, etc), which are finding applications in electronic, magnetic, optical and other devices. The Japan Applied Physics Society has established a group to develop the research field of studying buried function interfaces with x-rays and neutrons. As the methods can be applied to almost all types of materials, from semiconductor and electronic devices to soft materials, participants have fairly different backgrounds but share a common interest in state-of-the-art x-ray and neutron techniques and sophisticated applications. A series of workshops has been organized almost every year since 2001. Some international interactions have been continued intensively, although the community is part of a Japanese society. This special issue does not report the proceedings of the recent workshop, although all the authors are in some way involved in the activities of the above society. Initially, we intended to collect quite long overview papers, including the authors' latest and most important original results, as well as updates on recent progress and global trends in the field. We planned to cover quite a wide area of surface and buried interface science with x-rays and neutrons. Following a great deal of discussion during the editing process, we have decided to change direction. As we intend to publish similar special issues on a frequent basis, we will not insist on editing this issue as systematic and complete collections of research. Many authors decided to write an ordinary research paper rather than an article including systematic accounts. Due to this change in policy, some authors declined to contribute, and the number of papers is now just 12. However, readers will find that the special issue gives an interesting collection of new original research in surface and buried interface studies with x-rays and neutrons. The 12 papers cover the following research topics: (1) polymer analysis by diffuse scattering; (2) discussion of the electrochemical solid--liquid interface by synchrotron x-ray diffraction; (3) analysis of capped nanodots by grazing incidence small-angle x-ray scattering (GISAXS); (4) discussion of the strain distribution in silicon by high-resolution x-ray diffraction; (5) study of mesoporous structures by a combination of x-ray reflectivity and GISAXS; (6) discussion of energy-dispersive x-ray reflectometry and its applications; (7) neutron reflectivity studies on hydrogen terminated silicon interface; (8) the fabrication and performance of a special mirror for water windows; (9) depth selective analysis by total-reflection x-ray diffraction; (10) nanoparticle thin films prepared by a gas deposition technique; (11) discussion of crystal truncation rod (CTR) scattering of semiconductor nanostructures; (12) magnetic structure analysis of thin films by polarized neutron reflectivity. While not discussed in the present special issue, x-ray and neutron techniques have made great progress. The most important steps forward have been in 2D/3D real-space imaging, and realtime measurement. Advances in such technologies are bringing with them new opportunities in surface and buried interface science. In the not too distant future, we will publish a special issue or a book detailing such progress. Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques contents Lateral uniformity in chemical composition along a buried reaction front in polymers using off-specular reflectivity Kristopher A Lavery, Vivek M Prabhu, Sushil Satija and Wen-li Wu Orientation dependence of Pd growth on Au electrode surfaces M Takahasi, K Tamura, J Mizuki, T Kondo and K Uosaki A grazing incidence small-angle x-ray scattering analysis on capped Ge nanodots in layer structures Hiroshi Okuda, Masayuki Kato, Keiji Kuno, Shojiro Ochiai, Noritaka Usami, Kazuo Nakajima and Osami Sakata High resolution grazing-incidence in-plane x-ray diffraction for measuring the strain of a Si thin layer Kazuhiko Omote X-ray analysis of mesoporous silica thin films templated by Brij58 surfactant S Fall, M Kulij and A Gibaud Review of the applications of x-ray refraction and the x-ray waveguide phenomenon to estimation of film structures Kouichi Hayashi Epitaxial growth of largely mismatched crystals on H-terminated Si(111) surfaces Hidehito Asaoka Novel TiO2/ZnO multilayer mirrors at 'water-window' wavelengths fabricated by atomic layer epitaxy H Kumagai, Y Tanaka, M Murata, Y Masuda and T Shinagawa Depth-selective structural analysis of thin films using total-external-reflection x-ray diffraction Tomoaki Kawamura and Hiroo Omi Structures of Yb nanoparticle thin films grown by deposition in He and N2 gas atmospheres: AFM and x-ray reflectivity studies Martin Jerab and Kenji Sakurai Ga and As composition profiles in InP/GaInAs/InP heterostructures—x-ray CTR scattering and cross-sectional STM measurements Yoshikazu Takeda, Masao Tabuchi and Arao Nakamura Polarized neutron reflectivity study of a thermally treated MnIr/CoFe exchange bias system Naoki Awaji, Toyoo Miyajima, Shuuichi Doi and Kenji Nomura

Control Scheme for Quickly Starting X-ray Tube

NASA Astrophysics Data System (ADS)

Nakahama, Masayuki; Nakanishi, Toshiki; Ishitobi, Manabu; Ito, Tuyoshi; Hosoda, Kenichi

A control scheme for quickly starting a portable X-ray generator used in the livestock industry is proposed in this paper. A portable X-ray generator used to take X-ray images of animals such as horses, sheep and dogs should be capable of starting quickly because it is difficult for veterinarians to take X-ray images of animals at their timing. In order to develop a scheme for starting the X-ray tube quickly, it is necessary to analysis the X-ray tube. However, such an analysis has not been discussed until now. First, the states of an X-ray tube are classified into the temperature-limited state and the space-charge-limited state. Furthermore, existence of “mixed state” that comprises both is newly proposed in this paper. From these analyses, a novel scheme for quickly starting an X-ray generator is proposed; this scheme is considered with the characteristics of the X-ray tube. The proposed X-ray system that is capable of starting quickly is evaluated on the basis of experimental results.

RXTE Observations of Cygnus X-3

NASA Technical Reports Server (NTRS)

McCollough, M. L.; Robinson, C. R.; Zhang, S. N.; Harmon, B. A.; Paciesas, W. S.; Dieters, S. W.; Hjellming, R. M.; Rupen, M.; Mioduszewski, A. J.; Waltman, E. B.

1997-01-01

In the period between May 1997 and August 1997 a series of pointed RXTE observations were made of Cyg X-3. During this period Cyg X-3 made a transition from a quiescent radio state to a flare state (including a major flare) and then returned to a quiescent radio state. Analyses of the observations are made in the context of concurrent observations in the hard X-ray (CGRO/BATSE), soft X-ray (RXTE/ASM) and the radio (Green Bank Interferometer, Ryle Telescope, and RATAN-600). Preliminary analyses of the observations are presented.

Zinc(II) complexes with potent cyclin-dependent kinase inhibitors derived from 6-benzylaminopurine: synthesis, characterization, X-ray structures and biological activity.

PubMed

Trávnícek, Zdenek; Krystof, Vladimír; Sipl, Michal

2006-02-01

The synthesis, characterization and biological activity of the first zinc(II) complexes with potent inhibitors of cyclin-dependent kinases (CDKs) derived from 6-benzylaminopurine are described. Based on the results following from elemental analyses, infrared, NMR and ES+MS (electrospray mass spectra in the positive ion mode) spectroscopies, conductivity data, thermal analysis and X-ray structures, the tetrahedral Zn(II) complexes of the compositions [Zn(Olo)Cl(2)](n) (1), [Zn(iprOlo)Cl(2)](n) (2), [Zn(BohH(+))Cl(3)] x H(2)O (3) and [Zn(iprOloH(+))Cl(3)] x H(2)O (4) have been prepared, where Olo=2-(2-hydroxyethylamino)-6-benzylamino-9-methylpurine (Olomoucine), iprOlo=2-(2-hydroxyethylamino)-6-benzylamino-9-isopropylpurine (i-propyl-Olomoucine), Boh=2-(3-hydroxypropylamino)-6-benzylamino-9-isopropylpurine (Bohemine). The 1D-polymeric chain structure for [Zn(Olo)Cl(2)](n) (1) as well as the monomeric one for [Zn(BohH(+))Cl(3)] x H(2)O (3) and [Zn(iprOloH(+))Cl(3)] x H(2)O (4) have been revealed unambiguously by single crystal X-ray analyses. The 1D-polymeric chain of 1 consists of Zn(Olo)Cl(2) monomeric units in which the Zn(II) ion is coordinated by two chlorine atoms and one oxygen atom of the 2-hydroxyethylamino group of Olomoucine. The next monomeric unit is bonded to Zn(II) through the N7 atom of a purine ring. Thus, each of Zn(II) ions is tetrahedrally coordinated and a ZnCl(2)NO chromophore occurs in the complex 1. The complexes 3 and 4 are mononuclear species with a distorted tetrahedral arrangement of donor atoms around the Zn(II) ion with a ZnCl(3)N chromophore. The corresponding CDK inhibitor, i.e., both Boh and iprOlo, is coordinated to Zn(II) via the N7 atom of the purine ring in 3 and 4. The cytotoxicity of the zinc(II) complexes against human melanoma, sarcoma, leukaemia and carcinoma cell lines has been determined as well as the inhibition of the CDK2/cyclin E kinase. A relationship between the structure and biological activity of the complexes is also discussed.

An experimental study of the local electronic structure of B-site gallium doped bismuth ferrite powders

NASA Astrophysics Data System (ADS)

Gholam, Turghunjan; Ablat, Abduleziz; Mamat, Mamatrishat; Wu, Rong; Aimidula, Aimierding; Bake, Muhammad Ali; Zheng, Lirong; Wang, Jiaou; Qian, Haijie; Wu, Rui; Ibrahim, Kurash

2017-08-01

The un-doped and gallium (Ga) doped multiferroic bismuth ferrite (BiFeO3) compounds were successfully synthesized by the hydrothermal technique. This is then followed by a series of detailed investigations into the influence of Ga doping on the structural, morphological, optical and magnetic properties of BiFe1 - xGaxO3 (0 ≤ x ≤ 0.15). X-ray diffraction (XRD) analyses reveal that B-site doping of Ga may lead to the transformation of its crystal structure from a rhombohedral with a space group of R3c to an orthorhombic with a space group of Pbnm phase. The scanning electron microscope (SEM) images show that doping with Ga causes a significant reduction in particle size, when compared to un-doped BiFeO3. X-ray absorption near-edge structure (XANES) spectra have also shown that as the substitution of Ga increases, the Fe K and Bi LIII-edge absorption spectra shift towards higher energy site. It also implies that doping of Ga affects the local structures of both Bi and Fe atoms. Distinct transmission band fluctuations, as shown by Fourier transform infrared (FT-IR) spectra, can provide significant evidence for a transformation in crystal structure, following the increase of Ga concentration. The magnetization hysteresis measurements show that the magnetization decreases when Ga content is x ≥ 0.05. Such a phenomenon mainly stems from the substitution of Fe for an excessive amount of Ga, resulting in reduction of both valence fluctuations and the magnetization in the BiFe1 - xGaxO3 system.

Electronic structure of the organic semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from soft x-ray spectroscopies and density functional theory calculations.

PubMed

DeMasi, A; Piper, L F J; Zhang, Y; Reid, I; Wang, S; Smith, K E; Downes, J E; Peltekis, N; McGuinness, C; Matsuura, A

2008-12-14

The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq(3)) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq(3), and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studies and the present data reveal the presence of clear photon-induced damage in the former.

Full Field X-Ray Fluorescence Imaging Using Micro Pore Optics for Planetary Surface Exploration

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Blake, D. F.; Gailhanou, M.; Walter, P.; Schyns, E.; Marchis, F.; Thompson, K.; Bristow, T.

2016-01-01

Many planetary surface processes leave evidence as small features in the sub-millimetre scale. Current planetary X-ray fluorescence spectrometers lack the spatial resolution to analyse such small features as they only provide global analyses of areas greater than 100 mm(exp 2). A micro-XRF spectrometer will be deployed on the NASA Mars 2020 rover to analyse spots as small as 120m. When using its line-scanning capacity combined to perpendicular scanning by the rover arm, elemental maps can be generated. We present a new instrument that provides full-field XRF imaging, alleviating the need for precise positioning and scanning mechanisms. The Mapping X-ray Fluorescence Spectrometer - "Map-X" - will allow elemental imaging with approximately 100µm spatial resolution and simultaneously provide elemental chemistry at the scale where many relict physical, chemical and biological features can be imaged in ancient rocks. The arm-mounted Map-X instrument is placed directly on the surface of an object and held in a fixed position during measurements. A 25x25 mm(exp 2) surface area is uniformly illuminated with X-rays or alpha-particles and gamma-rays. A novel Micro Pore Optic focusses a fraction of the emitted X-ray fluorescence onto a CCD operated at a few frames per second. On board processing allows measuring the energy and coordinates of each X-ray photon collected. Large sets of frames are reduced into 2d histograms used to compute higher level data products such as elemental maps and XRF spectra from selected regions of interest. XRF spectra are processed on the ground to further determine quantitative elemental compositions. The instrument development will be presented with an emphasis on the characterization and modelling of the X-ray focussing Micro Pore Optic. An outlook on possible alternative XRF imaging applications will be discussed.

Finite element analyses of thin film active grazing incidence x-ray optics

NASA Astrophysics Data System (ADS)

Davis, William N.; Reid, Paul B.; Schwartz, Daniel A.

2010-09-01

The Chandra X-ray Observatory, with its sub-arc second resolution, has revolutionized X-ray astronomy by revealing an extremely complex X-ray sky and demonstrating the power of the X-ray window in exploring fundamental astrophysical problems. Larger area telescopes of still higher angular resolution promise further advances. We are engaged in the development of a mission concept, Generation-X, a 0.1 arc second resolution x-ray telescope with tens of square meters of collecting area, 500 times that of Chandra. To achieve these two requirements of imaging and area, we are developing a grazing incidence telescope comprised of many mirror segments. Each segment is an adjustable mirror that is a section of a paraboloid or hyperboloid, aligned and figure corrected in situ on-orbit. To that end, finite element analyses of thin glass mirrors are performed to determine influence functions for each actuator on the mirrors, in order to develop algorithms for correction of mirror deformations. The effects of several mirror mounting schemes are also studied. The finite element analysis results, combined with measurements made on prototype mirrors, will be used to further refine the correction algorithms.

In situ spectroscopic and solution analyses of the reductive dissolution of Mn02 by Fe(II)

USGS Publications Warehouse

Villinski, John E.; O'Day, Peggy A.; Corley, Timothy L.; Conklin, Martha H.

2001-01-01

The reductive dissolution of MnO2 by Fe(II) under conditions simulating acid mine drainage (pH 3, 100 mM SO42-) was investigated by utilizing a flow-through reaction cell and synchrotron X-ray absorption spectroscopy. This configuration allows collection of in situ, real-time X-ray absorption near-edge structure (XANES) spectra and bulk solution samples. Analysis of the solution chemistry suggests that the reaction mechanism changed (decreased reaction rate) as MnO2 was reduced and Fe(III) precipitated, primarily as ferrihydrite. Simultaneously, we observed an additional phase, with the local structure of jacobsite (MnFe2O4), in the Mn XANES spectra of reactants and products. The X-ray absorbance of this intermediate phase increased during the experiment, implying an increase in concentration. The presence of this phase, which probably formed as a surface coating, helps to explain the reduced rate of dissolution of manganese(IV) oxide. In natural environments affected by acid mine drainage, the formation of complex intermediate solid phases on mineral surfaces undergoing reductive dissolution may likewise influence the rate of release of metals to solution.

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

Estimations of Mo X-pinch plasma parameters on QiangGuang-1 facility by L-shell spectral analyses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Jian; Qiu, Aici; State Key Laboratory of Intense Pulsed Radiation Simulation and Effect, Northwest Institute of Nuclear Technology, Xi'an 710024

2013-08-15

Plasma parameters of molybdenum (Mo) X-pinches on the 1-MA QiangGuang-1 facility were estimated by L-shell spectral analysis. X-ray radiation from X-pinches had a pulsed width of 1 ns, and its spectra in 2–3 keV were measured with a time-integrated X-ray spectrometer. Relative intensities of spectral features were derived by correcting for the spectral sensitivity of the spectrometer. With an open source, atomic code FAC (flexible atomic code), ion structures, and various atomic radiative-collisional rates for O-, F-, Ne-, Na-, Mg-, and Al-like ionization stages were calculated, and synthetic spectra were constructed at given plasma parameters. By fitting the measured spectramore » with the modeled, Mo X-pinch plasmas on the QiangGuang-1 facility had an electron density of about 10{sup 21} cm{sup −3} and the electron temperature of about 1.2 keV.« less

A new generation of x-ray spectrometry UHV instruments at the SR facilities BESSY II, ELETTRA and SOLEIL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lubeck, J., E-mail: janin.lubeck@ptb.de; Fliegauf, R.; Holfelder, I.

A novel type of ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation (SR) has been constructed and commissioned at BESSY II. This versa-tile instrument was developed by the PTB, Germany’s national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, it integrates a rotational and translational movement of several photodiodes as well as a translational movement of a beam-geometry-defining aperture system. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors suchmore » as reference-free X-Ray Fluorescence (XRF) analysis, total-reflection XRF, grazing-incidence XRF, in addition to optional X-Ray Reflectometry (XRR) measurements or polarization-dependent X-ray absorption fine structure analyses (XAFS). Samples having a size of up to (100 × 100) mm{sup 2}; can be analyzed with respect to their mass deposition, elemental, spatial or species composition. Surface contamination, nanolayer composition and thickness, depth pro-file of matrix elements or implants, nanoparticles or buried interfaces as well as molecular orientation of bonds can be accessed. Three technology transfer projects of adapted instruments have enhanced X-Ray Spectrometry (XRS) research activities within Europe at the synchrotron radiation facilities ELETTRA (IAEA) and SOLEIL (CEA/LNE-LNHB) as well as at the X-ray innovation laboratory BLiX (TU Berlin) where different laboratory sources are used. Here, smaller chamber requirements led PTB in cooperation with TU Berlin to develop a modified instrument equipped with a 7-axis manipulator: reduced freedom in the choice of experimental geometry modifications (absence of out-of-SR-plane and reference-free XRS options) has been compensated by encoder-enhanced angular accuracy for GIXRF and XRR.« less

Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance.

PubMed

Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

2016-06-01

The structure of nanocrystalline calcium silicate hydrates (C-S-H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29 Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH) 2 -like structure, nanocrystalline and intermixed with C-S-H layers, at high Ca/Si ratios.

PREFACE: Buried Interface Sciences with X-rays and Neutrons 2010

NASA Astrophysics Data System (ADS)

Sakurai, Kenji

2011-09-01

The 2010 summer workshop on buried interface science with x-rays and neutrons was held at Nagoya University, Japan, on 25-27 July 2010. The workshop was organized by the Japan Applied Physics Society, which established a group to develop the research field of studying buried function interfaces with x-rays and neutrons. The workshop was the latest in a series held since 2001; Tsukuba (December 2001), Niigata (September 2002), Nagoya (July 2003), Tsukuba (July 2004), Saitama (March 2005), Yokohama (July 2006), Kusatsu (August 2006), Tokyo (December 2006), Sendai (July 2007), Sapporo (September 2007), Tokyo (December 2007), Tokyo-Akihabara (July 2009) and Hiratsuka (March 2010). The 2010 summer workshop had 64 participants and 34 presentations. Interfaces mark the boundaries of different material systems at which many interesting phenomena take place, thus making it extremely important to design, fabricate and analyse the structures of interfaces at both the atomic and macroscopic scale. For many applications, devices are prepared in the form of multi-layered thin films, with the result that interfaces are not exposed but buried under multiple layers. Because of such buried conditions, it is generally not easy to analyse such interfaces. In certain cases, for example, when the thin surface layer is not a solid but a liquid such as water, scientists can observe the atomic arrangement of the liquid-solid interface directly by using a scanning probe microscope, of which the tip is soaked in water. However, it has become clear that the use of a stylus tip positioned extremely close to the interface might change the structure of the water molecules. Therefore it is absolutely crucial to develop non-contact, non-destructive probes for buried interfaces. It is known that analysis using x-rays and neutrons is one of the most powerful tools for exploring near-surface structures including interfaces buried under several layers. In particular, x-ray analysis using 3rd generation synchrotron radiation is highly reliable in practice, as well as being quantitative and reproducible. The use of neutron analysis complements x-ray experiments, and helps to enhance information such as contrasts in soft materials and magnetic structures, which are not always given clearly by x-rays. The techniques ensure non-contact, non-destructive measurement, and one can also use the same specimen for further analysis by other methods. On the other hand, we are now aware that it not always straightforward to solve many realistic problems related to buried interfaces. Although advanced synchrotron x-rays and neutrons are highly useful, we still note many limitations. Collaboration with theoreticians is one of the most important directions in which to improve analysis. Over the past couple of years, scientists have argued over the existence of a depletion layer between oil and water. The argument is far from settled, even though highly sophisticated x-ray reflectometry seems to have given quite strong experimental evidence. In most cases, analysis of x-ray reflectivity depends on the model. This is good provided that one can be sure of the validity of the model, as in the case of multilayered thin films in industrial devices. However, sometimes our main interest lies in the model itself. Therefore, we should insist on introducing something new to justify the model scientifically, instead of just claiming that x-ray data can be explained by a certain model. Probably collaboration with theoretical research could be helpful. Another important direction would be to develop a method of model-free analysis. During this workshop, participants talked about the present status of their own work. The workshop was open to those who are not particular specialists in x-ray and neutron experiments, but discussions were detailed and thorough. We discussed how buried interface research by x-ray and neutron experiments can be strengthened in the future. One of the most important extensions is high resolution in space (micro area) and time (quick and realtime). Current x-ray methods can give atomic-scale information for quite a large area on a scale of mm2-cm2, but it is also important to see a specific small area rather than the average structure of the wide area. In addition, there is a need to see unstable changing structures and related phenomena in order to understand more about the mechanism of the functioning of nano materials. Quick measurements are therefore important. Another effective extension would come with combining several x-ray and neutron techniques (reflectivity, grazing-incidence small angle scattering (GISAS), diffraction, x-ray absorption and emission spectroscopy etc). The use of coherent beams and several other new approaches are also significant. We do not, in this current volume, intend to present what could be termed conference proceedings in a strict sense. Some papers were contributed by those who could not attend the workshop. Other papers were written on topics that were not presented during the workshop. We have always argued in favour of the significance of publishing such collections of papers; isn't it more important for young scientists to publish their results in a good ordinary journal with a high impact factor? The answer is obvious. We have already published so many papers in leading journals, and therefore, the next step would be to share information among specialists (including those who will become specialists) at a deeper level. Young scientists should contribute their work to such collections of papers, in addition to ordinary journals. In this way, almost all specialists in this field will read and respond to them. Publishing papers here will become a starting point for new discussions. I would also like to mention that almost all the papers included in this issue were reviewed thoroughly by four reviewers, who mainly make up the specialist group of the Japan Applied Physics Society. I sincerely acknowledge the efforts and assistance of all my colleagues during the editing of this issue. This publication was financially supported by National Institute for Materials Science, Japan. Kenji Sakurai National Institute for Materials Science Chairman of the workshop A list of previous publications by our group: 1. J. Phys.: Condens. Matter 22 (2010) http://iopscience.iop.org/0953-8984/22/47 2. Trans MRS Japan 34 No 4 (2009) 3. 'Introduction to X-ray reflectivity' (Kodansha, 2009) [in Japanese] 4. Trans MRS Japan 33 No 3 (2008) 5. J. Phys.: Conf. Ser. 83 (2007) http://www.iop.org/EJ/toc/1742-6596/83/1 6. Trans MRS Japan 32 No 1 (2007) 7. Report on buried interface sciences with X-rays and neutrons (2006) http://www.nims.go.jp/xray/lab/hot/kaimen.pdf [in Japanese] 8. KEK Proceedings, 2006-3, 'Buried Interface Science with X-rays and Neutrons' (2006) 9. KEK Proceedings, 2004-5, 'Nano science/technology with synchrotron and neutron reflectivity' (2004) [in Japanese] 10. Trans MRS Japan 28 special issue (2003) 11. KEK Proceedings, 2001-25, 'Structural analysis of thin films and multilayers by X-ray and neutron reflectivity' (2002) [in Japanese

Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

PubMed Central

Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

2016-01-01

For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

X-ray crystal structure and small-angle X-ray scattering of sheep liver sorbitol dehydrogenase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yennawar, Hemant; Møller, Magda; University of Copenhagen, DK-2100 Copenhagen

The X-ray crystal structure and a small-angle X-ray scattering solution structure of sheep liver sorbitol dehydrogenase have been determined. The details of the interactions that enable the tetramer scaffold to be the functional biological unit have been analyzed. The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer that superposes well with that seen in hSDH (despite belonging to a different space group) and obeying the 222 crystalmore » symmetry is seen in slSDH. An acetate molecule is bound in the active site, coordinating to the active-site zinc through a water molecule. Glycerol, a substrate of slSDH, also occupies the substrate-binding pocket together with the acetate designed by nature to fit large polyol substrates. The substrate-binding pocket is seen to be in close proximity to the tetramer interface, which explains the need for the structural integrity of the tetramer for enzyme activity. Small-angle X-ray scattering was also used to identify the quaternary structure of the tetramer of slSDH in solution.« less

Common structural features of toxic intermediates from α-synuclein and GroES fibrillogenesis detected using cryogenic coherent X-ray diffraction imaging.

PubMed

Kameda, Hiroshi; Usugi, Sayaka; Kobayashi, Mana; Fukui, Naoya; Lee, Seki; Hongo, Kunihiro; Mizobata, Tomohiro; Sekiguchi, Yuki; Masaki, Yu; Kobayashi, Amane; Oroguchi, Tomotaka; Nakasako, Masayoshi; Takayama, Yuki; Yamamoto, Masaki; Kawata, Yasushi

2017-01-01

The aggregation and deposition of α-synuclein (αSyn) in neuronal cells is correlated to pathogenesis of Parkinson's disease. Although the mechanism of αSyn aggregation and fibril formation has been studied extensively, the structural hallmarks that are directly responsible for toxicity toward cells are still under debate. Here, we have compared the structural characteristics of the toxic intermediate molecular species of αSyn and similar toxic species of another protein, GroES, using coherent X-ray diffraction analysis. Using coherent X-ray free electron laser pulses of SACLA, we analysed αSyn and GroES fibril intermediate species and characterized various aggregate structures. Unlike previous studies where an annular oligomeric form of αSyn was identified, particle reconstruction from scattering traces suggested that the specific forms of the toxic particles were varied, with the sizes of the particles falling within a specific range. We did however discover a common structural feature in both αSyn and GroES samples; the edges of the detected particles were nearly parallel and produced a characteristic diffraction pattern in the diffraction experiments. The presence of parallel-edged particles in toxic intermediates of αSyn and GroES fibrillogenesis pointed towards a plausible common molecular interface that leads to the formation of mature fibrils. © The Authors 2016. Published by Oxford University Press on behalf of the Japanese Biochemical Society. All rights reserved.

Influence of Fabrication Conditions on the Structural and the Magnetic Properties of Co-doped BaFe12O19 Hexaferrites

NASA Astrophysics Data System (ADS)

Tran, Ngo; Kim, Deok Hyeon; Lee, Bo Wha

2018-03-01

BaFe11CoO19 hexaferrites were prepared by using a co-precipitation method and heat treatment. By changing the ion molar ratio of (Fe + Co)/Ba = ( x + 1)/1, we found a clear difference in the crystalline structural and magnetic properties. Particularly, the magnetic properties became optimal at x = 11 - 13 based on the saturation magnetization and coercivity values. The effects of heat treatment on the morphological, structural and magnetic properties were assessed. With the results of thermal gravimetric analyses, X-ray diffraction patterns, and magnetic-field-dependent magnetization, we found that M-type hexaferrite nanocrystals start being formed at a temperature of 650°C, which was much lower than temperatures reported previously.

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

DOE PAGES

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

2012-11-05

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as wellmore » as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ 1,3 XES spectra of Mn II and Mn 2 III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. Furthermore, the technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II.« less

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

PubMed Central

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Schafer, Donald W.; Sellberg, Jonas; Kenney, Christopher; Herbst, Ryan; Pines, Jack; Hart, Philip; Herrmann, Sven; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; Fry, Alan R.; Messerschmidt, Marc M.; Miahnahri, Alan; Seibert, M. Marvin; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

2012-01-01

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as well as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. The technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II. PMID:23129631

Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula

NASA Technical Reports Server (NTRS)

Weisskopf, M.; Hester, J. J.; Tennant, A. F.; Elsner, R. F.; Schulz, N. S.; Marshall, H. L.; Karovska, M.; Nichols, J. S.; Swartz, D. A.; Kolodziejczak, J. J.

2000-01-01

The Chandra X-ray Observatory observed the Crab Nebula and Pulsar During orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) read-out by the Advanced CCD Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure, at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the Nebula.

Evidence for magnetic energy storage in coronal active regions

NASA Technical Reports Server (NTRS)

Krieger, A. S.; De Feiter, L. D.; Vaiana, G. S.

1976-01-01

Examination of X-ray images obtained by the S-054 X-ray spectrographic telescope on Skylab shows the presence of some atypical X-ray-emitting coronal structures in active regions which are not consistent with potential extrapolations of photospheric magnetic fields. Analysis of the observed temporal changes in the X-ray-emitting active-region structures demonstrates that the majority of these consist of brightness changes representing temperature (and perhaps density) variations of the material in the loops.

Microanalysis of iron oxidation state in iron oxides using X Ray Absorption Near Edge Structure (XANES)

NASA Technical Reports Server (NTRS)

Sutton, S. R.; Delaney, J.; Bajt, S.; Rivers, M. L.; Smith, J. V.

1993-01-01

An exploratory application of x ray absorption near edge structure (XANES) analysis using the synchrotron x ray microprobe was undertaken to obtain Fe XANES spectra on individual sub-millimeter grains in conventional polished sections. The experiments concentrated on determinations of Fe valence in a suite of iron oxide minerals for which independent estimates of the iron speciation could be made by electron microprobe analysis and x ray diffraction.

High-power laser interaction with low-density C–Cu foams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pérez, F.; Colvin, J. D.; May, M. J.

2015-11-15

We study the propagation of high-power laser beams in micro-structured carbon foams by monitoring the x-ray output from deliberately introduced Cu content. In particular, we characterize this phenomenon measuring absolute time-resolved x-ray yields, time-resolved x-ray imaging, and x-ray spectroscopy. New experimental results for C–Cu foams show a faster heat front velocity than simulation that assumed homogeneous plasma. We suggest the foam micro-structure may explain this trend.

High-power laser interaction with low-density C–Cu foams

DOE PAGES

Pérez, F.; Colvin, J. D.; May, M. J.; ...

2015-11-19

Here, we study the propagation of high-power laser beams in micro-structured carbon foams by monitoring the x-ray output from deliberately introduced Cu content. In particular, we characterize this phenomenon measuring absolute time-resolved x-ray yields, time-resolved x-ray imaging, and x-ray spectroscopy. New experimental results for C–Cu foams show a faster heat front velocity than simulation that assumed homogeneous plasma. We suggest the foam micro-structure may explain this trend.

On the molecular and supramolecular properties of N,N‧-disubstituted iminoisoindolines: Synthesis, spectroscopy, X-ray structure and Hirshfeld surface analyses, and DFT calculations of two (E)-N,N‧-bis(aryl)iminoisoindolines (aryl = 2-tert-butylphenyl or perfluorophenyl)

NASA Astrophysics Data System (ADS)

Bitzer, Rodrigo S.; Visentin, Lorenzo C.; Hörner, Manfredo; Nascimento, Marco A. C.; Filgueiras, Carlos A. L.

2017-02-01

Supramolecular studies of iminoisoindoline-derived compounds have been prompted by their biological and photophysical properties. In this article, we report the synthesis, spectroscopy, X-ray structural characterization, and DFT study of two N,N‧-(aryl)-disubstituted 1-iminoisoindolines, namely (E)-N,N‧-bis(2-tert-butylphenyl)iminoisoindoline (2-t-BuPhimiso) and (E)-N,N‧-bis(perfluorophenyl)iminoisoindoline (F5Phimiso). Our X-ray structural analyses have shown that the isoindoline N2 atom of 2-t-BuPhimiso is slightly pyramidalized whereas the respective atom of F5Phimiso displays the expected trigonal planar geometry. The supramolecular arrangement of 2-t-BuPhimiso comprises one-dimensional chains along the [101] direction formed by Csbnd H···πarene interactions, in which the isoindoline ring behaves as a hydrogen-bond donor. For 2-t-BuPhimiso, DFT calculations at the B97-D3/6-311G** level have shown that the dimer formed by this Csbnd H···πarene contact displays a binding energy of -12.83 kcal mol-1. Product F5Phimiso assembles in the crystal state through type-I F3 synthons in addition to Csbnd H⋯F, C-Fδ-···πF+, and πarene/F-πarene/F stacking interactions. Accordingly, our DFT-D3 calculations have confirmed that these interactions synergistically play a dominating role in the crystal packing of F5Phimiso. Finally, the relative stability of the (Z) and (E) isomers of each product has been evaluated at the DFT level of theory. Our calculations have shown that the (E) forms are the most stable ones.

Small angle x-ray scattering of chromatin. Radius and mass per unit length depend on linker length.

PubMed Central

Williams, S P; Langmore, J P

1991-01-01

Analyses of low angle x-ray scattering from chromatin, isolated by identical procedures but from different species, indicate that fiber diameter and number of nucleosomes per unit length increase with the amount of nucleosome linker DNA. Experiments were conducted at physiological ionic strength to obtain parameters reflecting the structure most likely present in living cells. Guinier analyses were performed on scattering from solutions of soluble chromatin from Necturus maculosus erythrocytes (linker length 48 bp), chicken erythrocytes (linker length 64 bp), and Thyone briareus sperm (linker length 87 bp). The results were extrapolated to infinite dilution to eliminate interparticle contributions to the scattering. Cross-sectional radii of gyration were found to be 10.9 +/- 0.5, 12.1 +/- 0.4, and 15.9 +/- 0.5 nm for Necturus, chicken, and Thyone chromatin, respectively, which are consistent with fiber diameters of 30.8, 34.2, and 45.0 nm. Mass per unit lengths were found to be 6.9 +/- 0.5, 8.3 +/- 0.6, and 11.8 +/- 1.4 nucleosomes per 10 nm for Necturus, chicken, and Thyone chromatin, respectively. The geometrical consequences of the experimental mass per unit lengths and radii of gyration are consistent with a conserved interaction among nucleosomes. Cross-linking agents were found to have little effect on fiber external geometry, but significant effect on internal structure. The absolute values of fiber diameter and mass per unit length, and their dependencies upon linker length agree with the predictions of the double-helical crossed-linker model. A compilation of all published x-ray scattering data from the last decade indicates that the relationship between chromatin structure and linker length is consistent with data obtained by other investigators. Images FIGURE 1 PMID:2049522

Structures and standard molar enthalpies of formation of a series of Ln(III)–Cu(II) heteronuclear compounds with pyrazine-2,3-dicarboxylic acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Qi; Xie, Gang; Wei, Qing

2014-07-01

Fifteen lanthanide–copper heteronuclear compounds, formulated as [CuLn{sub 2}(pzdc){sub 4}(H{sub 2}O){sub 6}]·xH{sub 2}O (1–6(x=2), 8(x=3), 9–10(x=4)); [CuLn{sub 2}(pzdc){sub 4}(H{sub 2}O){sub 4}]·xH{sub 2}O (7, 12–13, 15(x=4), 14(x=5), 11(x=8)) (Ln(III)=La(1); Ce(2); Pr(3); Nd(4); Sm(5); Eu(6); Gd(7); Tb(8); Dy(9); Ho(10); Er(11); Tm(12); Yb(13); Lu(14); Y(15); H{sub 2}pzdc (C{sub 6}H{sub 4}N{sub 2}O{sub 4})=pyrazine-2,3-dicarboxylic acid) have been hydrothermally synthesized. All compounds were characterized by element analysis, IR spectroscopy, single-crystal X-ray diffraction and thermal analysis. X-ray diffraction analyses confirm that all compounds are isostructural and feature a 3D brick-like framework structure with (4.6{sup 2}){sub 2}(4{sup 2}.6{sup 2}.8{sup 2})(6{sup 3}){sup 2}(6{sup 5}.8){sub 2} topology. Using 1 mol cm{supmore » −3} HCl(aq) as calorimetric solvent, with an isoperibol solution–reaction calorimeter, the standard molar enthalpies of formation of all compounds were determined by a designed thermochemical cycle. In addition, solid state luminescence properties of compounds 5, 6, 8 and 9 were studied in the solid state. - Graphical abstract: According to Hess' rule, the standard molar enthalpies of formation of Ln–Cu heterometallic coordination compounds were determined by a designed thermochemical cycle. - Highlights: • Fifteen lanthanide–copper heteronuclear isostructural compounds. • Structurally characterization by IR, X-ray diffraction and thermal analysis. • The standard molar enthalpy of formation. • Isoperibol solution–reaction calorimetry.« less

Observation of multiple dielectric relaxations in BaTiO3-Bi(Li1/3Ti2/3)O3 ceramics

NASA Astrophysics Data System (ADS)

Zhou, Changrong; Feteira, Antonio

2017-11-01

Dense (1 - x)BaTiO3- xBi(Li1/3Ti2/3)O3 ceramics were fabricated by the solid state reaction route. Powder X-ray diffraction analyses revealed an increase in the unit cell volume with increasing x and a change on the average crystal structure from tetragonal (space group P4mm) to cubic ( Pm\\bar{3}m ) at x > 0.10. Raman spectroscopy analyses corroborated a change of symmetry, but also showed the local structure for x > 0.10 to be inconsistent with the centrosymmetric ( Pm\\bar{3}m ) space group. The dielectric measurements revealed for the first time, to our knowledge, a double relaxor behaviour in a BaTiO3-based solid solution. Basically, with increasing x, the sharp ferroelectric anomaly at the Curie temperature ( T c) shifts towards lower temperatures until a relaxor-type response is observed, but simultaneously, another relaxation emerges above T c. The first arises from poor coupling between polar nanoregions, whereas the later obeys the Arrhenius Law and may be associated either with a defect-dipole reorientation or a Skanavi-type mechanism.

Tracking reaction dynamics in solution by pump-probe X-ray absorption spectroscopy and X-ray liquidography (solution scattering).

PubMed

Kim, Jeongho; Kim, Kyung Hwan; Oang, Key Young; Lee, Jae Hyuk; Hong, Kiryong; Cho, Hana; Huse, Nils; Schoenlein, Robert W; Kim, Tae Kyu; Ihee, Hyotcherl

2016-03-07

Characterization of transient molecular structures formed during chemical and biological processes is essential for understanding their mechanisms and functions. Over the last decade, time-resolved X-ray liquidography (TRXL) and time-resolved X-ray absorption spectroscopy (TRXAS) have emerged as powerful techniques for molecular and electronic structural analysis of photoinduced reactions in the solution phase. Both techniques make use of a pump-probe scheme that consists of (1) an optical pump pulse to initiate a photoinduced process and (2) an X-ray probe pulse to monitor changes in the molecular structure as a function of time delay between pump and probe pulses. TRXL is sensitive to changes in the global molecular structure and therefore can be used to elucidate structural changes of reacting solute molecules as well as the collective response of solvent molecules. On the other hand, TRXAS can be used to probe changes in both local geometrical and electronic structures of specific X-ray-absorbing atoms due to the element-specific nature of core-level transitions. These techniques are complementary to each other and a combination of the two methods will enhance the capability of accurately obtaining structural changes induced by photoexcitation. Here we review the principles of TRXL and TRXAS and present recent application examples of the two methods for studying chemical and biological processes in solution. Furthermore, we briefly discuss the prospect of using X-ray free electron lasers for the two techniques, which will allow us to keep track of structural dynamics on femtosecond time scales in various solution-phase molecular reactions.

3D X-ray ultra-microscopy of bone tissue.

PubMed

Langer, M; Peyrin, F

2016-02-01

We review the current X-ray techniques with 3D imaging capability at the nano-scale: transmission X-ray microscopy, ptychography and in-line phase nano-tomography. We further review the different ultra-structural features that have so far been resolved: the lacuno-canalicular network, collagen orientation, nano-scale mineralization and their use as basis for mechanical simulations. X-ray computed tomography at the micro-metric scale is increasingly considered as the reference technique in imaging of bone micro-structure. The trend has been to push towards increasingly higher resolution. Due to the difficulty of realizing optics in the hard X-ray regime, the magnification has mainly been due to the use of visible light optics and indirect detection of the X-rays, which limits the attainable resolution with respect to the wavelength of the visible light used in detection. Recent developments in X-ray optics and instrumentation have allowed to implement several types of methods that achieve imaging that is limited in resolution by the X-ray wavelength, thus enabling computed tomography at the nano-scale. We review here the X-ray techniques with 3D imaging capability at the nano-scale: transmission X-ray microscopy, ptychography and in-line phase nano-tomography. Further, we review the different ultra-structural features that have so far been resolved and the applications that have been reported: imaging of the lacuno-canalicular network, direct analysis of collagen orientation, analysis of mineralization on the nano-scale and use of 3D images at the nano-scale to drive mechanical simulations. Finally, we discuss the issue of going beyond qualitative description to quantification of ultra-structural features.

Probing molecular dynamics in solution with x-ray valence-to-core spectroscopy

NASA Astrophysics Data System (ADS)

Doumy, Gilles; March, Anne Marie; Tu, Ming-Feng; Al Haddad, Andre; Southworth, Stephen; Young, Linda; Walko, Donald; Bostedt, Christoph

2017-04-01

Hard X-ray spectroscopies are powerful tools for probing the electronic and geometric structure of molecules in complex or disordered systems and have been particularly useful for studying molecules in the solution phase. They are element specific, sensitive to the electronic structure and the local arrangements of surrounding atoms of the element being selectively probed. When combined in a pump-probe scheme with ultrafast lasers, X-ray spectroscopies can be used to track the evolution of structural changes that occur after photoexcitation. Efficient use of hard x-ray radiation coming from high brilliance synchrotrons and upcoming high repetition rate X-ray Free Electron Lasers requires MHz repetition rate lasers and data acquisition systems. High information content Valence-to-Core x-ray emission is directly sensitive to the molecular orbitals involved in photochemistry. We report on recent progress towards fully enabling this photon-hungry technique for the study of time-resolved molecular dynamics, including efficient detection and use of polychromatic x-ray micro-probe at the Advanced Photon Source. Work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

Exposure to ionizing radiation during dental X-rays is not associated with risk of developing meningioma: a meta-analysis based on seven case-control studies.

PubMed

Xu, Ping; Luo, Hong; Huang, Guang-Lei; Yin, Xin-Hai; Luo, Si-Yang; Song, Ju-Kun

2015-01-01

Many observational studies have found that exposure to dental X-rays is associated with the risk of development of meningioma. However, these findings are inconsistent. We conducted a meta-analysis to assess the relationship between exposure to dental X-rays and the risk of development of meningioma. The PubMed and EMBASE databases were searched to identify eligible studies. Summary odds ratio (OR) estimates and 95% confidence intervals (95% CIs) were used to compute the risk of meningioma development according to heterogeneity. Subgroup and sensitivity analyses were performed to further explore the potential heterogeneity. Finally, publication bias was assessed. Seven case-control studies involving 6,174 patients and 19,459 controls were included in the meta-analysis. Neither exposure to dental X-rays nor performance of full-mouth panorex X-rays was associated with an increased risk of development of meningioma (overall: OR, 0.97; 95% CI, 0.70-1.32; dental X-rays: OR, 1.05; 95% CI, 0.89-1.25; panorex X-rays: OR, 1.01; 95% CI, 0.76-1.34). However, exposure to bitewing X-rays was associated with a slightly increased risk of development of meningioma (OR, 1.73; 95% CI, 1.28-2.34). Similar results were obtained in the subgroup and sensitivity analyses. Little evidence of publication bias was observed. Based on the currently limited data, there is no association between exposure to dental X-rays and the risk of development of meningioma. However, these results should be cautiously interpreted because of the heterogeneity among studies. Additional large, high-quality clinical trials are needed to evaluate the association between exposure to dental X-rays and the risk of development of meningioma.

Role of phi cells and the endodermis under salt stress in Brassica oleracea.

PubMed

Fernandez-Garcia, N; Lopez-Perez, L; Hernandez, M; Olmos, E

2009-01-01

Phi cell layers were discovered in the 19th century in a small number of species, including members of the Brassicaceae family. A mechanical role was first suggested for this structure; however, this has never been demonstrated. The main objective of the present work was to analyse the ultrastructure of phi cells, their influence on ion movement from the cortex to the stele, and their contribution to salt stress tolerance in Brassica oleracea. Transmission electron microscopy and X-ray microanalysis studies were used to analyse the subcellular structure and distribution of ions in phi cells and the endodermis under salt stress. Ion movement was analysed using lanthanum as an apoplastic tracer. The ultrastructural results confirm that phi cells are specialized cells showing cell wall ingrowths in the inner tangential cell walls. X-ray microanalysis confirmed a build-up of sodium. Phi thickenings were lignified and lanthanum moved periplasmically at this level. To the best of our knowledge, this is the first study reporting the possible role of the phi cells as a barrier controlling the movement of ions from the cortex to the stele. Therefore, the phi cell layer and endodermis seem to be regulating ion transport in Brassica oleracea under salt stress.

X-ray Point Source Populations in Spiral and Elliptical Galaxies

NASA Astrophysics Data System (ADS)

Colbert, E.; Heckman, T.; Weaver, K.; Strickland, D.

2002-01-01

The hard-X-ray luminosity of non-active galaxies has been known to be fairly well correlated with the total blue luminosity since the days of the Einstein satellite. However, the origin of this hard component was not well understood. Some possibilities that were considered included X-ray binaries, extended upscattered far-infrared light via the inverse-Compton process, extended hot 107 K gas (especially in ellipitical galaxies), or even an active nucleus. Chandra images of normal, elliptical and starburst galaxies now show that a significant amount of the total hard X-ray emission comes from individual point sources. We present here spatial and spectral analyses of the point sources in a small sample of Chandra obervations of starburst galaxies, and compare with Chandra point source analyses from comparison galaxies (elliptical, Seyfert and normal galaxies). We discuss possible relationships between the number and total hard luminosity of the X-ray point sources and various measures of the galaxy star formation rate, and discuss possible options for the numerous compact sources that are observed.

X-ray and optical substructures of the DAFT/FADA survey clusters

NASA Astrophysics Data System (ADS)

Guennou, L.; Durret, F.; Adami, C.; Lima Neto, G. B.

2013-04-01

We have undertaken the DAFT/FADA survey with the double aim of setting constraints on dark energy based on weak lensing tomography and of obtaining homogeneous and high quality data for a sample of 91 massive clusters in the redshift range 0.4-0.9 for which there were HST archive data. We have analysed the XMM-Newton data available for 42 of these clusters to derive their X-ray temperatures and luminosities and search for substructures. Out of these, a spatial analysis was possible for 30 clusters, but only 23 had deep enough X-ray data for a really robust analysis. This study was coupled with a dynamical analysis for the 26 clusters having at least 30 spectroscopic galaxy redshifts in the cluster range. Altogether, the X-ray sample of 23 clusters and the optical sample of 26 clusters have 14 clusters in common. We present preliminary results on the coupled X-ray and dynamical analyses of these 14 clusters.

X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.

2016-05-15

A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer ofmore » the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.« less

Local Structure Determination of Carbon/Nickel Ferrite Composite Nanofibers Probed by X-ray Absorption Spectroscopy.

PubMed

Nilmoung, Sukunya; Kidkhunthod, Pinit; Maensiri, Santi

2015-11-01

Carbon/NiFe2O4 composite nanofibers have been successfully prepared by electrospinning method using a various concentration solution of Ni and Fe nitrates dispersed into polyacrylonitride (PAN) solution in N,N' dimethylformamide. The phase and mophology of PAN/NiFe2O4 composite samples were characterized and investigated by X-ray diffraction and scanning electron microscopy. The magnetic properties of the prepared samples were measured at ambient temperature by a vibrating sample magnetometer. It is found that all composite samples exhibit ferromagnetism. This could be local-structurally explained by the existed oxidation states of Ni2+ and Fe3+ in the samples. Moreover, local environments around Ni and Fe ions could be revealed by X-ray absorption spectroscopy (XAS) measurement including X-ray absorption near edge structure (XANES) and Extended X-ray absorption fine structure (EXAFS).

Zn(II) coordination polymers with flexible V-shaped dicarboxylate ligand: Syntheses, helical structures and properties

NASA Astrophysics Data System (ADS)

Li, Lin; Liu, Chong-Bo; Yang, Gao-Shan; Xiong, Zhi-Qiang; Liu, Hong; Wen, Hui-Liang

2015-11-01

Hydrothermal reactions of 2,2‧-[hexafluoroisopropylidenebis(p-phenyleneoxy)]diacetic acid (H2L) and zinc ions in the presence of N-donor ancillary ligands afford four novel coordination polymers, namely, [Zn2(μ2-OH)(μ4-O)0.5(L)]·0.5H2O (1), [Zn(L)(2,2‧-bipy)(H2O)] (2), [Zn3(L)3(phen)2]·H2O (3) and [Zn2(L)2(4,4‧-bipy)] (4) (2,2‧-bipy=2,2‧-bipyridine; 4,4‧-bipy=4,4‧-bipyridine; phen=1,10-phenanthroline). Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra, powder X-ray diffraction (PXRD), and thermogravimetric (TG) analyses. Complex 1 shows a 3-D clover framework consisting of [Zn4(μ4-O)(μ2-OH)2]4+ clusters, and exhibits a novel (3,8)-connected topological net with the Schläfli symbol of {3·4·5}2{34·44·52·66·710·82}, and contains double-stranded and two kinds of meso-helices. 2 displays a helical chain structure, which is further extended via hydrogen bonds into a 3-D supramolecular structure with meso-helix chains. 3 displays a 2-D {44·62} parallelogram structure, which is further extended via hydrogen bonds into a 3-D supramolecular structure with single-stranded helical chains. 4 shows a 2-D {44·62} square structure with left- and right-handed helical chains. Moreover, the luminescent properties of 1-4 have been investigated.

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

NASA Astrophysics Data System (ADS)

Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W.; Suino-Powell, Kelly M.; Boutet, Sébastien; Williams, Garth J.; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N.; Spence, John C. H.; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C.; Cherezov, Vadim; Melcher, Karsten; Xu, H. Eric

2016-04-01

Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex.

PubMed

Zhou, X Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W; Suino-Powell, Kelly M; Boutet, Sébastien; Williams, Garth J; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N; Spence, John C H; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C; Cherezov, Vadim; Melcher, Karsten; Xu, H Eric

2016-04-12

Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, X. Edward; Gao, Xiang; Barty, Anton

Here, serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solvedmore » with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.« less

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

PubMed Central

Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W.; Suino-Powell, Kelly M.; Boutet, Sébastien; Williams, Garth J.; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N.; Spence, John C.H.; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C.; Cherezov, Vadim; Melcher, Karsten; Xu, H. Eric

2016-01-01

Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes. PMID:27070998

X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

DOE PAGES

Zhou, X. Edward; Gao, Xiang; Barty, Anton; ...

2016-04-12

Here, serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solvedmore » with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.« less

Diterpenoid glycosides from the bitter fern Gleichenia quadripartita.

PubMed

Socolsky, Cecilia; Asakawa, Yoshinori; Bardón, Alicia

2007-12-01

Fifteen new diterpenoid glycosides (1a-n, 2) were isolated from an Argentine collection of the bitter fern Gleichenia quadripartita along with the known flavonoid glycoside afzelin. Structure elucidation was accomplished by 1D and 2D NMR spectroscopy and by high-resolution MS analyses. In addition, X-ray crystallographic analysis of a monocrystal of 1a as well as chemical derivatization of 1h and 1m were performed to confirm their structures.

Novel Drift Structures for Silicon and Compound Semiconductor X-Ray and Gamma-Ray Detectors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bradley E. Patt; Jan S. Iwanczyk

Recently developed silicon- and compound-semiconductor-based drift detector structures have produced excellent performance for charged particles, X rays, and gamma rays and for low-signal visible light detection. The silicon drift detector (SDD) structures that we discuss relate to direct X-ray detectors and scintillation photon detectors coupled with scintillators for gamma rays. Recent designs include several novel features that ensure very low dark current (both bulk silicon dark current and surface dark current) and hence low noise. In addition, application of thin window technology ensures a very high quantum efficiency entrance window on the drift photodetector.

Thermal expansion behavior study of Co nanowire array with in situ x-ray diffraction and x-ray absorption fine structure techniques

NASA Astrophysics Data System (ADS)

Mo, Guang; Cai, Quan; Jiang, Longsheng; Wang, Wei; Zhang, Kunhao; Cheng, Weidong; Xing, Xueqing; Chen, Zhongjun; Wu, Zhonghua

2008-10-01

In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10-6/°C and the second-order thermal expansion coefficient of 5.9×10-9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.

Syntheses and characterizations of transition-metal-substituted aluminophosphate molecular sieves |(C3N2H5) 8|[M8Al16P24O96] (M = Co, Mn, Zn) with zeotype LAU topology.

PubMed

Song, Xiaowei; Li, Jiyang; Guo, Yanan; Pan, Qinhe; Gan, Lin; Yu, Jihong; Xu, Ruren

2009-01-05

Three transitional-metal-substituted aluminophosphate molecular sieves, |(C3N2H5)8|[M8Al16P24O96] (denoted MAPO-LAU, M = Co, Mn, Zn), have been synthesized under solvothermal conditions in the presence of imidazole as the structure-directing agent. Their structures are determined by single-crystal X-ray diffraction and further characterized by powder X-ray diffraction, inductively coupled plasma, thermogravimetric, and diffuse reflectance spectroscopy (UV-vis) analyses. The structure of MAPO-LAU is based on the strict alternation of MO4/AlO4 tetrahedra and PO4 tetrahedra through vertex oxygen atoms. Their frameworks are analogous to the zeotype LAU structure in which 33% of the aluminum sites are replaced by transitional-metal ions. The protonated imidazole cations resided in the 10-ring channels. These compounds show photoluminescent properties due to the existence of imidazole molecules in the structures. Magnetic measurements reveal that there is very weak antiferromagnetic interaction among the metal centers of MnAPO-LAU.

Pyrano-isoflavones with erectile-dysfunction activity from Eriosema kraussianum.

PubMed

Drewes, Siegfried E; Horn, Marion M; Munro, Orde Q; Dhlamini, Jabu T B; Meyer, J J Marion; Rakuambo, N Christopher

2002-04-01

Five pyrano-isoflavones have been isolated from the rootstock of Eriosema kraussianum N. E. Br (Papilionaceae). Spectral data and single crystal X-ray analyses were used for structural elucidation. The most active of the compounds had an activity of 75% of that found in Viagra in the erectile dysfunction test on rabbit penile smooth muscle.

Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Surendra, E-mail: surendra@barc.gov.in; Basu, Saibal

2016-05-23

X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependentmore » structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.« less

Spectroscopic imaging, diffraction, and holography with x-ray photoemission

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1992-02-01

X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimentalmore » fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons.« less

Studies on the growth, structural, spectral and third-order nonlinear optical properties of ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate single crystal.

PubMed

Silambarasan, A; Krishna Kumar, M; Thirunavukkarasu, A; Mohan Kumar, R; Umarani, P R

2015-01-25

An organic nonlinear optical bulk single crystal, Ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate (ACHBS) was successfully grown by solution growth technique. Single crystal X-ray diffraction study confirms that, the grown crystal belongs to P21/c space group. Powder X-ray diffraction and high resolution X-ray diffraction analyses revealed the crystallinity of the grown crystal. Infrared spectral analysis showed the vibrational behavior of chemical bonds and its functional groups. The thermal stability and decomposition stages of the grown crystal were studied by TG-DTA analysis. UV-Visible transmittance studies showed the transparency region and cut-off wavelength of the grown crystal. The third-order nonlinear optical susceptibility of the grown crystal was estimated by Z-scan technique using He-Ne laser source. The mechanical property of the grown crystal was studied by using Vicker's microhardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

X-ray structure determination using low-resolution electron microscopy maps for molecular replacement

DOE PAGES

Jackson, Ryan N.; McCoy, Airlie J.; Terwilliger, Thomas C.; ...

2015-07-30

Structures of multi-subunit macromolecular machines are primarily determined by either electron microscopy (EM) or X-ray crystallography. In many cases, a structure for a complex can be obtained at low resolution (at a coarse level of detail) with EM and at higher resolution (with finer detail) by X-ray crystallography. The integration of these two structural techniques is becoming increasingly important for generating atomic models of macromolecular complexes. A low-resolution EM image can be a powerful tool for obtaining the "phase" information that is missing from an X-ray crystallography experiment, however integration of EM and X-ray diffraction data has been technically challenging.more » Here we show a step-by-step protocol that explains how low-resolution EM maps can be placed in the crystallographic unit cell by molecular replacement, and how initial phases computed from the placed EM density are extended to high resolution by averaging maps over non-crystallographic symmetry. As the resolution gap between EM and Xray crystallography continues to narrow, the use of EM maps to help with X-ray crystal structure determination, as described in this protocol, will become increasingly effective.« less

Investigation of (Ti-Zr-Hf-V-Nb)N Multicomponent Nanostructured Coatings before and after Thermal Annealing by Nuclear Physics Methods of Analysis

NASA Astrophysics Data System (ADS)

Pogrebnjak, A. D.; Beresnev, V. M.; Bondar', A. V.; Kaverin, M. V.; Ponomarev, A. G.

2013-10-01

(Ti-Zr-Hf-V-Nb)N multicomponent nanostructured coatings with thickness of 1.0-1.4 μm synthesized by the method of cathode arc-vapor deposition at temperatures of 250-300°С are investigated by various mutually complementary methods of elemental structural analysis using slow positron beams (SPB), proton microbeam based particle-induced x-ray emission (μ-PIXE), energy-dispersive x-ray spectroscopy (EDS) and scanning electron microscopy (SEM) analyses based on electron micro- and nanobeams, x-ray diffraction (XRD) method of phase structural analysis, and the "a-sin2φ" method of measuring a stressed-strained state (x-ray tensometry). The elemental composition, microstructure, residual stress in nanograins, profiles of defect and atom distributions with depth and over the coating surface in 3D-representation are studied for these coatings, and their phase composition, severely strained state, and composition of coatings before and after annealing at Tann = 600°С for annealing time τ = 30 min are investigated. It is demonstrated that the oxidation resistance of the examined coatings can be significantly increased by high-temperature annealing that leads to the formation of elastic severely strained compression state of the coating. Redistribution of elements and defects, their segregation near the interface boundaries and around grains and subgrains in the process of thermostimulated diffusion, and termination of spinodal segregation without considerable change of the average nanograin size are revealed.

Lithiation-induced zinc clustering of Zn 3, Zn 12, and Zn 18 units in Zintl-like Ca ~30Li 3+xZn 60-x (x=0.44-1.38)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Qisheng

2014-11-14

Zinc clusters are not common for binary intermetallics with relatively low zinc content, but this work shows that zinc clustering can be triggered by lithiation, as exemplified by Ca ~30Li 3+xZn 60-x, P6/mmm, Z = 1, which can be directly converted from CaZn 2. Two end members of the solid solution (x = 0.44 and 1.38) were established and structurally characterized by single-crystal X-ray diffraction analyses: Ca 30Li 3.44(6)Zn59.56(6), a = 15.4651(9) Å, c = 9.3898(3) Å; Ca 30.45(2)Li 4.38(6)Zn 58.62(6), a = 15.524(3) Å, c = 9.413(2) Å. The structures of Ca ~30Li 3+xZn 60-x feature a condensed anionicmore » network of Zn3 triangles, lithium-centered Zn12 icosahedra, and arachno-(Zn,Li)18 tubular clusters that are surrounded respectively by Ca 14, Ca 20, and Ca 30 polyhedra. These polyhedra share faces and form a clathrate-like cationic framework. The specific occupation of lithium in the structure is consistent with theoretical “coloring” analyses. Analysis by the linear muffin-tin orbital (LMTO) method within the atomic sphere approximation reveals that Ca ~30Li 3+xZn 60-x is a metallic, Zintl-like phase with an open-shell electronic structure. The contribution of Ca–Zn polar covalent interactions is about 41%.« less

Exploring interface morphology of a deeply buried layer in periodic multilayer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Das, Gangadhar; Srivastava, A. K.; Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in

2016-06-27

Long-term durability of a thin film device is strongly correlated with the nature of interface structure associated between different constituent layers. Synthetic periodic multilayer structures are primarily employed as artificial X-ray Bragg reflectors in many applications, and their reflection efficiency is predominantly dictated by the nature of the buried interfaces between the different layers. Herein, we demonstrate the applicability of the combined analysis approach of the X-ray reflectivity and grazing incidence X-ray fluorescence measurements for the reliable and precise determination of a buried interface structure inside periodic X-ray multilayer structures. X-ray standing wave field (XSW) generated under Bragg reflection conditionmore » is used to probe the different constituent layers of the W- B{sub 4}C multilayer structure at 10 keV and 12 keV incident X-ray energies. Our results show that the XSW assisted fluorescence measurements are markedly sensitive to the location and interface morphology of a buried layer structure inside a periodic multilayer structure. The cross sectional transmission electron microscopy results obtained on the W-B{sub 4}C multilayer structure provide a deeper look on the overall reliability and accuracy of the XSW method. The method described here would also be applicable for nondestructive characterization of a wide range of thin film based semiconductor and optical devices.« less

Electronic Structure of the Organic Semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from Soft X-ray Spectroscopies and Density Functional Theory Calculations

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeMasi, A.; Piper, L; Zhang, Y

2008-01-01

The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq3) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq3, and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studiesmore » and the present data reveal the presence of clear photon-induced damage in the former.« less

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

NASA Astrophysics Data System (ADS)

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-04-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called ``molecular movie'' within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

PubMed Central

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-01-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes. PMID:24740172

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

DOE PAGES

Gaudin, J.; Fourment, C.; Cho, B. I.; ...

2014-04-17

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

21 CFR 892.1650 - Image-intensified fluoroscopic x-ray system.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Image-intensified fluoroscopic x-ray system. 892... fluoroscopic x-ray system. (a) Identification. An image-intensified fluoroscopic x-ray system is a device intended to visualize anatomical structures by converting a pattern of x-radiation into a visible image...

21 CFR 892.1650 - Image-intensified fluoroscopic x-ray system.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Image-intensified fluoroscopic x-ray system. 892... fluoroscopic x-ray system. (a) Identification. An image-intensified fluoroscopic x-ray system is a device intended to visualize anatomical structures by converting a pattern of x-radiation into a visible image...

The use of C-near edge X-ray absorption fine structure spectroscopy for the elaboration of chemistry in lignocellulosics

Treesearch

Lucian A. Lucia; Hiroki Nanko; Alan W. Rudie; Doug G. Mancosky; Sue Wirick

2006-01-01

The research presented elucidates the oxidation chemistry occurring in hydrogen peroxide bleached kraft pulp fibers by employing carbon near edge x-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft x-ray technique that selectively interrogates atomic moieties using photoelectrons (Xrays) of variable energies. The X1A beam line at the National...

Tracing the Mass-Dependent Star Formation History of Late-Type Galaxies using X-ray Emission: Results from the CHANDRA Deep Fields

NASA Technical Reports Server (NTRS)

Lehmer, B.D; Brandt, W.N.; Schneider, D.P.; Steffen, A.T.; Alexander, D.M.; Bell, E.F.; Hornschemeier, A.E.; McIntosh, D.H.; Bauer, F.E.; Gilli, R.;

Hunting for Intrinsically X-ray Weak Quasars: The Case of PHL 1811 Analogs

NASA Astrophysics Data System (ADS)

Brandt, William

2009-09-01

A central dogma of X-ray astronomy is that luminous X-ray emission is a universal property of efficiently accreting supermassive black holes. One interesting challenge to this idea has come from the quasar PHL 1811 which appears to be intrinsically X-ray weak and also has distinctive emission-line properties. We propose to observe a sample of eight SDSS quasars, selected to have similar UV emission-line properties to that of PHL 1811, to test if they are also X-ray weak. Our analyses of the currently available X-ray data appear to support this hypothesis but do not provide a proper test. Our results will have implications for the nature of accretion-disk coronae, emission-line formation, and AGN selection.

OSO-8 X-ray spectra of clusters of galaxies. 2: Discussion. [hot intracluster gas structures

NASA Technical Reports Server (NTRS)

Smith, B. W.; Mushotzky, R. F.; Serlemitsos, P. J.

1978-01-01

X-ray spectral parameters obtained from 2 to 20 keV OSO-8 data on X-ray clusters and optical cluster properties were examined to obtain information for restricting models for hot intracluster gas structures. Topics discussed include the radius of the X-ray core in relation to the galaxy core radius, the viral mass of hotter clusters, and galaxy density and optical central cluster properties. A population of cool, dim X-ray clusters which have not been observed is predicted. The iron abundance determinations recently quoted for intracluster gas are uncertain by 50 to greater than 100 percent from this nonstatistical cause alone.

Synthesis and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.

A facile synthesis of zinc oxide/multiwalled carbon nanotube nanocomposite lithium ion battery anodes by sol-gel method

NASA Astrophysics Data System (ADS)

Köse, Hilal; Karaal, Şeyma; Aydın, Ali Osman; Akbulut, Hatem

2015-11-01

Free standing zinc oxide (ZnO) and multiwalled carbon nanotube (MWCNT) nanocomposite materials are prepared by a sol gel technique giving a new high capacity anode material for lithium ion batteries. Free-standing ZnO/MWCNT nanocomposite anodes with two different chelating agent additives, triethanolamine (TEA) and glycerin (GLY), yield different electrochemical performances. Field emission gun scanning electron microscopy (FEG-SEM), energy dispersive X-ray spectrometer (EDS), high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) analyses reveal the produced anode electrodes exhibit a unique structure of ZnO coating on the MWCNT surfaces. Li-ion cell assembly using a ZnO/MWCNT/GLY free-standing anode and Li metal cathode possesses the best discharge capacity, remaining as high as 460 mAh g-1 after 100 cycles. This core-shell structured anode can offer increased energy storage and performance over conventional anodes in Li-ion batteries.

Synthesis, crystal structures, computational studies and antimicrobial activity of new designed bis((5-aryl-1,3,4-oxadiazol-2-yl)thio)alkanes

NASA Astrophysics Data System (ADS)

Ahmed, Muhammad Naeem; Sadiq, Beenish; Al-Masoudi, Najim A.; Yasin, Khawaja Ansar; Hameed, Shahid; Mahmood, Tariq; Ayub, Khurshid; Tahir, Muhammad Nawaz

2018-03-01

A new series of bis((5-aryl-1,3,4-oxadiazol-2-yl)thio)alkanes 4-14 have been synthesized via nucleophilic substitution reaction of dihaloalkanes with respective 1,3,4-oxadiazole-2-thiols 3a-f, and characterized by spectroscopic techniques. The structures of 4 and 12 were unambiguously confirmed by single-crystal X-ray diffraction analysis. Density functional theory calculations at B3LYP/6-31 + G(d) level of theory were performed for comparison of X-ray geometric parameters, molecular electrostatic potential (MEP) and frontier molecular orbital analyses of synthesized compounds. MEP analysis revealed that these compounds are nucleophilic in nature. Frontier molecular orbitals (FMOs) analysis of 4-14 was performed for evaluation of kinetic stability. All synthesized compounds were screened in vitro for antimicrobial activity against three bacterial and three fungal strains and showed promising results.

Tautomerism in N-(2-hydroxy-1-naphthylidene)amino acids and the search for an answer to the difficult question about where the proton belongs

NASA Astrophysics Data System (ADS)

Warncke, Gisela; Fels, Sabine; Brendler, Erica; Böhme, Uwe

2016-08-01

N-(2-hydroxy-1-naphthylidene)-L-valine 1, N-(2-hydroxy-1-naphthylidene)-L-phenylalanine 2, and N-(2-hydroxy-1-naphthylidene)-L-threonine 3 were prepared and characterized with spectroscopic methods, elemental analyses, and values of optical rotation. Compound 1 undergoes a solid state order-disorder phase transition at 231 K. The X-ray structures of the high and low temperature phase of 1 have been determined. Single crystal X-ray structures of 2 and 3 have been determined as well. The tautomerism of N-(2-hydroxy-1-naphthylidene)amino acid derivatives is discussed controversial in the literature. A bond lengths statistical analysis shows that all three compounds exist uniformly in the keto-amine form in the solid state. Quantum chemical calculations, NMR, and UV-Vis spectroscopy were used to obtain further insight into the existence of phenol-imine and keto-amine structures in this class of compounds.

Digital 3D Microstructure Analysis of Concrete using X-Ray Micro Computed Tomography SkyScan 1173: A Preliminary Study

NASA Astrophysics Data System (ADS)

Latief, F. D. E.; Mohammad, I. H.; Rarasati, A. D.

2017-11-01

Digital imaging of a concrete sample using high resolution tomographic imaging by means of X-Ray Micro Computed Tomography (μ-CT) has been conducted to assess the characteristic of the sample’s structure. A standard procedure of image acquisition, reconstruction, image processing of the method using a particular scanning device i.e., the Bruker SkyScan 1173 High Energy Micro-CT are elaborated. A qualitative and a quantitative analysis were briefly performed on the sample to deliver some basic ideas of the capability of the system and the bundled software package. Calculation of total VOI volume, object volume, percent of object volume, total VOI surface, object surface, object surface/volume ratio, object surface density, structure thickness, structure separation, total porosity were conducted and analysed. This paper should serve as a brief description of how the device can produce the preferred image quality as well as the ability of the bundled software packages to help in performing qualitative and quantitative analysis.

X-Ray Emission from Supernova Remnants.

NASA Astrophysics Data System (ADS)

Sackville Hamilton, Andrew James

1984-12-01

This thesis deals with the x-ray spectra of supernova remnants (SNRs), and in particular the x-ray spectra of the two young Type I SNRs SN1006 and Tycho. Firstly an extensive grid of nonequilibrium model spectra of SNRs in the adiabatic blast wave stage of evolution is computed, and numerous diagnostics of the state and composi- tion of the blast wave plasma are plotted over parameter space. It is demonstrated that the spectrum of an adiabatic blast wave is a good approximation to several other model SNR structures in which emission is dominated by gas undergoing quasi steady state ioni- zation near a shock front, including the one-fluid isothermal blast wave similarity solution, and the reverse shock similarity solution advocated by Chevalier for the early evolution of Type I SNe. None of these structures appears able to account for the observed spectra of SN1006 or Tycho. A new similarity solution for the early time evolution of uniform ejecta moving into an external medium is presented. It is argued that the x-ray spectra of SN1006 and Tycho are consistent with emission mainly from a reverse shock into 1.4M(,o) of initially uniform density SN ejecta consisting of pure heavy elements, moving into a uniform medium. Satisfactory fits to the observed spectra are obtained with a two layer structure of ejecta, an outer layer of unprocessed material, and an inner layer of mixed processed heavy elements. The structure of ejecta inferred is similar for both SN1006 and Tycho, the marked difference between the two spectra being attributed largely to the lower density of the ambient medium around SN1006. The results are consistent with the theory of Type I SNe as exploded white dwarfs, and resolve the apparent problems of too little iron, and too much total mass, deduced by other authors from earlier analyses of the x-ray emission of SN1006 and Tycho. Various salient aspects of the physics of a shock-heated pure heavy element plasma are discussed.

The Compton-thick AGN fraction from the deepest X-ray spectroscopy in the CDF-S

NASA Astrophysics Data System (ADS)

Corral, A.; Georgantopoulos, I.; Akylas, A.; Ranalli, P.

2017-10-01

Highly obscured AGN, especially Compton-thick (CT) AGN, likely play a key role in the galaxy-AGN co-evolution scenario. They would comprise the early stages of AGN activity, preceding the AGN-feedback/star-formation quenching phase, during which most of both the SMBH and galaxy growth take place. However, the actual CT fraction among the AGN population is still largely unconstrained. The most reliable way of confirming the obscured nature of an AGN by X-ray spectroscopy, but very deep observations are needed to extend local analyses to larger distances. We will present the X-ray spectral analysis of the deepest X-ray data obtained to date, the almost 7Ms observation of the Chandra Deep Field South. The unprecedented depth of this survey allow us to carry out reliable spectral analyses down to a flux limit of 10^{-16} erg cm^{-2} s^{-1} in the hard 2-8 keV band. Besides the new deeper X-ray data, our approach also includes the implementation of Bayesian inference in the determination of the CT fraction. Our results favor X-ray background synthesis models which postulate a moderate fraction (25%) of CT objects among the obscured AGN population.

Simultaneous measurements of X-ray reflectivity and grazing incidence fluorescence at BL-16 beamline of Indus-2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Das, Gangadhar; Kane, S. R.; Khooha, Ajay

2015-05-15

A new multipurpose x-ray reflectometer station has been developed and augmented at the microfocus beamline (BL-16) of Indus-2 synchrotron radiation source to facilitate synchronous measurements of specular x-ray reflectivity and grazing incidence x-ray fluorescence emission from thin layered structures. The design and various salient features of the x-ray reflectometer are discussed. The performance of the reflectometer has been evaluated by analyzing several thin layered structures having different surface interface properties. The results reveal in-depth information for precise determination of surface and interface properties of thin layered materials demonstrating the immense potential of the combined measurements of x-ray reflectivity and grazingmore » incidence fluorescence on a single reflectometer.« less

X-rays from the radio halo of Virgo A = M87

NASA Technical Reports Server (NTRS)

1985-01-01

The purpose of this study is to investigate in more detail the associated X-ray and radio emission in the Virgo A halo discovered by SGF. Improved Einstein HRI data and new radio maps obtained with the Very Large Array are described and the relation between the X-ray and radio structures is carefully examined. Several possible explanations are presented for the X-ray emission. The inverse compton model is found to be viable only if the magnetic field is variable and substantially weaker than the equipartition value. The principal alternative is excess thermal X-rays due to compression of the intracluster medium by the radio lobe. In either case, the association of such prominent radio and X-ray structures is unique among known radio galaxies.

Probing interfacial characteristics of rubrene/pentacene and pentacene/rubrene bilayers with soft X-ray spectroscopy.

PubMed

Seo, J H; Pedersen, T M; Chang, G S; Moewes, A; Yoo, K-H; Cho, S J; Whang, C N

2007-08-16

The electronic structure of rubrene/pentacene and pentacene/rubrene bilayers has been investigated using soft X-ray absorption spectroscopy, resonant X-ray emission spectroscopy, and density-functional theory calculations. X-ray absorption and emission measurements reveal that it has been possible to alter the lowest unoccupied and the highest occupied molecular orbital states of rubrene in rubrene/pentacene bilayer. In the reverse case, one gets p* molecular orbital states originating from the pentacene layer. Resonant X-ray emission spectra suggest a reduction in the hole-transition probabilities for the pentacene/rubrene bilayer in comparison to reference pentacene layer. For the rubrenepentacene structure, the hole-transition probability shows an increase in comparison to the rubrene reference. We also determined the energy level alignment of the pentacene-rubrene interface by using X-ray and ultraviolet photoelectron spectroscopy. From these comparisons, it is found that the electronic structure of the pentacene-rubrene interface has a strong dependence on interface characteristics which depends on the order of the layers used.

The BALDER Beamline at the MAX IV Laboratory

NASA Astrophysics Data System (ADS)

Klementiev, K.; Norén, K.; Carlson, S.; Sigfridsson Clauss, K. G. V.; Persson, I.

2016-05-01

X-ray absorption spectroscopy (XAS) includes well-established methods to study the local structure around the absorbing element - extended X-ray absorption fine structure (EXAFS), and the effective oxidation number or to quantitatively determine the speciation of an element in a complex matrix - X-ray absorption near-edge structure (XANES). The increased brilliance and intensities available at the new generation of synchrotron light sources makes it possible to study, in-situ and in-operando, much more dilute systems with relevance for natural systems, as well as the micro-scale variability and dynamics of chemical reactions on the millisecond time-scale. The design of the BALDER beamline at the MAX IV Laboratory 3 GeV ring has focused on a high flux of photons in a wide energy range, 2.4-40 keV, where the K-edge is covered for the elements S to La, and the L 3-edge for all elements heavier than Sb. The overall design of the beamline will allow large flexibility in energy range, beam size and data collection time. The other focus of the beamline design is the possibility to perform multi-technique analyses on samples. Development of sample environment requires focus on implementation of auxiliary methods in such a way that techniques like Fourier transform infrared (FTIR) spectroscopy, UV-Raman spectroscopy, X-ray diffraction and/or mass spectrometry can be performed simultaneously as the XAS study. It will be a flexible system where different instruments can be plugged in and out depending on the needs for the particular investigation. Many research areas will benefit from the properties of the wiggler based light source and the capabilities to perform in-situ and in-operando measurements, for example environmental and geochemical sciences, nuclear chemistry, catalysis, materials sciences, and cultural heritage.

On the large scale structure of X-ray background sources

NASA Technical Reports Server (NTRS)

Bi, H. G.; Meszaros, A.; Meszaros, P.

1991-01-01

The large scale clustering of the sources responsible for the X-ray background is discussed, under the assumption of a discrete origin. The formalism necessary for calculating the X-ray spatial fluctuations in the most general case where the source density contrast in structures varies with redshift is developed. A comparison of this with observational limits is useful for obtaining information concerning various galaxy formation scenarios. The calculations presented show that a varying density contrast has a small impact on the expected X-ray fluctuations. This strengthens and extends previous conclusions concerning the size and comoving density of large scale structures at redshifts 0.5 between 4.0.

High-resolution structural and elemental analyses of calcium storage structures synthesized by the noble crayfish Astacus astacus.

PubMed

Luquet, Gilles; Salomé, Murielle; Ziegler, Andreas; Paris, Céline; Percot, Aline; Dauphin, Yannicke

2016-11-01

During premolt, crayfish develop deposits of calcium ions, called gastroliths, in their stomach wall. The stored calcium is used for the calcification of parts of the skeleton regularly renewed for allowing growth. Structural and molecular analyses of gastroliths have been primarily performed on three crayfish species, Orconectes virilis, Procambarus clarkii, and more recently, Cherax quadricarinatus. We have performed high-resolution analyses of gastroliths from the native noble crayfish, Astacus astacus, focusing on the microstructure, the mineralogical and elemental composition and distribution in a comparative perspective. Field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) observations showed a classical layered microstructure composed of 200-nm diameter granules aligned along fibers. These granules are themselves composed of agglomerated nanogranules of 50nm-mean diameters. Denser regions of bigger fused granules are also present. Micro-Raman spectroscopy show that if A. astacus gastroliths, similarly to the other analyzed gastroliths, are mainly composed of amorphous calcium carbonate (ACC), they are also rich in amorphous calcium phosphate (ACP). The presence of a carotenoid pigment is also observed in A. astacus gastrolith contrary to C. quadricarinatus. Energy-dispersive X-ray spectroscopy (EDX) analyses demonstrate the presence of minor elements such as Mg, Sr, Si and P. The distribution of this last element is particularly heterogeneous. X-ray absorption near edge structure spectroscopy (XANES) reveals an alternation of layers more or less rich in phosphorus evidenced in the mineral phase as well as in the organic matrix in different molecular forms. Putative functions of the different P-comprising molecules are discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

Development of XAFS Into a Structure Determination Technique

NASA Astrophysics Data System (ADS)

Stern, E. A.

After the detection of diffraction of x-rays by M. Laue in 1912, the technique was soon applied to structure determination by Bragg within a year. On the other hand, although the edge steps in X-Ray absorption were discovered even earlier by Barkla and both the near edge (XANES) and extended X-Ray fine structure (EXAFS) past the edge were detected by 1929, it still took over 40 years to realize the structure information contained in this X-Ray absorption fine structure (XAFS). To understand this delay a brief historical review of the development of the scientific ideas that transformed XAFS into the premiere technique for local structure determination is given. The development includes both advances in theoretical understanding and calculational capabilities, and in experimental facilities, especially synchrotron radiation sources. The present state of the XAFS technique and its capabilities are summarized.

Structural investigation of porcine stomach mucin by X-ray fiber diffraction and homology modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Veluraja, K., E-mail: veluraja@msuniv.ac.in; Vennila, K.N.; Umamakeshvari, K.

Research highlights: {yields} Techniques to get oriented mucin fibre. {yields} X-ray fibre diffraction pattern for mucin. {yields} Molecular modeling of mucin based on X-ray fibre diffraction pattern. -- Abstract: The basic understanding of the three dimensional structure of mucin is essential to understand its physiological function. Technology has been developed to achieve orientated porcine stomach mucin molecules. X-ray fiber diffraction of partially orientated porcine stomach mucin molecules show d-spacing signals at 2.99, 4.06, 4.22, 4.7, 5.37 and 6.5 A. The high intense d-spacing signal at 4.22 A is attributed to the antiparallel {beta}-sheet structure identified in the fraction of themore » homology modeled mucin molecule (amino acid residues 800-980) using Nidogen-Laminin complex structure as a template. The X-ray fiber diffraction signal at 6.5 A reveals partial organization of oligosaccharides in porcine stomach mucin. This partial structure of mucin will be helpful in establishing a three dimensional structure for the whole mucin molecule.« less

An Excel Spreadsheet for a One-Dimensional Fourier Map in X-ray Crystallography

ERIC Educational Resources Information Center

Clegg, William

2004-01-01

The teaching of crystal structure determination with single-crystal X-ray diffraction at undergraduate level faces numerous challenges. Single-crystal X-ray diffraction is used in a vast range of chemical research projects and forms the basis for a high proportion of structural results that are presented to high-school, undergraduate, and graduate…

X-ray crystallography

NASA Technical Reports Server (NTRS)

2001-01-01

X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

Transition metal coordination polymers based on tetrabromoterephthalic and bis(imidazole) ligands: Syntheses, structures, topological analysis and photoluminescence properties

NASA Astrophysics Data System (ADS)

Zhang, Xiaowei; Xing, Peiqi; Geng, Xiujuan; Sun, Daofeng; Xiao, Zhenyu; Wang, Lei

2015-09-01

Eight new coordination polymers (CPs), namely, [Zn(1,2-mbix)(tbtpa)]n (1), [Co(1,2-mbix)(tbtpa)]n (2), [CdCl(1,2-mbix)(tbtpa)0.5]n (3), {[Cd(1,2-bix)(tbtpa)]·H2O}n (4), {[Cd0.5(1,2-bix)(tbtpa)0.5]·H2O}n (5), {[Co0.5(1,2-bix)(tbtpa)0.5]·2H2O}n (6), {[Co(1,2-bix)(tbtpa)]·H2O}n (7) and {[Co(1,2-bix)(tbtpa)]·Diox·2H2O}n (8), were synthesized under solvothermal conditions based on mix-ligand strategy (H2tbtpa=tetrabromoterephthalic acid and 1,2-mbix=1,2-bis((2-methyl-1H-imidazol-1-yl)methyl)benzene, 1,2-bix=1,2-bis(imidazol-1-ylmethyl)benzene). All of the CPs have been structurally characterized by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectroscopy, powder X-ray diffraction (PXRD), and thermogravimetric analyses (TGA). X-ray diffraction analyses show that 1 and 2 are isotypics which have 2D highly undulated networks with (4,4)-sql topology with the existence of C-H ⋯Br interactions; for 3, it has a 2D planar network with (4,4)-sql topology with the occurrence of C-H ⋯Cl interactions other than C-H ⋯Br interactions; 4 shows a 3D 2-fold interpenetrated nets with rare 65·8-mok topology which has a self-catention property. As the same case as 1 and 2, 5 and 6 are also isostructural with planar layers with 44-sql topology which further assembled into 3D supramolecular structure through the interdigitated stacking fashion and the C-Br ⋯Cph interactions. As for 7, it has a 2D slightly undulated networks with (4,4)-sql topology which has one dimension channel. While 8 has a 2-fold interpenetrated networks with (3,4)-connect jeb topology with point symbol {63}{65·8}. And their structures can be tuned by conformations of bis(imidazol) ligands and solvent mixture. Besides, the TGA properties for all compounds and the luminescent properties for 1, 3, 4, 5 are discussed in detail.

Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

Treesearch

Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

2005-01-01

The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

3D/4D analyses of damage and fracture behaviours in structural materials via synchrotron X-ray tomography.

PubMed

Toda, Hiroyuki

2014-11-01

X-ray microtomography has been utilized for the in-situ observation of various structural metals under external loading. Recent advances in X-ray microtomography provide remarkable tools to image the interior of materials. In-situ X-ray microtomography provides a unique possibility to access the 3D character of internal microstructure and its time evolution behaviours non-destructively, thereby enabling advanced techniques for measuring local strain distribution. Local strain mapping is readily enabled by processing such high-resolution tomographic images either by the particle tracking technique or the digital image correlation technique [1]. Procedures for tracking microstructural features which have been developed by the authors [2], have been applied to analyse localised deformation and damage evolution in a material [3]. Typically several tens of thousands of microstructural features, such as particles and pores, are tracked in a tomographic specimen (0.2 - 0.3 mm(3) in volume). When a sufficient number of microstructural features is dispersed in 3D space, the Delaunay tessellation algorithm is used to obtain local strain distribution. With these techniques, 3D strain fields can be measured with reasonable accuracy. Even local crack driving forces, such as local variations in the stress intensity factor, crack tip opening displacement and J integral along a crack front line, can be measured from discrete crack tip displacement fields [4]. In the present presentation, complicated crack initiation and growth behaviour and the extensive formation of micro cracks ahead of a crack tip are introduced as examples.A novel experimental method has recently been developed by amalgamating a pencil beam X-Ray diffraction (XRD) technique with the microstructural tracking technique [5]. The technique provides information about individual grain orientations and 1-micron-level grain morphologies in 3D together with high-density local strain mapping. The application of this technique to the deformation behavior of a polycrystalline aluminium alloy will be demonstrated in the presentation [6].The synchrotron-based microtomography has been mainly utilized to light materials due to their good X-ray transmission. In the present talk, the application of the synchrotron-based microtomography to steels will be also introduced. Degradation of contrast and spatial resolution due to forward scattering could be avoided by selecting appropriate experimental conditions in order to obtain superior spatial resolution close to the physical limit even in ferrous materials [7]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Differences observed in the surface morphology and microstructure of Ni-Fe-Cu ternary thin films electrochemically deposited at low and high applied current densities

NASA Astrophysics Data System (ADS)

Sarac, U.; Kaya, M.; Baykul, M. C.

2016-10-01

In this research, nanocrystalline Ni-Fe-Cu ternary thin films using electrochemical deposition technique were produced at low and high applied current densities onto Indium Tin Oxide (ITO) coated conducting glass substrates. Change of surface morphology and microstructural properties of the films were investigated. Energy dispersive X-ray spectroscopy (EDX) measurements showed that the Ni-Fe-Cu ternary thin films exhibit anomalous codeposition behaviour during the electrochemical deposition process. From the X-ray diffraction (XRD) analyses, it was revealed that there are two segregated phases such as Cu- rich and Ni-rich within the films. The crystallographic structure of the films was face-centered cubic (FCC). It was also observed that the film has lower lattice micro-strain and higher texture degree at high applied current density. Scanning electron microscopy (SEM) studies revealed that the films have rounded shape particles on the base part and cauliflower-like structures on the upper part. The film electrodeposited at high current density had considerably smaller rounded shape particles and cauliflower-like structures. From the atomic force microscopy (AFM) analyses, it was shown that the film deposited at high current density has smaller particle size and surface roughness than the film grown at low current density.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Yan; Pan, Cheng-Ling; Xiao, Li-Na

Three new supramolecular compounds based on triethylenediamine and different polyoxometalates [W{sup VI}{sub 3}V{sup V}{sub 3}O{sub 19}H]{l_brace}[Cu(HDABCO)]{sub 2}(H{sub 2}O){r_brace} (1), [P{sub 2}Mo{sup VI}{sub 18}O{sub 62}][HDABCO]{sub 2}[H{sub 2}DABCO]{sub 2}.12 H{sub 2}O (2) and [Mo{sup VI}{sub 7.5}W{sup VI}{sub 0.5}O{sub 27}][Cu(HDABCO)]{sub 2}.2 H{sub 3}O.2 H{sub 2}O (3) (DABCO=triethylenediamine) have been synthesized hydrothermally and characterized by IR, TG, XPS and X-ray diffraction analyses. Crystal structure analyses reveal that compound 1 exhibits a face-centered cubic packing motif, compound 2 displays a supramolecular structure constructed form the 'chains' arranged hexagonally, compound 3 contains [Mo{sub 7.5}W{sub 0.5}O{sub 27}]{sub {infinity}} chain decorated by [Cu(HDABCO)]{sup 2+} cations, which was thenmore » packed into a layer structure. These results show that the same organonitrogen combining with the different POMs will yield different supramolecular networks. -- Graphical abstract: Three new supramolecular compounds based on triethylenediamine and different polyoxometalates have been hydrothermally synthesized and characterized by IR, XPS, TG, elemental analysis and X-ray diffraction analysis.« less

Structural and magnetic properties of multi-core nanoparticles analysed using a generalised numerical inversion method

PubMed Central

Bender, P.; Bogart, L. K.; Posth, O.; Szczerba, W.; Rogers, S. E.; Castro, A.; Nilsson, L.; Zeng, L. J.; Sugunan, A.; Sommertune, J.; Fornara, A.; González-Alonso, D.; Barquín, L. Fernández; Johansson, C.

2017-01-01

The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions. PMID:28397851

Synthesis and photoluminescence properties of silver(I) complexes based on N-benzoyl-L-glutamic acid and N-donor ligands with different flexibility

NASA Astrophysics Data System (ADS)

Yan, Ming-Jie; Feng, Qi; Song, Hui-Hua

2016-05-01

By changing the N-donor ancillary ligand, three novel silver (I) complexes {[Ag(HbzgluO) (4,4‧-bipy)]·H2O}n (1), {[Ag2(HbzgluO)2 (bpe)2]·2H2O}n (2) and {[Ag(HbzgluO)(bpp)]·2H2O}n (3) (H2bzgluO = N-benzoyl-L-glutamic acid, 4,4‧-bipy = 4,4ˊ-bipyridine, bpe = 1,2-di(4-pyridyl)ethane, bpp = 1,3-di(4-pyridyl)propane) were synthesized. Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectra, powder X-ray diffraction (PXRD), and thermogravimetric analyses (TGA). In this study, the N-donor ligands are changed from rigidity (4,4‧-bipy), quasi-flexibility (bpe) to flexibility (bpp), the structures of complexes also change. Complex 1 features a 1D chain structure which is further linked together to construct a 2D supramolecular structure through hydrogen bonds. Complex 2 is a 1D double-chains configuration which eventually forms a 3D supramolecular network via hydrogen bonding interactions. Whereas, complex 3 exhibits a 2D pleated grid structure which is linked by hydrogen bonding interactions into a 3D supramolecular network. The present observations demonstrate that the modulation of coordination polymers with different structures can accomplish by changing the spacer length of N-donor ligands. In addition, the solid-state circular dichroism (CD) spectra indicated that compound 2 exhibited negative cotton effect which originated from the chiral ligands H2bzgluO and the solid-state fluorescence spectra of the three complexes demonstrated the auxiliary ligands have influence on the photoluminescence properties of the complexes.

X-ray (image)

MedlinePlus

X-rays are a form of electromagnetic radiation, just like visible light. Structures that are dense (such as bone) will block most of the x-ray particles, and will appear white. Metal and contrast media ( ...

Structural investigation of Mimosa pudica Linn fibre

NASA Astrophysics Data System (ADS)

Patra, S. R.; Pattojoshi, P.; Tiwari, T. N.; Mallick, B.

2017-04-01

Sensitive plant ( Mimosa pudica Linn.) fibre is a natural fibre with electrically conductive property. Because of its electro-active sensing nature, it has been found very interesting among physicists, chemists, biologists, material scientists and technologists. So far as our knowledge is concerned; there is no report on the X-ray structure of M. pudica fibre using diffraction technique. In the present report, the M. pudica fibre has been extracted from the stem of the herb by sinking the stem in 10% NaOH solution for one week. The diffraction pattern of the fibre is found out to be cellulose-I. The effect of the fibre structure and its orientation due to different mounting have been investigated using X-ray diffraction technique. The I max of cellulose-I has been observed along (002) and (10\\overline{1)} for the perpendicular and parallel mounting of the native-fibre, respectively. Full width at half maxima of the diffraction profile turns out to be decreased with fibre orientation. Dimension of crystallite size D hkl estimated in the perpendicular mounting D_{hkl}^{ \\bot } is more as compared to that of the parallel mounting D_{hkl}^{{^{allel } }}. The smallest crystallite sizes observed in both parallel and perpendicular mounting are 18.78 and 30.78 Å respectively. It is expected that the present study may help to analyse the X-ray diffraction of fibre materials in general and natural fibres in particular.

Detection of Reaction Intermediates in Mg2+-Dependent DNA Synthesis and RNA Degradation by Time-Resolved X-Ray Crystallography.

PubMed

Samara, Nadine L; Gao, Yang; Wu, Jinjun; Yang, Wei

2017-01-01

Structures of enzyme-substrate/product complexes have been studied for over four decades but have been limited to either before or after a chemical reaction. Recently using in crystallo catalysis combined with X-ray diffraction, we have discovered that many enzymatic reactions in nucleic acid metabolism require additional metal ion cofactors that are not present in the substrate or product state. By controlling metal ions essential for catalysis, the in crystallo approach has revealed unprecedented details of reaction intermediates. Here we present protocols used for successful studies of Mg 2+ -dependent DNA polymerases and ribonucleases that are applicable to analyses of a variety of metal ion-dependent reactions. © 2017 Elsevier Inc. All rights reserved.

Mono- and bi-functional arenethiols as surfactants for gold nanoparticles: synthesis and characterization

PubMed Central

2011-01-01

Stable gold nanoparticles stabilized by different mono and bi-functional arenethiols, namely, benzylthiol and 1,4-benzenedimethanethiol, have been prepared by using a modified Brust's two-phase synthesis. The size, shape, and crystalline structure of the gold nanoparticles have been determined by high-resolution electron microscopy and full-pattern X-ray powder diffraction analyses. Nanocrystals diameters have been tuned in the range 2 ÷ 9 nm by a proper variation of Au/S molar ratio. The chemical composition of gold nanoparticles and their interaction with thiols have been investigated by X-ray photoelectron spectroscopy. In particular, the formation of networks has been observed with interconnected gold nanoparticles containing 1,4-benzenedimethanethiol as ligand. PMID:21711615

A multiple technique approach to the analysis of urinary calculi.

PubMed

Rodgers, A L; Nassimbeni, L R; Mulder, K J

1982-01-01

10 urinary calculi have been qualitatively and quantitatively analysed using X-ray diffraction, infra-red, scanning electron microscopy, X-ray fluorescence, atomic absorption and density gradient procedures. Constituents and compositional features which often go undetected due to limitations in the particular analytical procedure being used, have been identified and a detailed picture of each stone's composition and structure has been obtained. In all cases at least two components were detected suggesting that the multiple technique approach might cast some doubt as to the existence of "pure" stones. Evidence for a continuous, non-sequential deposition mechanism has been detected. In addition, the usefulness of each technique in the analysis of urinary stones has been assessed and the multiple technique approach has been evaluated as a whole.

Synthesis of noble metal/carbon nanotube composites in supercritical methanol.

PubMed

Sun, Zhenyu; Fu, Lei; Liu, Zhimin; Han, Buxing; Liu, Yunqi; Du, Jimin

2006-03-01

A simple and efficient route has been employed to deposit noble metal nanoparticles (Pt, Ru, Pt-Ru, Rh, Ru-Sn) onto carbon nanotubes (CNTs) in supercritical methanol solution. In this method, the inorganic metallic salts acted as metal precursors, and methanol as solvent as well as reductant for the precursors. The as-prepared nanocomposites were structurally and morphologically characterized by X-ray diffraction spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy, and X-ray photoelectron spectroscopy analyses. It was demonstrated that the CNTs were decorated by crystalline metal nanoparticles with uniform sizes and a narrow particle size distribution. The size and loading content of the nanoparticles on CNTs could be tuned by manipulating reaction parameters. Furthermore, the formation mechanism of the composites was also discussed.

A comparison of coronal X-ray structures of active regions with magnetic fields computed from photospheric observations

NASA Technical Reports Server (NTRS)

Poletto, G.; Vaiana, G. S.; Zombeck, M. V.; Krieger, A. S.; Timothy, A. F.

1975-01-01

The appearances of several X-ray active regions observed on March 7, 1970 and June 15, 1973 are compared with the corresponding coronal magnetic-field topology. Coronal fields have been computed from measurements of the longitudinal component of the underlying magnetic fields, based on the current-free hypothesis. An overall correspondence between X-ray structures and calculated field lines is established, and the magnetic counterparts of different X-ray features are also examined. A correspondence between enhanced X-ray emission and the location of compact closed field lines is suggested. Representative magnetic-field values calculated under the assumption of current-free fields are given for heights up to 200 sec.

Beyond crystallography: Diffractive imaging using coherent x-ray light sources

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miao, J.; Ishikawa, T.; Robinson, I. K.

X-ray crystallography has been central to the development of many fields of science over the past century. It has now matured to a point that as long as good-quality crystals are available, their atomic structure can be routinely determined in three dimensions. However, many samples in physics, chemistry, materials science, nanoscience, geology, and biology are noncrystalline, and thus their three-dimensional structures are not accessible by traditional x-ray crystallography. Overcoming this hurdle has required the development of new coherent imaging methods to harness new coherent x-ray light sources. Here we review the revolutionary advances that are transforming x-ray sources and imagingmore » in the 21st century.« less

X-ray Radiative Transfer in Protoplanetary Disks with ProDiMo

NASA Astrophysics Data System (ADS)

Rab, Christian; Woitke, Peter; Güdel, Manuel; Min, Michiel; Diana Team

2013-07-01

X-ray emission is a common property of YSOs. T Tauri stars show X-ray luminosities up to 10^32 erg/s but also Herbig Ae/Be stars can have moderate X-ray emission in the range of 10^28 to 10^31 erg/s. We want to investigate the impact of X-ray radiation on the thermal and chemical structure of protoplanetary discs around these YSOs. Therefore we have added a new X-ray Radiative Transfer module to the radiation thermo-chemical code ProDiMo (Protoplanetary Disc Modeling) extending the existing implementation of X-ray chemistry implemented by Aresu et al. This new module considers gas and dust opacities (including scattering) and a possible X-ray background field. Further we added a new set of FUV - photoreactions to the X-ray chemistry module of ProDiMo as fast electrons created in X-ray ionisation can produce a significant secondary FUV radiation field by exciting atomic or molecular hydrogen. We discuss the importance of these processes on the thermal and chemical structure of the protoplanetary disc, and present them on the basis of a typical T Tauri disc model. This work is performed in the context of the EU FP7-project DIANA (www.diana-project.com).

Improving material identification by combining x-ray and neutron tomography

NASA Astrophysics Data System (ADS)

LaManna, Jacob M.; Hussey, Daniel S.; Baltic, Eli; Jacobson, David L.

2017-09-01

X-rays and neutrons provide complementary non-destructive probes for the analysis of structure and chemical composition of materials. Contrast differences between the modes arise due to the differences in interaction with matter. Due to the high sensitivity to hydrogen, neutrons excel at separating liquid water or hydrogenous phases from the underlying structure while X-rays resolve the solid structure. Many samples of interest, such as fluid flow in porous materials or curing concrete, are stochastic or slowly changing with time which makes analysis of sequential imaging with X-rays and neutrons difficult as the sample may change between scans. To alleviate this issue, NIST has developed a system for simultaneous X-ray and neutron tomography by orienting a 90 keVpeak micro-focus X-ray tube orthogonally to a thermal neutron beam. This system allows for non-destructive, multimodal tomography of dynamic or stochastic samples while penetrating through sample environment equipment such as pressure and flow vessels. Current efforts are underway to develop methods for 2D histogram based segmentation of reconstructed volumes. By leveraging the contrast differences between X-rays and neutrons, greater histogram peak separation can occur in 2D vs 1D enabling improved material identification.

Probing the Hot and Energetic Universe: X-rays and Astrophysics

NASA Astrophysics Data System (ADS)

Bautz, Marshall; Kraft, Ralph

2016-03-01

X-ray observations are a cornerstone of our understanding of the formation and evolution of structure in the Universe, from solar-system-sized supermassive black holes (SMBH) to the largest galaxy clusters. At the most basic level, a significant fraction of the energy output in the Universe is in X-rays, and much of this emission traces the response of baryonic matter to the inexorable, gravity-driven growth of cosmic structure. At present, for example, half or more of the baryons in the Universe reside in a hot (>1 MK) X-ray-emitting phase. We discuss some of the remarkable progress that has been made in understanding the broad outlines of these processes with the current generation of X-ray observatories. We summarize the potential of recently launched and forthcoming X-ray observatories to track the development of large-scale cosmic structure and to understand the physics linking the growth of SMBH with that of the (many orders of magnitude larger) galaxies and clusters which host them. We briefly review nearer-term prospects for smaller, focussed missions, including one that will soon exploit pulsating X-ray emission from neutron stars to probe the equation of state of matter at nuclear densities.

Quantitative X-ray diffraction and fluorescence analysis of paint pigment systems : final report.

DOT National Transportation Integrated Search

1978-01-01

This study attempted to correlate measured X-ray intensities with concentrations of each member of paint pigment systems, thereby establishing calibration curves for the quantitative analyses of such systems.

Novel drift structures for silicon and compound semiconductor X-ray and gamma-ray detectors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patt, B.E.; Iwanczyk, J.S.

Recently developed silicon- and compound-semiconductor-based drift detector structures have produced excellent performance for charged particles, X-rays, and gamma rays and for low-signal visible light detection. The silicon drift detector (SDD) structures that the authors discuss relate to direct X-ray detectors and scintillation photon detectors coupled with scintillators for gamma rays. Recent designs include several novel features that ensure very low dark current and hence low noise. In addition, application of thin window technology ensures a very high quantum efficiency entrance window on the drift photodetector. The main features of the silicon drift structures for X rays and light detection aremore » very small anode capacitance independent of the overall detector size, low noise, and high throughput. To take advantage of the small detector capacitance, the first stage of the electronics needs to be integrated into the detector anode. In the gamma-ray application, factors other than electronic noise dominate, and there is no need to integrate the electronics into the anode. Thus, a different drift structure is needed in conjunction with a high-Z material. The main features in this case are large active detector volume and electron-only induced signal.« less

Nucleoplasmin-like domain of FKBP39 from Drosophila melanogaster forms a tetramer with partly disordered tentacle-like C-terminal segments

PubMed Central

Kozłowska, Małgorzata; Tarczewska, Aneta; Jakób, Michał; Bystranowska, Dominika; Taube, Michał; Kozak, Maciej; Czarnocki-Cieciura, Mariusz; Dziembowski, Andrzej; Orłowski, Marek; Tkocz, Katarzyna; Ożyhar, Andrzej

2017-01-01

Nucleoplasmins are a nuclear chaperone family defined by the presence of a highly conserved N-terminal core domain. X-ray crystallographic studies of isolated nucleoplasmin core domains revealed a β-propeller structure consisting of a set of five monomers that together form a stable pentamer. Recent studies on isolated N-terminal domains from Drosophila 39-kDa FK506-binding protein (FKBP39) and from other chromatin-associated proteins showed analogous, nucleoplasmin-like (NPL) pentameric structures. Here, we report that the NPL domain of the full-length FKBP39 does not form pentameric complexes. Multi-angle light scattering (MALS) and sedimentation equilibrium ultracentrifugation (SE AUC) analyses of the molecular mass of the full-length protein indicated that FKBP39 forms homotetrameric complexes. Molecular models reconstructed from small-angle X-ray scattering (SAXS) revealed that the NPL domain forms a stable, tetrameric core and that FK506-binding domains are linked to it by intrinsically disordered, flexible chains that form tentacle-like segments. Analyses of full-length FKBP39 and its isolated NPL domain suggested that the distal regions of the polypeptide chain influence and determine the quaternary conformation of the nucleoplasmin-like protein. These results provide new insights regarding the conserved structure of nucleoplasmin core domains and provide a potential explanation for the importance of the tetrameric structural organization of full-length nucleoplasmins. PMID:28074868

The Chandra Deep Field-North Survey and the cosmic X-ray background.

PubMed

Brandt, W Nielsen; Alexander, David M; Bauer, Franz E; Hornschemeier, Ann E

2002-09-15

Chandra has performed a 1.4 Ms survey centred on the Hubble Deep Field-North (HDF-N), probing the X-ray Universe 55-550 times deeper than was possible with pre-Chandra missions. We describe the detected point and extended X-ray sources and discuss their overall multi-wavelength (optical, infrared, submillimetre and radio) properties. Special attention is paid to the HDF-N X-ray sources, luminous infrared starburst galaxies, optically faint X-ray sources and high-to-extreme redshift active galactic nuclei. We also describe how stacking analyses have been used to probe the average X-ray-emission properties of normal and starburst galaxies at cosmologically interesting distances. Finally, we discuss plans to extend the survey and argue that a 5-10 Ms Chandra survey would lay key groundwork for future missions such as XEUS and Generation-X.

Attosecond time-energy structure of X-ray free-electron laser pulses

NASA Astrophysics Data System (ADS)

Hartmann, N.; Hartmann, G.; Heider, R.; Wagner, M. S.; Ilchen, M.; Buck, J.; Lindahl, A. O.; Benko, C.; Grünert, J.; Krzywinski, J.; Liu, J.; Lutman, A. A.; Marinelli, A.; Maxwell, T.; Miahnahri, A. A.; Moeller, S. P.; Planas, M.; Robinson, J.; Kazansky, A. K.; Kabachnik, N. M.; Viefhaus, J.; Feurer, T.; Kienberger, R.; Coffee, R. N.; Helml, W.

2018-04-01

The time-energy information of ultrashort X-ray free-electron laser pulses generated by the Linac Coherent Light Source is measured with attosecond resolution via angular streaking of neon 1s photoelectrons. The X-ray pulses promote electrons from the neon core level into an ionization continuum, where they are dressed with the electric field of a circularly polarized infrared laser. This induces characteristic modulations of the resulting photoelectron energy and angular distribution. From these modulations we recover the single-shot attosecond intensity structure and chirp of arbitrary X-ray pulses based on self-amplified spontaneous emission, which have eluded direct measurement so far. We characterize individual attosecond pulses, including their instantaneous frequency, and identify double pulses with well-defined delays and spectral properties, thus paving the way for X-ray pump/X-ray probe attosecond free-electron laser science.

A long-term space astrophysics research program: An x-ray perspective of the components and structure of galaxies

NASA Technical Reports Server (NTRS)

Fabbiano, G.

1995-01-01

X-ray studies of galaxies by the Smithsonian Astrophysical Observatory (SAO) and MIT are described. Activities at SAO include ROSAT PSPC x-ray data reduction and analysis pipeline; x-ray sources in nearby Sc galaxies; optical, x-ray, and radio study of ongoing galactic merger; a radio, far infrared, optical, and x-ray study of the Sc galaxy NGC247; and a multiparametric analysis of the Einstein sample of early-type galaxies. Activities at MIT included continued analysis of observations with ROSAT and ASCA, and continued development of new approaches to spectral analysis with ASCA and AXAF. Also, a new method for characterizing structure in galactic clusters was developed and applied to ROSAT images of a large sample of clusters. An appendix contains preprints generated by the research.

High precision detector robot arm system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shu, Deming; Chu, Yong

A method and high precision robot arm system are provided, for example, for X-ray nanodiffraction with an X-ray nanoprobe. The robot arm system includes duo-vertical-stages and a kinematic linkage system. A two-dimensional (2D) vertical plane ultra-precision robot arm supporting an X-ray detector provides positioning and manipulating of the X-ray detector. A vertical support for the 2D vertical plane robot arm includes spaced apart rails respectively engaging a first bearing structure and a second bearing structure carried by the 2D vertical plane robot arm.

Sub-arcsecond observations of the solar X-ray corona

NASA Technical Reports Server (NTRS)

Golub, L.; Nystrom, G.; Herant, M.; Kalata, K.; Lovas, I.

1990-01-01

Results from a high-resolution multi-layer-coated X-ray imaging telescope, part of the Normal Incidence X-ray Telescope sounding rocket payload are presented. Images of the peak of a two-ribbon flare showed detailed structure within each ribbon, as well as the expected bright arches of emission connecting the ribbons. The number of X-ray bright points is small, consistent with predictions based on the previous solar cycle. Topology of the magnetic structure is complex and highly tangled, implying that the magnetic complexity of the photosphere is paralleled in the corona.

Anti-Stokes resonant x-ray Raman scattering for atom specific and excited state selective dynamics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kunnus, Kristjan; Josefsson, Ida; Rajkovic, Ivan

Here, ultrafast electronic and structural dynamics of matter govern rate and selectivity of chemical reactions, as well as phase transitions and efficient switching in functional materials. Since x-rays determine electronic and structural properties with elemental, chemical, orbital and magnetic selectivity, short pulse x-ray sources have become central enablers of ultrafast science. Despite of these strengths, ultrafast x-rays have been poor at picking up excited state moieties from the unexcited ones. With time-resolved anti-Stokes resonant x-ray Raman scattering (AS-RXRS) performed at the LCLS, and ab initio theory we establish background free excited state selectivity in addition to the elemental, chemical, orbitalmore » and magnetic selectivity of x-rays. This unparalleled selectivity extracts low concentration excited state species along the pathway of photo induced ligand exchange of Fe(CO)5 in ethanol. Conceptually a full theoretical treatment of all accessible insights to excited state dynamics with AS-RXRS with transform-limited x-ray pulses is given—which will be covered experimentally by upcoming transform-limited x-ray sources.« less

Anti-Stokes resonant x-ray Raman scattering for atom specific and excited state selective dynamics

DOE PAGES

Kunnus, Kristjan; Josefsson, Ida; Rajkovic, Ivan; ...

2016-10-07

Here, ultrafast electronic and structural dynamics of matter govern rate and selectivity of chemical reactions, as well as phase transitions and efficient switching in functional materials. Since x-rays determine electronic and structural properties with elemental, chemical, orbital and magnetic selectivity, short pulse x-ray sources have become central enablers of ultrafast science. Despite of these strengths, ultrafast x-rays have been poor at picking up excited state moieties from the unexcited ones. With time-resolved anti-Stokes resonant x-ray Raman scattering (AS-RXRS) performed at the LCLS, and ab initio theory we establish background free excited state selectivity in addition to the elemental, chemical, orbitalmore » and magnetic selectivity of x-rays. This unparalleled selectivity extracts low concentration excited state species along the pathway of photo induced ligand exchange of Fe(CO)5 in ethanol. Conceptually a full theoretical treatment of all accessible insights to excited state dynamics with AS-RXRS with transform-limited x-ray pulses is given—which will be covered experimentally by upcoming transform-limited x-ray sources.« less

A nearly on-axis spectroscopic system for simultaneously measuring UV-visible absorption and X-ray diffraction in the SPring-8 structural genomics beamline.

PubMed

Sakaguchi, Miyuki; Kimura, Tetsunari; Nishida, Takuma; Tosha, Takehiko; Sugimoto, Hiroshi; Yamaguchi, Yoshihiro; Yanagisawa, Sachiko; Ueno, Go; Murakami, Hironori; Ago, Hideo; Yamamoto, Masaki; Ogura, Takashi; Shiro, Yoshitsugu; Kubo, Minoru

2016-01-01

UV-visible absorption spectroscopy is useful for probing the electronic and structural changes of protein active sites, and thus the on-line combination of X-ray diffraction and spectroscopic analysis is increasingly being applied. Herein, a novel absorption spectrometer was developed at SPring-8 BL26B2 with a nearly on-axis geometry between the X-ray and optical axes. A small prism mirror was placed near the X-ray beamstop to pass the light only 2° off the X-ray beam, enabling spectroscopic analysis of the X-ray-exposed volume of a crystal during X-ray diffraction data collection. The spectrometer was applied to NO reductase, a heme enzyme that catalyzes NO reduction to N2O. Radiation damage to the heme was monitored in real time during X-ray irradiation by evaluating the absorption spectral changes. Moreover, NO binding to the heme was probed via caged NO photolysis with UV light, demonstrating the extended capability of the spectrometer for intermediate analysis.

Analysis of solar X-ray data

NASA Technical Reports Server (NTRS)

Teske, R. G.

1972-01-01

Type III solar bursts occurring in the absence of solar flares were observed to be accompanied by weak X-radiation. The energy scale of an OSO-3 soft X-ray ion chamber was assessed using realistic theoretical X-ray spectra. Relationships between soft solar X-rays and solar activity were investigated. These included optical studies, the role of the Type III acceleration mechanism in establishing the soft X-ray source volume, H alpha flare intensity variations, and gross magnetic field structure.

Identification of a new androgen receptor (AR) co-regulator BUD31 and related peptides to suppress wild-type and mutated AR-mediated prostate cancer growth via peptide screening and X-ray structure analysis.

PubMed

Hsu, Cheng-Lung; Liu, Jai-Shin; Wu, Po-Long; Guan, Hong-Hsiang; Chen, Yuh-Ling; Lin, An-Chi; Ting, Huei-Ju; Pang, See-Tong; Yeh, Shauh-Der; Ma, Wen-Lung; Chen, Chung-Jung; Wu, Wen-Guey; Chang, Chawnshang

2014-12-01

Treatment with individual anti-androgens is associated with the development of hot-spot mutations in the androgen receptor (AR). Here, we found that anti-androgens-mt-ARs have similar binary structure to the 5α-dihydrotestosterone-wt-AR. Phage display revealed that these ARs bound to similar peptides, including BUD31, containing an Fxx(F/H/L/W/Y)Y motif cluster with Tyr in the +5 position. Structural analyses of the AR-LBD-BUD31 complex revealed formation of an extra hydrogen bond between the Tyr+5 residue of the peptide and the AR. Functional studies showed that BUD31-related peptides suppressed AR transactivation, interrupted AR N-C interaction, and suppressed AR-mediated cell growth. Combination of peptide screening and X-ray structure analysis may serve as a new strategy for developing anti-ARs that simultaneously suppress both wt and mutated AR function. Copyright © 2014 Federation of European Biochemical Societies. Published by Elsevier B.V. All rights reserved.

X-ray Structural and Biological Evaluation of a Series of Potent and Highly Selective Inhibitors of Human Coronavirus Papain-like Proteases

PubMed Central

2015-01-01

Structure-guided design was used to generate a series of noncovalent inhibitors with nanomolar potency against the papain-like protease (PLpro) from the SARS coronavirus (CoV). A number of inhibitors exhibit antiviral activity against SARS-CoV infected Vero E6 cells and broadened specificity toward the homologous PLP2 enzyme from the human coronavirus NL63. Selectivity and cytotoxicity studies established a more than 100-fold preference for the coronaviral enzyme over homologous human deubiquitinating enzymes (DUBs), and no significant cytotoxicity in Vero E6 and HEK293 cell lines is observed. X-ray structural analyses of inhibitor-bound crystal structures revealed subtle differences between binding modes of the initial benzodioxolane lead (15g) and the most potent analogues 3k and 3j, featuring a monofluoro substitution at para and meta positions of the benzyl ring, respectively. Finally, the less lipophilic bis(amide) 3e and methoxypyridine 5c exhibit significantly improved metabolic stability and are viable candidates for advancing to in vivo studies. PMID:24568342

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Energy Astronomy Observatory, Mission C, Phase A. Volume 2: Preliminary analyses and conceptual design

NASA Technical Reports Server (NTRS)

1972-01-01

An analysis and conceptual design of a baseline mission and spacecraft are presented. Aspects of the HEAO-C discussed include: baseline experiments with X-ray observations of space, analysis of mission requirements, observatory design, structural analysis, thermal control, attitude sensing and control system, communication and data handling, and space shuttle launch and retrieval of HEAO-C.

Structural and elemental changes in glioblastoma cells in situ: complementary imaging with high resolution visible light- and X-ray microscopy

DOE PAGES

Ducic, Tanja; Paunesku, Tatjana; Chen, Si; ...

2016-12-09

The glioblastoma (GBM) is characterized by a short median survival and an almost 100% tumor related mortality. GBM cells exhibit highly invasive behavior whose mechanisms are not yet fully understood. The present study explores application of X-ray and visible light microscopy to display the elemental and structural images of cells from 3 patient derived GMB samples and an established GMB cell line. Slight differences in elemental concentrations, in actin cytoskeleton organization and cell morphology were noted between all cells types by X-ray fluorescence and full field soft X-ray microscopy, as well as the Structured Illumination Super-resolution Microscope (SIM). Different samplemore » preparation approaches were used to match each imaging technique. While preparation for SIM included cell fixation and staining, intact frozen hydrated cells were used for the trace element imaging by hard X-ray fluorescence and exploration of the structural features by soft X-ray absorption tomography. In conclusion, each technique documented differences between samples with regard to morphology and elemental composition and underscored the importance of use of multiple patient derived samples for detailed GBM study.« less

A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

NASA Astrophysics Data System (ADS)

Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

2017-10-01

Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

Structural and elemental changes in glioblastoma cells in situ: complementary imaging with high resolution visible light- and X-ray microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ducic, Tanja; Paunesku, Tatjana; Chen, Si

The glioblastoma (GBM) is characterized by a short median survival and an almost 100% tumor related mortality. GBM cells exhibit highly invasive behavior whose mechanisms are not yet fully understood. The present study explores application of X-ray and visible light microscopy to display the elemental and structural images of cells from 3 patient derived GMB samples and an established GMB cell line. Slight differences in elemental concentrations, in actin cytoskeleton organization and cell morphology were noted between all cells types by X-ray fluorescence and full field soft X-ray microscopy, as well as the Structured Illumination Super-resolution Microscope (SIM). Different samplemore » preparation approaches were used to match each imaging technique. While preparation for SIM included cell fixation and staining, intact frozen hydrated cells were used for the trace element imaging by hard X-ray fluorescence and exploration of the structural features by soft X-ray absorption tomography. In conclusion, each technique documented differences between samples with regard to morphology and elemental composition and underscored the importance of use of multiple patient derived samples for detailed GBM study.« less

X-ray Diffraction from Membrane Protein Nanocrystals

PubMed Central

Hunter, M.S.; DePonte, D.P.; Shapiro, D.A.; Kirian, R.A.; Wang, X.; Starodub, D.; Marchesini, S.; Weierstall, U.; Doak, R.B.; Spence, J.C.H.; Fromme, P.

2011-01-01

Membrane proteins constitute >30% of the proteins in an average cell, and yet the number of currently known structures of unique membrane proteins is <300. To develop new concepts for membrane protein structure determination, we have explored the serial nanocrystallography method, in which fully hydrated protein nanocrystals are delivered to an x-ray beam within a liquid jet at room temperature. As a model system, we have collected x-ray powder diffraction data from the integral membrane protein Photosystem I, which consists of 36 subunits and 381 cofactors. Data were collected from crystals ranging in size from 100 nm to 2 μm. The results demonstrate that there are membrane protein crystals that contain <100 unit cells (200 total molecules) and that 3D crystals of membrane proteins, which contain <200 molecules, may be suitable for structural investigation. Serial nanocrystallography overcomes the problem of x-ray damage, which is currently one of the major limitations for x-ray structure determination of small crystals. By combining serial nanocrystallography with x-ray free-electron laser sources in the future, it may be possible to produce molecular-resolution electron-density maps using membrane protein crystals that contain only a few hundred or thousand unit cells. PMID:21190672

Crystal growth, structural, optical, spectral and thermal studies of tris(L-phenylalanine)L-phenylalaninium nitrate: a new organic nonlinear optical material.

PubMed

Prakash, M; Geetha, D; Lydia Caroline, M

2011-10-15

Tris(L-phenylalanine)L-phenylalaninium nitrate, C(9)H(12)NO(2)(+)·NO(3)(-)·3C(9)H(11)NO(2) (TPLPN), a new organic nonlinear optical material was grown from aqueous solution by slow evaporation solution growth at room temperature. The grown crystals were subjected to powder X-ray diffraction and single crystal X-ray diffraction studies to confirm the crystalline nature and crystal structure. The modes of vibration of different molecular groups present in TPLPN have been identified by FTIR spectral analysis. The presence of hydrogen and carbon in the grown crystal were confirmed by using proton and carbon nuclear magnetic resonance (NMR) spectral analyses. The optical transmission spectral study establishes good transmitting ability of the crystal in the entire visible region. The thermogravimetric (TG) and differential thermal analyses (DTA) were carried out to understand the thermal stability of the sample. The nonlinear optical property of the compound observed using Kurtz powder second harmonic generation test assets the suitability of the grown material for the frequency conversion of laser radiation of Nd:YAG. Copyright © 2011 Elsevier B.V. All rights reserved.

Compositional dependence of magnetic anisotropy in chemically synthesized Co3- x Fe x O4 (0 ≤ x ≤ 2)

NASA Astrophysics Data System (ADS)

Hayashi, Kensuke; Yamada, Keisuke; Shima, Mutsuhiro

2018-01-01

Magnetic anisotropy of Co3- x Fe x O4 (CFO, 0 ≤ x ≤ 2) thin-film and powder samples prepared by a sol-gel method has been investigated as a function of Fe composition x. Structural analyses by X-ray diffraction show that CFO powder samples exhibit diffraction peaks associated with the spinel structure when x < 2, while CFO thin-film samples with thickness of 130-510 nm yield the peaks when 0 ≤ x ≤ 2. CFO thin-film samples are highly (111)-oriented with the Lotgering factor greater than 0.9 when 0.6 ≤ x ≤ 1.3. The magnetic anisotropy constant K 1 of CFO powder samples estimated from their room-temperature hysteresis loops yields a minimum when x = 0.9. Relatively large in-plane magnetic anisotropy (K eff = 5.7 × 105 erg/cm3) is observed for the CFO thin-film sample when x = 1.3. With increasing x, the magnetic easy axis of the spinel CFO changes from 〈111〉 to 〈100〉 when x = 0.9.

Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deng, Junjing; Vine, David J.; Chen, Si

Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolutionmore » beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub-30-nm resolution structural images and ~90-nm-resolution fluorescence images of several elements in frozen-hydrated green algae. Finally, this combined approach offers a way to study the role of trace elements in their structural context.« less

Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

DOE PAGES

Deng, Junjing; Vine, David J.; Chen, Si; ...

2015-02-24

Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolutionmore » beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub-30-nm resolution structural images and ~90-nm-resolution fluorescence images of several elements in frozen-hydrated green algae. Finally, this combined approach offers a way to study the role of trace elements in their structural context.« less

Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deng, Junjing; Vine, David J.; Chen, Si

Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolutionmore » beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub-30-nm resolution structural images and similar to 90-nm-resolution fluorescence images of several elements in frozen-hydrated green algae. This combined approach offers a way to study the role of trace elements in their structural context.« less

Insights into Photosystem II from Isomorphous Difference Fourier Maps of Femtosecond X-ray Diffraction Data and Quantum Mechanics/Molecular Mechanics Structural Models.

PubMed

Wang, Jimin; Askerka, Mikhail; Brudvig, Gary W; Batista, Victor S

2017-02-10

Understanding structure-function relations in photosystem II (PSII) is important for the development of biomimetic photocatalytic systems. X-ray crystallography, computational modeling, and spectroscopy have played central roles in elucidating the structure and function of PSII. Recent breakthroughs in femtosecond X-ray crystallography offer the possibility of collecting diffraction data from the X-ray free electron laser (XFEL) before radiation damage of the sample, thereby overcoming the main challenge of conventional X-ray diffraction methods. However, the interpretation of XFEL data from PSII intermediates is challenging because of the issues regarding data-processing, uncertainty on the precise positions of light oxygen atoms next to heavy metal centers, and different kinetics of the S-state transition in microcrystals compared to solution. Here, we summarize recent advances and outstanding challenges in PSII structure-function determination with emphasis on the implementation of quantum mechanics/molecular mechanics techniques combined with isomorphous difference Fourier maps, direct methods, and high-resolution spectroscopy.

Electrical interface characteristics (I-V), optical time of flight measurements, and the x-ray (20 keV) signal response of amorphous-selenium/crystalline-silicon heterojunction structures

NASA Astrophysics Data System (ADS)

Hunter, David M.; Ho, Chu An; Belev, George; De Crescenzo, Giovanni; Kasap, Safa O.; Yaffe, Martin J.

2011-03-01

We have investigated the dark current, optical TOF (time of flight) properties, and the X-ray response of amorphousselenium (a-Se)/crystalline-silicon (c-Si) heterostructures for application in digital radiography. The structures have been studied to determine if an x-ray generated electron signal, created in an a-Se layer, could be directly transferred to a c-Si based readout device such as a back-thinned CCD (charge coupled device). A simple first order band-theory of the structure indicates that x-ray generated electrons should transfer from the a-Se to the c-Si, while hole transfer from p-doped c-Si to the a-Se should be blocked, permitting a low dark signal as required. The structures we have tested have a thin metal bias electrode on the x-ray facing side of the a-Se which is deposited on the c-Si substrate. The heterostructures made with pure a-Se deposited on epitaxial p-doped (5×10 14 cm-3) c-Si exhibited very low dark current of 15 pA cm-2 at a negative bias field of 10 V μm-1 applied to the a-Se. The optical TOF (time of flight) measurements show that the applied bias drops almost entirely across the a-Se layer and that the a-Se hole and electron mobilities are within the range of commonly accepted values. The x-ray signal measurements demonstrate the structure has the expected x-ray quantum efficiency. We have made a back-thinned CCD coated with a-Se and although most areas of the device show a poor x-ray response, it does contain small regions which do work properly with the expected x-ray sensitivity. Improved understanding of the a-Se/c-Si interface and preparation methods should lead to properly functioning devices.

Three-dimensional imaging of nanoscale materials by using coherent x-rays

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miao, Jianwei

X-ray crystallography is currently the primary methodology used to determine the 3D structure of materials and macromolecules. However, many nanostructures, disordered materials, biomaterials, hybrid materials and biological specimens are noncrystalline and, hence, their structures are not accessible by X-ray crystallography. Probing these structures therefore requires the employment of different approaches. A very promising technique currently under rapid development is X-ray diffraction microscopy (or lensless imaging), in which the coherent X-ray diffraction pattern of a noncrystalline specimen is measured and then directly phased to obtain a high-resolution image. Through the DOE support over the past three years, we have applied X-raymore » diffraction microscopy to quantitative imaging of GaN quantum dot particles, and revealed the internal GaN-Ga2O3 core shell structure in three dimensions. By exploiting the abrupt change in the scattering cross-section near electronic resonances, we carried out the first experimental demonstration of resonant X-ray diffraction microscopy for element specific imaging. We performed nondestructive and quantitative imaging of buried Bi structures inside a Si crystal by directly phasing coherent X-ray diffraction patterns acquired below and above the Bi M5 edge. We have also applied X-ray diffraction microscopy to nondestructive imaging of mineral crystals inside biological composite materials - intramuscular fish bone - at the nanometer scale resolution. We identified mineral crystals in collagen fibrils at different stages of mineralization and proposed a dynamic mechanism to account for the nucleation and growth of mineral crystals in the collagen matrix. In addition, we have also discovered a novel 3D imaging modality, denoted ankylography, which allows for complete 3D structure determination without the necessity of sample titling or scanning. We showed that when the diffraction pattern of a finite object is sampled at a sufficiently fine scale on the Ewald sphere, the 3D structure of the object is determined by the 2D spherical pattern. We confirmed the theoretical analysis by performing 3D numerical reconstructions of a sodium silicate glass structure at 2 A resolution from a 2D spherical diffraction pattern alone. As X-ray free electron lasers are under rapid development worldwide, ankylography may open up a new horizon to obtain the 3D structure of a non-crystalline specimen from a single pulse and allow time-resolved 3D structure determination of disordered materials.« less

Intact Imaging of Human Heart Structure Using X-ray Phase-Contrast Tomography.

PubMed

Kaneko, Yukihiro; Shinohara, Gen; Hoshino, Masato; Morishita, Hiroyuki; Morita, Kiyozo; Oshima, Yoshihiro; Takahashi, Masashi; Yagi, Naoto; Okita, Yutaka; Tsukube, Takuro

2017-02-01

Structural examination of human heart specimens at the microscopic level is a prerequisite for understanding congenital heart diseases. It is desirable not to destroy or alter the properties of such specimens because of their scarcity. However, many of the currently available imaging techniques either destroy the specimen through sectioning or alter the chemical and mechanical properties of the specimen through staining and contrast agent injection. As a result, subsequent studies may not be possible. X-ray phase-contrast tomography is an imaging modality for biological soft tissues that does not destroy or alter the properties of the specimen. The feasibility of X-ray phase-contrast tomography for the structural examination of heart specimens was tested using infantile and fetal heart specimens without congenital diseases. X-ray phase-contrast tomography was carried out at the SPring-8 synchrotron radiation facility using the Talbot grating interferometer at the bending magnet beamline BL20B2 to visualize the structure of five non-pretreated whole heart specimens obtained by autopsy. High-resolution, three-dimensional images were obtained for all specimens. The images clearly showed the myocardial structure, coronary vessels, and conduction bundle. X-ray phase-contrast tomography allows high-resolution, three-dimensional imaging of human heart specimens. Intact imaging using X-ray phase-contrast tomography can contribute to further structural investigation of heart specimens with congenital heart diseases.

From lows to highs: using low-resolution models to phase X-ray data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stuart, David I.; Diamond Light Source Ltd, Diamond House, Harwell Science and Innovation Campus, Didcot; Abrescia, Nicola G. A., E-mail: nabrescia@cicbiogune.es

2013-11-01

An unusual example of how virus structure determination pushes the limits of the molecular replacement method is presented. The study of virus structures has contributed to methodological advances in structural biology that are generally applicable (molecular replacement and noncrystallographic symmetry are just two of the best known examples). Moreover, structural virology has been instrumental in forging the more general concept of exploiting phase information derived from multiple structural techniques. This hybridization of structural methods, primarily electron microscopy (EM) and X-ray crystallography, but also small-angle X-ray scattering (SAXS) and nuclear magnetic resonance (NMR) spectroscopy, is central to integrative structural biology. Here,more » the interplay of X-ray crystallography and EM is illustrated through the example of the structural determination of the marine lipid-containing bacteriophage PM2. Molecular replacement starting from an ∼13 Å cryo-EM reconstruction, followed by cycling density averaging, phase extension and solvent flattening, gave the X-ray structure of the intact virus at 7 Å resolution This in turn served as a bridge to phase, to 2.5 Å resolution, data from twinned crystals of the major coat protein (P2), ultimately yielding a quasi-atomic model of the particle, which provided significant insights into virus evolution and viral membrane biogenesis.« less

Covering complete proteomes with X-ray structures: A current snapshot

DOE PAGES

Mizianty, Marcin J.; Fan, Xiao; Yan, Jing; ...

2014-10-23

Structural genomics programs have developed and applied structure-determination pipelines to a wide range of protein targets, facilitating the visualization of macromolecular interactions and the understanding of their molecular and biochemical functions. The fundamental question of whether three-dimensional structures of all proteins and all functional annotations can be determined using X-ray crystallography is investigated. A first-of-its-kind large-scale analysis of crystallization propensity for all proteins encoded in 1953 fully sequenced genomes was performed. It is shown that current X-ray crystallographic knowhow combined with homology modeling can provide structures for 25% of modeling families (protein clusters for which structural models can be obtainedmore » through homology modeling), with at least one structural model produced for each Gene Ontology functional annotation. The coverage varies between superkingdoms, with 19% for eukaryotes, 35% for bacteria and 49% for archaea, and with those of viruses following the coverage values of their hosts. It is shown that the crystallization propensities of proteomes from the taxonomic superkingdoms are distinct. The use of knowledge-based target selection is shown to substantially increase the ability to produce X-ray structures. It is demonstrated that the human proteome has one of the highest attainable coverage values among eukaryotes, and GPCR membrane proteins suitable for X-ray structure determination were determined.« less

Microgravity

NASA Image and Video Library

2001-06-06

X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

Small-angle X-ray scattering (SAXS) studies of the structure of mesoporous silicas

NASA Astrophysics Data System (ADS)

Zienkiewicz-Strzałka, M.; Skibińska, M.; Pikus, S.

2017-11-01

Mesoporous ordered silica nanostructures show strong interaction with X-ray radiation in the range of small-angles. Small-angle X-ray scattering (SAXS) measurements based on the elastically scattered X-rays are important in analysis of condensed matter. In the case of mesoporous silica materials SAXS technique provides information on the distribution of electron density in the mesoporous material, in particular describing their structure and size of the unit cell as well as type of ordered structure and finally their parameters. The characterization of nanopowder materials, nanocomposites and porous materials by Small-Angle X-ray Scattering seems to be valuable and useful. In presented work, the SAXS investigation of structures from the group of mesoporous ordered silicates was performed. This work has an objective to prepare functional materials modified by noble metal ions and nanoparticles and using the small-angle X-ray scattering to illustrate their properties. We report the new procedure for describing mesoporous materials belonging to SBA-15 and MCM-41 family modified by platinum, palladium and silver nanoparticles, based on detailed analysis of characteristic peaks in the small-angle range of X-ray scattering. This procedure allows to obtained the most useful parameters for mesoporous materials characterization and their successfully compare with experimental measurements reducing the time and material consumption with good precision for particles and pores with a size below 10 nm.

The STAR-X X-Ray Telescope Assembly (XTA)

NASA Technical Reports Server (NTRS)

McClelland, Ryan S.; Bautz, Mark W.; Bonafede, Joseph A.; Miller, Eric D.; Saha, Timo T.; Solly, Peter M.; Zhang, William W.

2017-01-01

The Survey and Time-domain Astrophysical Research eXplorer (STAR-X) science goals are to discover what powers the most violent explosions in the Universe, understand how black holes grow across cosmic time and mass scale, and measure how structure formation heats the majority of baryons in the Universe. To achieve these goals, STAR-X requires a powerful X-ray telescope with a large field of view, large collecting area, and excellent point spread function. The STAR-X instrument, the X-Ray Telescope Assembly (XTA), meets these requirements using a powerful X-ray mirror technology based on precision-polished single crystal silicon and a mature CCD detector technology. The XTA is composed of three major subsystems: an X-ray Mirror Assembly (MA) of high resolution, lightweight mirror segments fabricated out of single crystal silicon; a Focal Plane Assembly (FPA) made of back-illuminated CCD's capable of detecting X-rays with excellent quantum efficiency; and a composite Telescope Tube that structurally links the MA and FPA. The MA consists of 5,972 silicon mirror segments mounted into five subassemblies called meta-shells. A meta-shell is constructed from an annular central structural shell covered with interlocking layers of mirror segments. This paper describes the requirements, design, and analysis of the XTA subsystems with particular focus on the MA.

The STAR-X X-Ray Telescope Assembly (XTA)

NASA Astrophysics Data System (ADS)

McClelland, Ryan S.

2017-08-01

The Survey and Time-domain Astrophysical Research eXplorer (STAR-X) science goals are to discover what powers the most violent explosions in the Universe, understand how black holes grow across cosmic time and mass scale, and measure how structure formation heats the majority of baryons in the Universe. To achieve these goals, STAR-X requires a powerful X-ray telescope with a large field of view, large collecting area, and excellent point spread function. The STAR-X instrument, the X-Ray Telescope Assembly (XTA), meets these requirements using a powerful X-ray mirror technology based on precision-polished single crystal silicon and a mature CCD detector technology. The XTA is composed of three major subsystems: an X-ray Mirror Assembly (MA) of high resolution, lightweight mirror segments fabricated out of single crystal silicon; a Focal Plane Assembly (FPA) made of back-illuminated CCDs capable of detecting X-rays with excellent quantum efficiency; and a composite Telescope Tube that structurally links the MA and FPA. The MA consists of 5,972 silicon mirror segments mounted into five subassemblies called metashells. A meta-shell is constructed from an annular central structural shell covered with interlocking layers of mirror segments. This paper describes the requirements, design, and analysis of the XTA subsystems with particular focus on the MA.

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Effects of X-ray irradiation on the Eu3+ → Eu2+ conversion in CaAl2O4 phosphors

NASA Astrophysics Data System (ADS)

Gomes, Manassés A.; Carvalho, Jéssica C.; Andrade, Adriano B.; Rezende, Marcos V.; Macedo, Zélia S.; Valerio, Mário E. G.

2018-01-01

This paper reports structural and luminescence properties of Eu-doped CaAl2O4 produced by an alternative sol-gel method using coconut water. Results of differential thermal analysis (DTA), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) allowed us to identify the best synthesis conditions for sample preparation. Simultaneous measurements of X-ray absorption spectroscopy (XAS) and X-ray excited optical luminescence (XEOL) were also performed in the X-ray energy range of the Eu LIII edge. Results from photoluminescence (PL) showed only the characteristic Eu3+ emission. However, radioluminescence emission spectra from Eu-doped CaAl2O4 shows a process of conversion of Eu3+ to Eu2+, which is induced by X-ray irradiation and is dependent on the radiation dose energy. X-ray absorption near edge structure (XANES) measurements corroborate Eu reduction due to irradiation, showing that only the Eu3+ ion is present in stable form in the CaAl2O4.

Volcanic Chemostratigraphy on the Outcrop Using Field-Portable X-Ray Fluorescence: An Example from the Basaltic Flows of Hewitt's Cove, MA.

NASA Astrophysics Data System (ADS)

Wall, A. M.; Brabander, D. J.

2005-05-01

The area of Hewitt's Cove, Hingham, Massachusetts structurally represents the southern extent of the Boston Basin, and as such, provides the opportunity to identify and recognize basin-wide events. While the stratigraphy of the Boston Basin has been developed since the advent of U-Pb geochronology and formal stratigraphic facies descriptions (Socci and Smith, 2001), the stratigraphy of the Hewitt's Cove area has not been thoroughly addressed since the work of William O. Crosby in 1894 (Billings, 1976, Bailey and Bland, 2001). Hewitt's Cove consists of an andesitic basaltic flow, approximately 150 m thick, overlain by siltstone and conglomeratic sequences. Field-Portable X-Ray Fluorescence (FP-XRF) was used on fresh and weathered surfaces on the outcrop and in hand samples, and these analyses were compared with conventional laboratory XRF analyses. The in situ field-based analyses produced a reproducible chemostratigraphy that is consistent with subsequent laboratory-based analyses. These data suggest that the series of andesitic basalt flows at Hewitt's Cove are the result of compositionally different magmatic pulses. Additional analyses must be completed to determine the extent of these pulses and the extent of variation in this area before further conclusions can be made. This study particularly demonstrates the utility of using FP-XRF in igneous geologic applications.

Alternative difference analysis scheme combining R -space EXAFS fit with global optimization XANES fit for X-ray transient absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhan, Fei; Tao, Ye; Zhao, Haifeng

Time-resolved X-ray absorption spectroscopy (TR-XAS), based on the laser-pump/X-ray-probe method, is powerful in capturing the change of the geometrical and electronic structure of the absorbing atom upon excitation. TR-XAS data analysis is generally performed on the laser-on minus laser-off difference spectrum. Here, a new analysis scheme is presented for the TR-XAS difference fitting in both the extended X-ray absorption fine-structure (EXAFS) and the X-ray absorption near-edge structure (XANES) regions.R-space EXAFS difference fitting could quickly provide the main quantitative structure change of the first shell. The XANES fitting part introduces a global non-derivative optimization algorithm and optimizes the local structure changemore » in a flexible way where both the core XAS calculation package and the search method in the fitting shell are changeable. The scheme was applied to the TR-XAS difference analysis of Fe(phen) 3spin crossover complex and yielded reliable distance change and excitation population.« less

Depth profiling of marker layers using x-ray waveguide structures

NASA Astrophysics Data System (ADS)

Gupta, Ajay; Rajput, Parasmani; Saraiya, Amit; Reddy, V. R.; Gupta, Mukul; Bernstorff, Sigrid; Amenitsch, H.

2005-08-01

It is demonstrated that x-ray waveguide structures can be used for depth profiling of a marker layer inside the guiding layer with an accuracy of better than 0.2 nm. A combination of x-ray fluorescence and x-ray reflectivity measurements can provide detailed information about the structure of the guiding layer. The position and thickness of the marker layer affect different aspects of the angle-dependent x-ray fluorescence pattern, thus making it possible to determine the structure of the marker layer in an unambiguous manner. As an example, effects of swift heavy ion irradiation on a Si/M/Si trilayer ( M=Fe , W), forming the cavity of the waveguide structure, have been studied. It is found that in accordance with the prediction of thermal spike model, Fe is much more sensitive to swift heavy ion induced modifications as compared to W, even in thin film form. However, a clear evidence of movement of the Fe marker layer towards the surface is observed after irradiation, which cannot be understood in terms of the thermal spike model alone.

Reactor for tracking catalyst nanoparticles in liquid at high temperature under a high-pressure gas phase with X-ray absorption spectroscopy.

PubMed

Nguyen, Luan; Tao, Franklin Feng

2018-02-01

Structure of catalyst nanoparticles dispersed in liquid phase at high temperature under gas phase of reactant(s) at higher pressure (≥5 bars) is important for fundamental understanding of catalytic reactions performed on these catalyst nanoparticles. Most structural characterizations of a catalyst performing catalysis in liquid at high temperature under gas phase at high pressure were performed in an ex situ condition in terms of characterizations before or after catalysis since, from technical point of view, access to the catalyst nanoparticles during catalysis in liquid phase at high temperature under high pressure reactant gas is challenging. Here we designed a reactor which allows us to perform structural characterization using X-ray absorption spectroscopy including X-ray absorption near edge structure spectroscopy and extended X-ray absorption fine structure spectroscopy to study catalyst nanoparticles under harsh catalysis conditions in terms of liquid up to 350 °C under gas phase with a pressure up to 50 bars. This reactor remains nanoparticles of a catalyst homogeneously dispersed in liquid during catalysis and X-ray absorption spectroscopy characterization.

Alternative difference analysis scheme combining R-space EXAFS fit with global optimization XANES fit for X-ray transient absorption spectroscopy.

PubMed

Zhan, Fei; Tao, Ye; Zhao, Haifeng

2017-07-01

Time-resolved X-ray absorption spectroscopy (TR-XAS), based on the laser-pump/X-ray-probe method, is powerful in capturing the change of the geometrical and electronic structure of the absorbing atom upon excitation. TR-XAS data analysis is generally performed on the laser-on minus laser-off difference spectrum. Here, a new analysis scheme is presented for the TR-XAS difference fitting in both the extended X-ray absorption fine-structure (EXAFS) and the X-ray absorption near-edge structure (XANES) regions. R-space EXAFS difference fitting could quickly provide the main quantitative structure change of the first shell. The XANES fitting part introduces a global non-derivative optimization algorithm and optimizes the local structure change in a flexible way where both the core XAS calculation package and the search method in the fitting shell are changeable. The scheme was applied to the TR-XAS difference analysis of Fe(phen) 3 spin crossover complex and yielded reliable distance change and excitation population.

Characterization of Metal Powders Used for Additive Manufacturing.

PubMed

Slotwinski, J A; Garboczi, E J; Stutzman, P E; Ferraris, C F; Watson, S S; Peltz, M A

2014-01-01

Additive manufacturing (AM) techniques can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process.

Driving extreme variability: Measuring the evolving coronæ and evidence for jet launching in AGN

NASA Astrophysics Data System (ADS)

Wilkins, D. R.

2016-05-01

Relativistically blurred reflection from the accretion disc provides a powerful probe of the extreme environments close to supermassive black holes; the inner regions of the accretion flow and the corona that produces the intense X-ray continuum. Techniques by which the geometry and extent of the corona can be measured through the observed X-ray spectrum are reviewed along with the evolution in the structure of the corona that is seen to accompany variations in the X-ray luminosity both on long and short timescales. Detailed analyses of the narrow line Seyfert 1 galaxies Mrk 335 and 1H 0707-495, over observations with XMM-Newton as well as Suzaku and NuSTAR spanning nearly a decade reveal that increases in the X-ray luminosity coincide with an expansion of the corona to cover a larger area of the inner accretion disc. Underlying this long timescale variability lie more complex patterns of behaviour on short timescales. Flares in the X-ray emission during a low flux state of Mrk 335 observed in 2013 and 2014 are found to mark a reconfiguration of the corona while there is evidence that the flares were caused by a vertical collimation and ejection of coronal material, reminiscent of an aborted jet-launching event. Measurements of the corona and reflecting accretion disc are combined to infer the conditions on the inner disc that lead to the flaring event.

Investigation of Energy Release in Microflares Observed by the Second Sounding Rocket Flight of the Focusing Optics X-ray Solar Imager (FOXSI-2)

NASA Astrophysics Data System (ADS)

Vievering, J. T.; Glesener, L.; Panchapakesan, S. A.; Ryan, D.; Krucker, S.; Christe, S.; Buitrago-Casas, J. C.; Inglis, A. R.; Musset, S.

2017-12-01

Observations of the Sun in hard x-rays can provide insight into many solar phenomena which are not currently well-understood, including the mechanisms behind particle acceleration in flares. RHESSI is the only solar-dedicated imager currently operating in the hard x-ray regime. Though RHESSI has greatly added to our knowledge of flare particle acceleration, the indirect imaging method of rotating collimating optics is fundamentally limited in sensitivity and dynamic range. By instead using a direct imaging technique, the structure and evolution of even small flares and active regions can be investigated in greater depth. FOXSI (Focusing Optics X-ray Solar Imager), a hard x-ray instrument flown on two sounding rocket campaigns, seeks to achieve these improved capabilities by using focusing optics for solar observations in the 4-20 keV range. During the second of the FOXSI flights, flown on December 11, 2014, two microflares were observed, estimated as GOES class A0.5 and A2.5 (upper limits). Here we present current imaging and spectral analyses of these microflares, exploring the nature of energy release and comparing to observations from other instruments. Additionally, we feature the first analysis of data from the FOXSI-2 CdTe strip detectors, which provide improved efficiency above 10 keV. Through this analysis, we investigate the capabilities of FOXSI in enhancing our knowledge of smaller-scale solar events.

Emission properties of Ce-doped alkaline earth borate glasses for scintillator applications

NASA Astrophysics Data System (ADS)

Torimoto, Aya; Masai, Hirokazu; Okada, Go; Kawaguchi, Noriaki; Yanagida, Takayuki

2017-11-01

We investigate the photoluminescence (PL) and X-ray-induced luminescence properties of 0.1 mol% Ce-doped MO-B2O3 (M = Ca, Sr, and Ba) glasses. We also determine the Ce3+/(Ce3++Ce4+) ratio by X-ray absorption near-edge structure analyses. The emission intensities of PL, X-ray scintillation, and thermally stimulated luminescence (TSL) depend on the host glass composition. The order of the PL intensity from highest to lowest is as follows: Ca-substituted glass, Ba-substituted glass, and Sr-substituted glass. Our results suggest that the optical absorption edge and quantum yield (QY) are influenced by the local coordination state of Ce3+, which, in turn, is likely to be affected by the optical basicity. The order of the X-ray scintillation intensity from highest to lowest is reverse of that of the PL intensity. This is probably because the interaction probability of X-rays with matter depends on the effective atomic number of the material and the effective atomic number has a stronger influence on the scintillation intensity than does the QY. Though the TSL glow curves reveal that the density and energy depth of the trap sites depend on the substituted alkaline earth oxides, we are unable to correlate the electron spin resonance (ESR) spectra with the TSL results. Therefore, it is considered that the ESR active sites are not responsible for the TSL in these systems.

Hyperspectral Analyses of Wild 2 Grains Using Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Simionovici, A. S.; Lemelle, L.; Ferroir, T.; Gillet, P.; Borg, J.; Grossemy, F.; Djouadi, Z.; Bleuet, P.; Susini, J.

2006-12-01

This work is part of the Preliminary Examination Team (PET) on Bulk Chemistry investigation of Wild 2 cometary grains brought back to Earth by the NASA Stardust mission [1]. X-rays are among the least destructive yet sensitive micro-probes, capable of analysing minute samples embedded in low density collectors, so methods based on Synchrotron Radiation had access to Stardust samples in priority. The main goal of the PET was to produce a preliminary characterization of the abundance and nature of the elements present in the returned samples [2]. In this phase it was paramount to analyze the grains in-situ, in the aerogel foam of the collectors to record the total mass fragments and avoid extraction risks. We have performed measurements on beamlines ID22/ID21 of the ESRF synchrotron in Grenoble, France, devoted to high/low energy microspectroscopy and recorded results on a collection of 6 keystones. Terminal particles as well as fragmentation tracks in the aerogel were mapped out with micron resolution, recording total mass composition for elements of Z>15 by means of X-ray fluorescence [3], as well as structural information by X-ray diffraction. This allowed the direct identification of the mineralogy of some of the grains. Finally, we recorded the evolution of the charge states of S and Fe as a function of the position in the track by means of micro-Xanes measurements. All these analyses were combined to produce a description of the Wild 2 cometary grains [4], as well as a history of their formation and of the thermal interactions during their slowing down in the aerogel collectors. [1] Brownlee, D. E. et al., LPSC XXXVII, abstract nr. 2286, 2006. [2] G. J. Flynn et al., LPSC XXXVII, abstract nr. 1217, 2006. [3] A. Simionovici, P. Chevallier, Chap. 7, Handbook of Practical X-Ray Fluorescence Analysis, 66-83, Springer, 2006. [4] G. J. Flynn et al., Science, (submitted), 2006.

Deformation and Failure of Protein Materials in Physiologically Extreme Conditions and Disease

DTIC Science & Technology

2009-03-01

resonance (NMR) spectroscopy and X- ray crystallography have advanced our ability to identify 3D protein structures57. Site-specific studies using NMR, a... ray crystallography, providing structural and temporal information about mechanisms of deformation and assembly (for example in intermediate...tens of thousands of 3D atomistic protein structures, identifying the structure of numerous proteins from varying species sources60. X- ray

Publications - GMC 58 | Alaska Division of Geological & Geophysical Surveys

Science.gov Websites

DGGS GMC 58 Publication Details Title: X-ray diffraction and scanning electron microscopy mineral , Michael, and Core Laboratories, 1985, X-ray diffraction and scanning electron microscopy mineral analyses

The Race To X-ray Microbeam and Nanobeam Science

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ice, Gene E; Budai, John D; Pang, Judy

2011-01-01

X-ray microbeams are an emerging characterization tool with transformational implications for broad areas of science ranging from materials structure and dynamics, geophysics and environmental science to biophysics and protein crystallography. In this review, we discuss the race toward sub-10 nm- x-ray beams with the ability to penetrate tens to hundreds of microns into most materials and with the ability to determine local (crystal) structure. Examples of science enabled by current micro/nanobeam technologies are presented and we provide a perspective on future directions. Applications highlighted are chosen to illustrate the important features of various submicron beam strategies and to highlight themore » directions of current and future research. While it is clear that x-ray microprobes will impact science broadly, the practical limit for hard x-ray beam size, the limit to trace element sensitivity, and the ultimate limitations associated with near-atomic structure determinations are the subject of ongoing research.« less

Annealing induced atomic rearrangements on (Ga,In) (N,As) probed by hard X-ray photoelectron spectroscopy and X-ray absorption fine structure.

PubMed

Ishikawa, Fumitaro; Higashi, Kotaro; Fuyuno, Satoshi; Morifuji, Masato; Kondow, Masahiko; Trampert, Achim

2018-04-13

We study the effects of annealing on (Ga 0.64 ,In 0.36 ) (N 0.045 ,As 0.955 ) using hard X-ray photoelectron spectroscopy and X-ray absorption fine structure measurements. We observed surface oxidation and termination of the N-As bond defects caused by the annealing process. Specifically, we observed a characteristic chemical shift towards lower binding energies in the photoelectron spectra related to In. This phenomenon appears to be caused by the atomic arrangement, which produces increased In-N bond configurations within the matrix, as indicated by the X-ray absorption fine structure measurements. The reduction in the binding energies of group-III In, which occurs concomitantly with the atomic rearrangements of the matrix, causes the differences in the electronic properties of the system before and after annealing.

Surface studies of solids using integral x-ray-induced photoemission yield

DOE PAGES

Stoupin, Stanislav; Zhernenkov, Mikhail; Shi, Bing

2016-11-22

X-ray induced photoemission yield contains structural information complementary to that provided by X-ray Fresnel reflectivity, which presents an advantage to a wide variety of surface studies if this information is made easily accessible. Photoemission in materials research is commonly acknowledged as a method with a probing depth limited by the escape depth of the photoelectrons. Here we show that the integral hard-X-ray-induced photoemission yield is modulated by the Fresnel reflectivity of a multilayer structure and carries structural information that extends well beyond the photoelectron escape depth. A simple electric self-detection of the integral photoemission yield and Fourier data analysis permitmore » extraction of thicknesses of individual layers. The approach does not require detection of the reflected radiation and can be considered as a framework for non-invasive evaluation of buried layers with hard X-rays under grazing incidence.« less

Surface studies of solids using integral X-ray-induced photoemission yield

PubMed Central

Stoupin, Stanislav; Zhernenkov, Mikhail; Shi, Bing

2016-01-01

X-ray induced photoemission yield contains structural information complementary to that provided by X-ray Fresnel reflectivity, which presents an advantage to a wide variety of surface studies if this information is made easily accessible. Photoemission in materials research is commonly acknowledged as a method with a probing depth limited by the escape depth of the photoelectrons. Here we show that the integral hard-X-ray-induced photoemission yield is modulated by the Fresnel reflectivity of a multilayer structure and carries structural information that extends well beyond the photoelectron escape depth. A simple electric self-detection of the integral photoemission yield and Fourier data analysis permit extraction of thicknesses of individual layers. The approach does not require detection of the reflected radiation and can be considered as a framework for non-invasive evaluation of buried layers with hard X-rays under grazing incidence. PMID:27874041

Correlation between protein sequence similarity and x-ray diffraction quality in the protein data bank.

PubMed

Lu, Hui-Meng; Yin, Da-Chuan; Ye, Ya-Jing; Luo, Hui-Min; Geng, Li-Qiang; Li, Hai-Sheng; Guo, Wei-Hong; Shang, Peng

2009-01-01

As the most widely utilized technique to determine the 3-dimensional structure of protein molecules, X-ray crystallography can provide structure of the highest resolution among the developed techniques. The resolution obtained via X-ray crystallography is known to be influenced by many factors, such as the crystal quality, diffraction techniques, and X-ray sources, etc. In this paper, the authors found that the protein sequence could also be one of the factors. We extracted information of the resolution and the sequence of proteins from the Protein Data Bank (PDB), classified the proteins into different clusters according to the sequence similarity, and statistically analyzed the relationship between the sequence similarity and the best resolution obtained. The results showed that there was a pronounced correlation between the sequence similarity and the obtained resolution. These results indicate that protein structure itself is one variable that may affect resolution when X-ray crystallography is used.

CdO-NPs; synthesis from 1D new nano Cd coordination polymer, characterization and application as anti-cancer drug for reducing the viability of cancer cells

NASA Astrophysics Data System (ADS)

Afzalian Mend, Behnaz; Delavar, Mahmoud; Darroudi, Majid

2017-04-01

The hexagonal CdO nano-particles (CdO-NPs) was prepared using new nano Cd coordination polymer, [Cd(NO3)(bipy)(pzca)]n (1) as a precursor, through direct calcination process at 500 °C. The precursor (1) was synthesized by sonochemical method. The new nano compound (1) was characterized by IR spectroscopy, elemental analyses, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and thermal gravimetric analyses. The structure of nano coordination polymer was determined by comparing the XRD pattern of nano and single-crystal of compound (1). The nano CdO was characterized by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). In addition, the activity and efficiency of nano CdO as an anti-cancer drug was studied on cancer cells with different concentration. The results shows that the viability of cancer cells reduced above 2 μg/mL of CdO-NPs concentration.

Sulfur and iron accumulation in three marine-archaeological shipwrecks in the Baltic Sea: The Ghost, the Crown and the Sword

NASA Astrophysics Data System (ADS)

Fors, Yvonne; Grudd, Håkan; Rindby, Anders; Jalilehvand, Farideh; Sandström, Magnus; Cato, Ingemar; Bornmalm, Lennart

2014-02-01

Sulfur and iron concentrations in wood from three 17th century shipwrecks in the Baltic Sea, the Ghost wreck, the Crown and the Sword, were obtained by X-ray fluorescence (XRF) scanning. In near anaerobic environments symbiotic microorganisms degrade waterlogged wood, reduce sulfate and promote accumulation of low-valent sulfur compounds, as previously found for the famous wrecks of the Vasa and Mary Rose. Sulfur K-edge X-ray absorption near-edge structure (XANES) analyses of Ghost wreck wood show that organic thiols and disulfides dominate, together with elemental sulfur probably generated by sulfur-oxidizing Beggiatoa bacteria. Iron sulfides were not detected, consistent with the relatively low iron concentration in the wood. In a museum climate with high atmospheric humidity oxidation processes, especially of iron sulfides formed in the presence of corroding iron, may induce post-conservation wood degradation. Subject to more general confirmation by further analyses no severe conservation concerns are expected for the Ghost wreck wood.

Laboratory-size three-dimensional water-window x-ray microscope with Wolter type I mirror optics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ohsuka, Shinji; The Graduate School for the Creation of New Photonics Industries, 1955-1 Kurematsu-cho, Nishi-ku, Hamamatsu-City, 431-1202; Ohba, Akira

2016-01-28

We constructed a laboratory-size three-dimensional water-window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques. It consists of an electron-impact x-ray source emitting oxygen Kα x-rays, Wolter type I grazing incidence mirror optics, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit better than 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm-scale three-dimensional fine structures were resolved.

Observation of human tissue with phase-contrast x-ray computed tomography

NASA Astrophysics Data System (ADS)

Momose, Atsushi; Takeda, Tohoru; Itai, Yuji; Tu, Jinhong; Hirano, Keiichi

1999-05-01

Human tissues obtained from cancerous kidneys fixed in formalin were observed with phase-contrast X-ray computed tomography (CT) using 17.7-keV synchrotron X-rays. By measuring the distributions of the X-ray phase shift caused by samples using an X-ray interferometer, sectional images that map the distribution of the refractive index were reconstructed. Because of the high sensitivity of phase- contrast X-ray CT, a cancerous lesion was differentiated from normal tissue and a variety of other structures were revealed without the need for staining.

Phase-contrast x-ray computed tomography for observing biological specimens and organic materials

NASA Astrophysics Data System (ADS)

Momose, Atsushi; Takeda, Tohoru; Itai, Yuji

1995-02-01

A novel three-dimensional x-ray imaging method has been developed by combining a phase-contrast x-ray imaging technique with x-ray computed tomography. This phase-contrast x-ray computed tomography (PCX-CT) provides sectional images of organic specimens that would produce absorption-contrast x-ray CT images with little contrast. Comparing PCX-CT images of rat cerebellum and cancerous rabbit liver specimens with corresponding absorption-contrast CT images shows that PCX-CT is much more sensitive to the internal structure of organic specimens.

Probing Photoinduced Structural Phase Transitions by Fast or Ultra-Fast Time-Resolved X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Cailleau, Hervé Collet, Eric; Buron-Le Cointe, Marylise; Lemée-Cailleau, Marie-Hélène Koshihara, Shin-Ya

A new frontier in the field of structural science is the emergence of the fast and ultra-fast X-ray science. Recent developments in time-resolved X-ray diffraction promise direct access to the dynamics of electronic, atomic and molecular motions in condensed matter triggered by a pulsed laser irradiation, i.e. to record "molecular movies" during the transformation of matter initiated by light pulse. These laser pump and X-ray probe techniques now provide an outstanding opportunity for the direct observation of a photoinduced structural phase transition as it takes place. The use of X-ray short-pulse of about 100ps around third-generation synchrotron sources allows structural investigations of fast photoinduced processes. Other new X-ray sources, such as laser-produced plasma ones, generate ultra-short pulses down to 100 fs. This opens the way to femtosecond X-ray crystallography, but with rather low X-ray intensities and more limited experimental possibilities at present. However this new ultra-fast science rapidly progresses around these sources and new large-scale projects exist. It is the aim of this contribution to overview the state of art and the perspectives of fast and ultra-fast X-ray scattering techniques to study photoinduced phase transitions (here, the word ultra-fast is used for sub-picosecond time resolution). In particular we would like to largely present the contribution of crystallographic methods in comparison with optical methods, such as pump-probe reflectivity measurements, the reader being not necessary familiar with X-ray scattering. Thus we want to present which type of physical information can be obtained from the positions of the Bragg peaks, their intensity and their shape, as well as from the diffuse scattering beyond Bragg peaks. An important physical feature is to take into consideration the difference in nature between a photoinduced phase transition and conventional homogeneous photoinduced chemical or biochemical processes where molecules transform in an independent way each other. Actually the photoinduced phase transition with the establishment of the new electronic and structural oscopic order is preceded by precursor co-operative phenomena due to the formation of nano-scale correlated objects. These are the counterpart of pre-transitional fluctuations at thermal equilibrium which take place above the transition temperature (short range order preceding long range one). Moreover ultra-fast X-ray scattering will play a central role within the fascinating field of manipulating coherence, for instance to directly observe coherent atomic motions induced by a light pulse, such as optical phonons. In the first part of this contribution we present what experimental features are accessible by X-ray scattering to describe the physical picture for a photoinduced structural phase transition. The second part shows how a time-resolved X-ray scattering experiment can be performed with regards to the different pulsed X-ray sources. The first time-resolved X-ray diffraction experiments on photoinduced phase transitions are described and discussed in the third part. Finally some challenges for future are briefly indicated in the conclusion.

Advances in functional X-ray imaging techniques and contrast agents

PubMed Central

Chen, Hongyu; Rogalski, Melissa M.

2012-01-01

X-rays have been used for non-invasive high-resolution imaging of thick biological specimens since their discovery in 1895. They are widely used for structural imaging of bone, metal implants, and cavities in soft tissue. Recently, a number of new contrast methodologies have emerged which are expanding X-ray’s biomedical applications to functional as well as structural imaging. These techniques are promising to dramatically improve our ability to study in situ biochemistry and disease pathology. In this review, we discuss how X-ray absorption, X-ray fluorescence, and X-ray excited optical luminescence can be used for physiological, elemental, and molecular imaging of vasculature, tumours, pharmaceutical distribution, and the surface of implants. Imaging of endogenous elements, exogenous labels, and analytes detected with optical indicators will be discussed. PMID:22962667

Inorganic polymers from laterite using activation with phosphoric acid and alkaline sodium silicate solution: Mechanical and microstructural properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lassinantti Gualtieri, Magdalena, E-mail: magdalena.gualtieri@unimore.it; Romagnoli, Marcello; Pollastri, Simone

2015-01-15

Geopolymers from laterite, an iron-rich soil available in developing countries, have great potential as building materials. In this work, laterite from Togo (Africa) was used to prepare geopolymers using both phosphoric acid and alkaline sodium silicate solution. Microstructural properties were investigated by scanning electron microscopy, X-ray powder diffraction and mercury porosimetry, whereas thermal properties were evaluated by thermal analyses. The local environment of iron was studied by X-ray Absorption Spectroscopy (XANES region). The mechanical properties were determined. Modulus of Rupture and Young's modulus fell in the ranges 3.3–4.5 MPa and 12–33 GPa, respectively, rendering the materials good candidates for constructionmore » purposes. Heating above 900 °C results in weight-gain, presumably due to iron redox reactions. X-ray Absorption Spectroscopy data evidence changes in the chemical and structural environments of iron following thermal treatment of geopolymers. These changes indicate interaction between the geopolymer structure and iron during heating, possibly leading to redox properties. -- Highlights: •Geopolymerization of laterite is promising for fabrication of building materials. •Both phosphoric acid and alkaline sodium silicate solution can be used for activation. •Thermally activated redox properties of the inorganic polymers were observed.« less

Three pharmaceuticals cocrystals of adefovir: Syntheses, structures and dissolution study

NASA Astrophysics Data System (ADS)

Zhang, Xiaoming; Sun, Fuxing; Zhang, Tingting; Jia, Jiangtao; Su, Hongmin; Wang, Chenhui; Zhu, Guangshan

2015-11-01

We report here three novel cocrystals, which are composed of adefovir as the API (Active Pharmaceutical Ingredient) with p-aminobenzoic acid (1, 2C8H12N5O4P·C7H6NO2·3H2O), 3,5-dihydroxybenzoic acid (2, C8H12N5O4P·C7H6O4·H2O) and 2,6-pyridinedicarboxlic acid (3, C8H12N5O4P·C7H5NO4) as CCFs (cocrystal formers) respectively by crystal engineering strategy. Their structures were characterized by single crystal X-ray diffraction, powder X-ray diffraction (PXRD) analysis, thermogravimetric analyses (TGA), elemental analysis (EA) and infrared spectral analysis (IR). The analysis of single crystal X-ray diffraction demonstrate that cocrystal 1 and 2 form a strong hydrogen-bonded assembly through the phosphoric acids of API with water in the lattice and carboxylic acids of CCF respectively. Cocrystal 3 is formed in which the phosphoric acid groups of API are also held by the carboxylic acid groups of CCF. The PXRD results indicate their high purity of as-synthesized samples. The TGA, EA, IR and dissolution study of API and the cocrystals were also measured and discussed.

Characterization of yellow and colorless decorative glasses from the Temple of the Emerald Buddha, Bangkok, Thailand

NASA Astrophysics Data System (ADS)

Klysubun, Wantana; Ravel, Bruce; Klysubun, Prapong; Sombunchoo, Panidtha; Deenan, Weeraya

2013-06-01

Yellow and colorless ancient glasses, which were once used to decorate the Temple of the Emerald Buddha, Bangkok, Thailand, around 150 years ago, are studied to unravel the long-lost glass-making recipes and manufacturing techniques. Analyses of chemical compositions, using synchrotron x-ray fluorescence (SRXRF), indicate that the Thai ancient glasses are soda lime silica glasses (60 % SiO2; 10 % Na2O; 10 % CaO) bearing lead oxide between 2-16 %. Iron (1.5-9.4 % Fe2O3) and manganese (1.7 % MnO) are present in larger abundance than the other 3 d transition metals detected (0.04-0.2 %). K-edge x-ray absorption near edge spectroscopy (XANES) and extended x-ray absorption fine structure spectroscopy (EXAFS) provide conclusive evidence on the oxidation states of Fe being 3+ and Mn being 2+ and on short-length tetrahedral structures around the cations. This suggests that iron is used as a yellow colorant with manganese as a decolorant. L 3-edge XANES results reveal the oxidation states of lead as 2+. The results from this work provide information crucial for replicating these decorative glasses for the future restoration of the Temple of the Emerald Buddha.

Dark-field phase retrieval under the constraint of the Friedel symmetry in coherent X-ray diffraction imaging.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2014-11-17

Coherent X-ray diffraction imaging (CXDI) is a lensless imaging technique that is suitable for visualizing the structures of non-crystalline particles with micrometer to sub-micrometer dimensions from material science and biology. One of the difficulties inherent to CXDI structural analyses is the reconstruction of electron density maps of specimen particles from diffraction patterns because saturated detector pixels and a beam stopper result in missing data in small-angle regions. To overcome this difficulty, the dark-field phase-retrieval (DFPR) method has been proposed. The DFPR method reconstructs electron density maps from diffraction data, which are modified by multiplying Gaussian masks with an observed diffraction pattern in the high-angle regions. In this paper, we incorporated Friedel centrosymmetry for diffraction patterns into the DFPR method to provide a constraint for the phase-retrieval calculation. A set of model simulations demonstrated that this constraint dramatically improved the probability of reconstructing correct electron density maps from diffraction patterns that were missing data in the small-angle region. In addition, the DFPR method with the constraint was applied successfully to experimentally obtained diffraction patterns with significant quantities of missing data. We also discuss this method's limitations with respect to the level of Poisson noise in X-ray detection.

X-ray Crystallography Facility

NASA Technical Reports Server (NTRS)

2000-01-01

Edward Snell, a National Research Council research fellow at NASA's Marshall Space Flight Center (MSFC), prepares a protein crystal for analysis by x-ray crystallography as part of NASA's structural biology program. The small, individual crystals are bombarded with x-rays to produce diffraction patterns, a map of the intensity of the x-rays as they reflect through the crystal.

Ultra-short wavelength x-ray system

DOEpatents

Umstadter, Donald [Ann Arbor, MI; He, Fei [Ann Arbor, MI; Lau, Yue-Ying [Potomac, MD

2008-01-22

A method and apparatus to generate a beam of coherent light including x-rays or XUV by colliding a high-intensity laser pulse with an electron beam that is accelerated by a synchronized laser pulse. Applications include x-ray and EUV lithography, protein structural analysis, plasma diagnostics, x-ray diffraction, crack analysis, non-destructive testing, surface science and ultrafast science.

A laboratory system for element specific hyperspectral X-ray imaging.

PubMed

Jacques, Simon D M; Egan, Christopher K; Wilson, Matthew D; Veale, Matthew C; Seller, Paul; Cernik, Robert J

2013-02-21

X-ray tomography is a ubiquitous tool used, for example, in medical diagnosis, explosives detection or to check structural integrity of complex engineered components. Conventional tomographic images are formed by measuring many transmitted X-rays and later mathematically reconstructing the object, however the structural and chemical information carried by scattered X-rays of different wavelengths is not utilised in any way. We show how a very simple; laboratory-based; high energy X-ray system can capture these scattered X-rays to deliver 3D images with structural or chemical information in each voxel. This type of imaging can be used to separate and identify chemical species in bulk objects with no special sample preparation. We demonstrate the capability of hyperspectral imaging by examining an electronic device where we can clearly distinguish the atomic composition of the circuit board components in both fluorescence and transmission geometries. We are not only able to obtain attenuation contrast but also to image chemical variations in the object, potentially opening up a very wide range of applications from security to medical diagnostics.

Ni doped Fe3O4 magnetic nanoparticles.

PubMed

Larumbe, S; Gómez-Polo, C; Pérez-Landazábal, J I; García-Prieto, A; Alonso, J; Fdez-Gubieda, M L; Cordero, D; Gómez, J

2012-03-01

In this work, the effect of nickel doping on the structural and magnetic properties of Fe3O4 nanoparticles is analysed. Ni(x)Fe(3-x)O4 nanoparticles (x = 0, 0.04, 0.06 and 0.11) were obtained by chemical co-precipitation method, starting from a mixture of FeCl2 x 4H2O and Ni(AcO)2 x 4H2O salts. The analysis of the structure and composition of the synthesized nanoparticles confirms their nanometer size (main sizes around 10 nm) and the inclusion of the Ni atoms in the characteristic spinel structure of the magnetite Fe3O4 phase. In order to characterize in detail the structure of the samples, X-ray absorption (XANES) measurements were performed on the Ni and Fe K-edges. The results indicate the oxidation of the Ni atoms to the 2+ state and the location of the Ni2+ cations in the Fe2+ octahedral sites. With respect to the magnetic properties, the samples display the characteristic superparamagnetic behaviour, with anhysteretic magnetic response at room temperature. The estimated magnetic moment confirms the partial substitution of the Fe2+ cations by Ni2+ atoms in the octahedral sites of the spinel structure.

Beyond crystallography: diffractive imaging using coherent x-ray light sources.

PubMed

Miao, Jianwei; Ishikawa, Tetsuya; Robinson, Ian K; Murnane, Margaret M

2015-05-01

X-ray crystallography has been central to the development of many fields of science over the past century. It has now matured to a point that as long as good-quality crystals are available, their atomic structure can be routinely determined in three dimensions. However, many samples in physics, chemistry, materials science, nanoscience, geology, and biology are noncrystalline, and thus their three-dimensional structures are not accessible by traditional x-ray crystallography. Overcoming this hurdle has required the development of new coherent imaging methods to harness new coherent x-ray light sources. Here we review the revolutionary advances that are transforming x-ray sources and imaging in the 21st century. Copyright © 2015, American Association for the Advancement of Science.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Improving packaged food quality and safety. Part 1: synchrotron X-ray analysis.

PubMed

López-Rubio, A; Hernandez-Muñoz, P; Catala, R; Gavara, R; Lagarón, J M

2005-10-01

The objective was to demonstrate, as an example of an application, the potential of synchrotron X-ray analysis to detect morphological alterations that can occur in barrier packaging materials and structures. These changes can affect the packaging barrier characteristics when conventional food preservation treatments are applied to packaged food. The paper presents the results of a number of experiments where time-resolved combined wide-angle X-ray scattering and small-angle X-ray scattering analysis as a function of temperature and humidity were applied to ethylene-vinyl alcohol co-polymers (EVOH), polypropylene (PP)/EVOH/PP structures, aliphatic polyketone terpolymer (PK) and amorphous polyamide (aPA) materials. A comparison between conventional retorting and high-pressure processing treatments in terms of morphologic alterations are also presented for EVOH. The impact of retorting on the EVOH structure contrasts with the good behaviour of the PK during this treatment and with that of aPA. However, no significant structural changes were observed by wide-angle X-ray scattering in the EVOH structures after high-pressure processing treatment. These structural observations have also been correlated with oxygen permeability measurements that are of importance when guaranteeing the intended levels of safety and quality of packaged food.

A non-destructive method for quality control of the pellet distribution within a MUPS tablet by terahertz pulsed imaging.

PubMed

Novikova, Anna; Markl, Daniel; Zeitler, J Axel; Rades, Thomas; Leopold, Claudia S

2018-01-01

Terahertz pulsed imaging (TPI) was applied to analyse the inner structure of multiple unit pellet system (MUPS) tablets. MUPS tablets containing different amounts of theophylline pellets coated with Eudragit® NE 30 D and with microcrystalline cellulose (MCC) as cushioning agent were analysed. The tablets were imaged by TPI and the results were compared to X-ray microtomography. The terahertz pulse beam propagates through the tablets and is back-reflected at the interface between the MCC matrix and the coated pellets within the tablet causing a peak in the terahertz waveform. Cross-section images of the tablets were extracted at different depths and parallel to the tablet faces from 3D terahertz data to visualise the surface-near structure of the MUPS tablets. The images of the surface-near structure of the MUPS tablets were compared to X-ray microtomography images at the same depths. The surface-near structure could be clearly resolved by TPI at depths between 24 and 152μm below the tablet surface. An increasing amount of pellets within the MUPS tablets appears to slightly decrease the detectability of the pellets within the tablets by TPI. TPI was shown to be a non-destructive method for the detection of pellets within the tablets and could resolve structures thicker than 30μm. In conclusion, a proof-of-concept was provided for TPI as a method of quality control for MUPS tablets. Copyright © 2017 Elsevier B.V. All rights reserved.

Coronal X-ray enhancements associated with H-alpha filament disappearances

NASA Technical Reports Server (NTRS)

Webb, D. F.; Krieger, A. S.; Rust, D. M.

1976-01-01

The X-ray telescope experiment aboard the Skylab/ATM mission provided high-resolution soft X-ray images of the lower corona away from active regions, revealing frequent large-scale transient X-ray enhancements which could often be associated with the disappearance of H-alpha filaments. The X-ray emitting structures featured peak brightnesses similar to those of nonflaring active region structures, durations from 3 to 40 hours, shapes that in general outlined the preexisting H-alpha filaments to as large as 400,000 km, apparent expansion velocities of the order of tens of km/sec, and observed peak temperatures of the order of a few million degrees. One such event is described and analyzed in detail. Two explanations of the events are discussed: (1) excess cool material is present in the filament cavity, contributing to the X-ray enhancement, and (2) the enhancement is due to the compression of preexisting material by a changing magnetic field.

Identification of differentially expressed genes associated with the enhancement of X-ray susceptibility by RITA in a hypopharyngeal squamous cell carcinoma cell line (FaDu).

PubMed

Luan, Jinwei; Li, Xianglan; Guo, Rutao; Liu, Shanshan; Luo, Hongyu; You, Qingshan

2016-06-01

Next generation sequencing and bio-informatic analyses were conducted to investigate the mechanism of reactivation of p53 and induction of tumor cell apoptosis (RITA)-enhancing X-ray susceptibility in FaDu cells. The cDNA was isolated from FaDu cells treated with 0 X-ray, 8 Gy X-ray, or 8 Gy X-ray + RITA. Then, cDNA libraries were created and sequenced using next generation sequencing, and each assay was repeated twice. Subsequently, differentially expressed genes (DEGs) were identified using Cuffdiff in Cufflinks and their functions were predicted by pathway enrichment analyses. Genes that were constantly up- or down-regulated in 8 Gy X-ray-treated FaDu cells and 8 Gy X-ray + RITA-treated FaDu cells were obtained as RITA genes. Afterward, the protein-protein interaction (PPI) relationships were obtained from the STRING database and a PPI network was constructed using Cytoscape. Furthermore, ClueGO was used for pathway enrichment analysis of genes in the PPI network. Total 2,040 and 297 DEGs were identified in FaDu cells treated with 8 Gy X-ray or 8 Gy X-ray + RITA, respectively. PARP3 and NEIL1 were enriched in base excision repair, and CDK1 was enriched in p53 signaling pathway. RFC2 and EZH2 were identified as RITA genes. In the PPI network, many interaction relationships were identified (e.g., RFC2-CDK1, EZH2-CDK1 and PARP3-EZH2). ClueGO analysis showed that RFC2 and EZH2 were related to cell cycle. RFC2, EZH2, CDK1, PARP3 and NEIL1 may be associated, and together enhance the susceptibility of FaDu cells treated with RITA to the deleterious effects of X-ray.

Structural studies of liquid Co–Sn alloys

PubMed Central

Yakymovych, A.; Shtablavyi, I.; Mudry, S.

2014-01-01

An analysis of the structure features of liquid Co–Sn alloys has been performed by means of X-ray diffraction method, viscosity coefficient analysis and computer simulation method. The X-ray diffraction investigations were carried out over a wide concentration range at the temperature 1473 K. It was found that the structure of these alloys can be described in the frame of independent X-ray scattering model. The viscosity coefficient was calculated by an excess entropy scaling and compared with experimental data. PMID:25328282

Cooling for a rotating anode X-ray tube

DOEpatents

Smither, Robert K.

1998-01-01

A method and apparatus for cooling a rotating anode X-ray tube. An electromagnetic motor is provided to rotate an X-ray anode with cooling passages in the anode. These cooling passages are coupled to a cooling structure located adjacent the electromagnetic motor. A liquid metal fills the passages of the cooling structure and electrical power is provided to the motor to rotate the anode and generate a rotating magnetic field which moves the liquid metal through the cooling passages and cooling structure.

Iron-doped nickel oxide nanocrystals as highly efficient electrocatalysts for alkaline water splitting.

PubMed

Fominykh, Ksenia; Chernev, Petko; Zaharieva, Ivelina; Sicklinger, Johannes; Stefanic, Goran; Döblinger, Markus; Müller, Alexander; Pokharel, Aneil; Böcklein, Sebastian; Scheu, Christina; Bein, Thomas; Fattakhova-Rohlfing, Dina

2015-05-26

Efficient electrochemical water splitting to hydrogen and oxygen is considered a promising technology to overcome our dependency on fossil fuels. Searching for novel catalytic materials for electrochemical oxygen generation is essential for improving the total efficiency of water splitting processes. We report the synthesis, structural characterization, and electrochemical performance in the oxygen evolution reaction of Fe-doped NiO nanocrystals. The facile solvothermal synthesis in tert-butanol leads to the formation of ultrasmall crystalline and highly dispersible FexNi1-xO nanoparticles with dopant concentrations of up to 20%. The increase in Fe content is accompanied by a decrease in particle size, resulting in nonagglomerated nanocrystals of 1.5-3.8 nm in size. The Fe content and composition of the nanoparticles are determined by X-ray photoelectron spectroscopy and energy-dispersive X-ray spectroscopy measurements, while Mössbauer and extended X-ray absorption fine structure analyses reveal a substitutional incorporation of Fe(III) into the NiO rock salt structure. The excellent dispersibility of the nanoparticles in ethanol allows for the preparation of homogeneous ca. 8 nm thin films with a smooth surface on various substrates. The turnover frequencies (TOF) of these films could be precisely calculated using a quartz crystal microbalance. Fe0.1Ni0.9O was found to have the highest electrocatalytic water oxidation activity in basic media with a TOF of 1.9 s(-1) at the overpotential of 300 mV. The current density of 10 mA cm(-2) is reached at an overpotential of 297 mV with a Tafel slope of 37 mV dec(-1). The extremely high catalytic activity, facile preparation, and low cost of the single crystalline FexNi1-xO nanoparticles make them very promising catalysts for the oxygen evolution reaction.

A Precessing Jet in the CH Cyg Symbiotic System

NASA Astrophysics Data System (ADS)

Karovska, Margarita; Gaetz, Terrance J.; Carilli, Christopher L.; Hack, Warren; Raymond, John C.; Lee, Nicholas P.

2010-02-01

Jets have been detected in only a few symbiotic binaries to date, and CH Cyg is one of them. In 2001, a non-relativistic jet was detected in CH Cyg for the first time in X-rays. We carried out coordinated Chandra, Hubble Space Telescope (HST), and VLA observations in 2008 to study the propagation of this jet and its interaction with the circumbinary medium. We detected the jet with Chandra and HST and determined that the apex has expanded to the south from ~300 AU to ~1400 AU, with the shock front propagating with velocity <100 km s-1. The shock front has significantly slowed down since 2001. Unexpectedly, we also discovered a powerful jet in the NE-SW direction, in the X-ray, optical and radio. This jet has a multi-component structure, including an inner jet and a counterjet at ~170 AU, and a SW component ending in several clumps extending out to ~750 AU. The structure of the jet and the curvature of the outer portion of the SW jet suggest an episodically powered precessing jet or a continuous precessing jet with occasional mass ejections or pulses. We carried out detailed spatial mapping of the X-ray emission and correlation with the optical and radio emission. X-ray spectra were extracted from the central source, inner NE counterjet, and the brightest clump at a distance of ~500 AU from the central source. We discuss the initial results of our analyses, including the multi-component spectral fitting of the jet components and of the central source.

Chemical imaging analysis of the brain with X-ray methods

NASA Astrophysics Data System (ADS)

Collingwood, Joanna F.; Adams, Freddy

2017-04-01

Cells employ various metal and metalloid ions to augment the structure and the function of proteins and to assist with vital biological processes. In the brain they mediate biochemical processes, and disrupted metabolism of metals may be a contributing factor in neurodegenerative disorders. In this tutorial review we will discuss the particular role of X-ray methods for elemental imaging analysis of accumulated metal species and metal-containing compounds in biological materials, in the context of post-mortem brain tissue. X-rays have the advantage that they have a short wavelength and can penetrate through a thick biological sample. Many of the X-ray microscopy techniques that provide the greatest sensitivity and specificity for trace metal concentrations in biological materials are emerging at synchrotron X-ray facilities. Here, the extremely high flux available across a wide range of soft and hard X-rays, combined with state-of-the-art focusing techniques and ultra-sensitive detectors, makes it viable to undertake direct imaging of a number of elements in brain tissue. The different methods for synchrotron imaging of metals in brain tissues at regional, cellular, and sub-cellular spatial resolution are discussed. Methods covered include X-ray fluorescence for elemental imaging, X-ray absorption spectrometry for speciation imaging, X-ray diffraction for structural imaging, phase contrast for enhanced contrast imaging and scanning transmission X-ray microscopy for spectromicroscopy. Two- and three-dimensional (confocal and tomographic) imaging methods are considered as well as the correlation of X-ray microscopy with other imaging tools.

Thermal analyses, spectral characterization and structural interpretation of Nd3+/Er3+ ions co-doped TeO2-ZnCl2 glasses system

NASA Astrophysics Data System (ADS)

Ahmed, Kasim F.; Ibrahim, Saeed O.; Sahar, Md. R.; Mawlud, Saman Q.; Khizir, Hersh A.

2017-09-01

The Nd3+/Er3+ ions co-doped in the system of zinc-tellurite with the composition of (70-2x)TeO2-30ZnCl2-xNd2O3-xEr2O3 concentration from 1.0 to 3.0 mol% (x=1, 2 and 3) glasses were prepared by using conventional melt-quenching technique. The amorphous nature of the glass been confirmed by using X-RAY Diffraction Spectroscopy. Thermal characteristic were determined using a DTA. The obtained results discussed in terms of the glass structure. The glass structure studied by means of FTIR. Seven significant vibrational peaks around 471, 687, 742, 768, 1632, 2833 and 3378 cm-1 which correspond to the structural bonding of the glass are observed in a range of 400-4000cm-1. The peaks observed are consistent with the stretching and bending vibrations of the Te-O, TeO4 trigonal bipyramids, TeO3 trigonal pyramids, Te-O-Te and OH linkages respectively.

Refractive Optics for Hard X-ray Transmission Microscopy

NASA Astrophysics Data System (ADS)

Simon, M.; Ahrens, G.; Last, A.; Mohr, J.; Nazmov, V.; Reznikova, E.; Voigt, A.

2011-09-01

For hard x-ray transmission microscopy at photon energies higher than 15 keV we design refractive condenser and imaging elements to be used with synchrotron light sources as well as with x-ray tube sources. The condenser lenses are optimized for low x-ray attenuation—resulting in apertures greater than 1 mm—and homogeneous intensity distribution on the detector plane, whereas the imaging enables high-resolution (<100 nm) full-field imaging. To obtain high image quality at reasonable exposure times, custom-tailored matched pairs of condenser and imaging lenses are being developed. The imaging lenses (compound refractive lenses, CRLs) are made of SU-8 negative resist by deep x-ray lithography. SU-8 shows high radiation stability. The fabrication technique enables high-quality lens structures regarding surface roughness and arrangement precision with arbitrary 2D geometry. To provide point foci, crossed pairs of lenses are used. Condenser lenses have been made utilizing deep x-ray lithographic patterning of thick SU-8 layers, too, whereas in this case, the aperture is limited due to process restrictions. Thus, in terms of large apertures, condenser lenses made of structured and rolled polyimide film are more attractive. Both condenser types, x-ray mosaic lenses and rolled x-ray prism lenses (RXPLs), are considered to be implemented into a microscope setup. The x-ray optical elements mentioned above are characterized with synchrotron radiation and x-ray laboratory sources, respectively.

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

DOE PAGES

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.; ...

2016-11-11

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

Nondestructive Imaging of Internal Structures of Frog (Xenopus laevis) Embryos by Shadow-Projection X-Ray Microtomography

NASA Astrophysics Data System (ADS)

Aoki, Sadao; Yoneda, Ikuo; Nagai, Takeharu; Ueno, Naoto; Murakami, Kazuo

1994-04-01

Nondestructive high-resolution imaging of frog ( Xenopus laevis) embryos has been developed by X-ray microtomography. Shadow-projection X-ray microtomography with a brilliant fine focus laboratory X-ray source could image fine structures of Xenopus embryos which were embedded in paraffin wax. The imaging system enabled us to not only distinguish endoderm from ectoderm at the gastrula stage, but also to obtain a cross-section view of the tail bud embryo showing muscle, notochord and neural tube without staining. Furthermore, the distribution of myosin was also imaged in combination with whole-mount immunohistochemistry.

Design of novel HIV-1 protease inhibitors incorporating isophthalamide-derived P2-P3 ligands: Synthesis, biological evaluation and X-ray structural studies of inhibitor-HIV-1 protease complex

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghosh, Arun K.; Brindisi, Margherita; Nyalapatla, Prasanth R.

Based upon molecular insights from the X-ray structures of inhibitor-bound HIV-1 protease complexes, we have designed a series of isophthalamide-derived inhibitors incorporating substituted pyrrolidines, piperidines and thiazolidines as P2-P3 ligands for specific interactions in the S2-S3 extended site. Compound 4b has shown an enzyme Ki of 0.025 nM and antiviral IC50 of 69 nM. An X-ray crystal structure of inhibitor 4b-HIV-1 protease complex was determined at 1.33 Å resolution. We have also determined X-ray structure of 3b-bound HIV-1 protease at 1.27 Å resolution. These structures revealed important molecular insight into the inhibitor–HIV-1 protease interactions in the active site.

Soft X-ray photoemission study of Co2(Cr1-xFex)Ga Heusler compounds

NASA Astrophysics Data System (ADS)

Tsunekawa, Masanori; Hattori, Yoshiro; Sekiyama, Akira; Fujiwara, Hidenori; Suga, Shigemasa; Muro, Takayuki; Kanomata, Takeshi; Imada, Shin

2015-08-01

We have performed soft X-ray photoemission spectroscopy (SXPES) and X-ray absorption spectroscopy (XAS) of the Co-based Heusler compounds Co2(Cr1-xFex)Ga (x = 0.0, 0.4, and 1.0) in order to study their electronic structures. Band-structure calculation was carried out and compared with the experimental results. SXPES spectra show hν-dependence, revealing the contributions of the Co, Cr, and Fe 3d electronic states in the valence band. The band width observed by the SXPES seems to be narrower than that predicted by the band-structure calculation. XAS spectra depend strongly on the the value of x in Co2(Cr1-xFex)Ga. The electron correlation effects are found to be stronger as x changes from 0.0 to 1.0.

High resolution x-ray absorption and emission spectroscopy of Li x CoO2 single crystals as a function delithiation

NASA Astrophysics Data System (ADS)

Simonelli, L.; Paris, E.; Iwai, C.; Miyoshi, K.; Takeuchi, J.; Mizokawa, T.; Saini, N. L.

2017-03-01

The effect of delithiation in Li x CoO2 is studied by high resolution Co K-edge x-ray absorption and x-ray emission spectroscopy. Polarization dependence of the x-ray absorption spectra on single crystal samples is exploited to reveal information on the anisotropic electronic structure. We find that the electronic structure of Li x CoO2 is significantly affected by delithiation in which the Co ions oxidation state tending to change from 3+  to 4+. The Co intersite (intrasite) 4p-3d hybridization suffers a decrease (increase) by delithiation. The unoccupied 3d t 2g orbitals with a 1g symmetry, containing substantial O 2p character, hybridize isotropically with Co 4p orbitals and likely to have itinerant character unlike anisotropically hybridized 3d e g orbitals. Such a peculiar electronic structure could have significant effect on the mobility of Li in Li x CoO2 cathode and hence the battery characteristics.

Partially coherent wavefront propagation simulations: Mirror and monochromator crystal quality assessment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wiegart, L., E-mail: lwiegart@bnl.gov; Fluerasu, A.; Chubar, O.

2016-07-27

We have applied fully-and partially-coherent synchrotron radiation wavefront propagation simulations, implemented in the “Synchrotron Radiation Workshop” (SRW) computer code, to analyse the effects of imperfect mirrors and monochromator at the Coherent Hard X-ray beamline. This beamline is designed for X-ray Photon Correlation Spectroscopy, a technique that heavily relies on the partial coherence of the X-ray beam and benefits from a careful preservation of the X-ray wavefront. We present simulations and a comparison with the measured beam profile at the sample position, which show the impact of imperfect optics on the wavefront.

Observation of Structure of Surfaces and Interfaces by Synchrotron X-ray Diffraction: Atomic-Scale Imaging and Time-Resolved Measurements

NASA Astrophysics Data System (ADS)

Wakabayashi, Yusuke; Shirasawa, Tetsuroh; Voegeli, Wolfgang; Takahashi, Toshio

2018-06-01

The recent developments in synchrotron optics, X-ray detectors, and data analysis algorithms have enhanced the capability of the surface X-ray diffraction technique. This technique has been used to clarify the atomic arrangement around surfaces in a non-contact and nondestructive manner. An overview of surface X-ray diffraction, from the historical development to recent topics, is presented. In the early stage of this technique, surface reconstructions of simple semiconductors or metals were studied. Currently, the surface or interface structures of complicated functional materials are examined with sub-Å resolution. As examples, the surface structure determination of organic semiconductors and of a one-dimensional structure on silicon are presented. A new frontier is time-resolved interfacial structure analysis. A recent observation of the structure and dynamics of the electric double layer of ionic liquids, and an investigation of the structural evolution in the wettability transition on a TiO2 surface that utilizes a newly designed time-resolved surface diffractometer, are presented.

X-ray aspects of the DAFT/FADA clusters

NASA Astrophysics Data System (ADS)

Guennou, L.; Durret, F.; Lima Neto, G. B.; Adami, C.

2012-12-01

We have undertaken the DAFT/FADA survey with the aim of applying constraints on dark energy based on weak lensing tomography as well as obtaining homogeneous and high quality data for a sample of 91 massive clusters in the redshift range [0.4,0.9] for which there are HST archive data. We have analysed the XMM-Newton data available for 42 of these clusters to derive their X-ray temperatures and luminosities and search for substructures. This study was coupled with a dynamical analysis for the 26 clusters having at least 30 spectroscopic galaxy redshifts in the cluster range. We present preliminary results on the coupled X-ray and dynamical analyses of these clusters.

Crystal and Vibrational Structure of Energetic 3,5-dinitro 1,3,5-oxadiazinane (DOD) by Single Crystal X-ray Diffractometry and Raman Spectroscopy

DTIC Science & Technology

2018-03-19

calculations using a temperature of 298 K. 15. SUBJECT TERMS 3,5-dinitro-1,3,5-oxadiazinane (DOD), X-ray crystallography , Raman, energetic material...X-ray analysis. 2.2 Characterization X-ray Crystallography . DOD crystals were characterized with a SuperNova, Dualflex, EosS2 diffractometer using

Separation and characterization of magnetic fractions from waste-to-energy bottom ash with an emphasis on the leachability of heavy metals.

PubMed

Wei, Yunmei; Mei, Xiaoxia; Shi, Dezhi; Liu, Guotao; Li, Li; Shimaoka, Takayuki

2017-06-01

Magnetic fractions were extracted from pulverized waste-to-energy (WTE) bottom ashes using a combined wet-dry extraction method. The resulting magnetic and non-magnetic fractions were subjected to compositional, mineralogical, and redox state analyses by X-ray diffraction (XRD), X-ray fluorescence, and X-ray photoelectron spectroscopy (XPS), respectively. The distribution and leaching toxicity of heavy metals were assessed to evaluate potential effects on the environment. Compositional analyses revealed that Fe accounted for 35% of the magnetic fraction of pulverized ashes, which was approximately seven times that of the raw ash. In addition to Fe, elemental Ni, Mn, and Cr were also significantly enriched in the magnetic fractions. The mineralogical analysis determined that Fe was primarily present as hematite and magnetite, and metallic iron was also identified in the magnetic fraction samples. The XPS analysis further proved the existence of zero-valence Fe. However, a significant amount of Fe remained in the non-magnetic fractions, which could partially be ascribed to the intergrowth structure of the various minerals. The elevated concentrations of toxicity characteristic leaching procedure (TCLP)-extracted Mn, Ni, Cr, Cu, Pb, and Zn were primarily ascribed to the lower buffering capability of the magnetic fractions, with the enrichment of Mn, Ni, and Cr in the magnetic fractions also contributing to this elevation.

Dissolution-Driven Permeability Reduction of a Fractured Carbonate Caprock

PubMed Central

Ellis, Brian R.; Fitts, Jeffrey P.; Bromhal, Grant S.; McIntyre, Dustin L.; Tappero, Ryan; Peters, Catherine A.

2013-01-01

Abstract Geochemical reactions may alter the permeability of leakage pathways in caprocks, which serve a critical role in confining CO2 in geologic carbon sequestration. A caprock specimen from a carbonate formation in the Michigan sedimentary Basin was fractured and studied in a high-pressure core flow experiment. Inflowing brine was saturated with CO2 at 40°C and 10 MPa, resulting in an initial pH of 4.6, and had a calcite saturation index of −0.8. Fracture permeability decreased during the experiment, but subsequent analyses did not reveal calcite precipitation. Instead, experimental observations indicate that calcite dissolution along the fracture pathway led to mobilization of less soluble mineral particles that clogged the flow path. Analyses of core sections via electron microscopy, synchrotron-based X-ray diffraction imaging, and the first application of microbeam Ca K-edge X-ray absorption near edge structure, provided evidence that these occlusions were fragments from the host rock rather than secondary precipitates. X-ray computed tomography showed a significant loss of rock mass within preferential flow paths, suggesting that dissolution also removed critical asperities and caused mechanical closure of the fracture. The decrease in fracture permeability despite a net removal of material along the fracture pathway demonstrates a nonintuitive, inverse relationship between dissolution and permeability evolution in a fractured carbonate caprock. PMID:23633894

Elucidation of structure and nature of the PdO-Pd transformation using in situ PDF and XAS techniques.

PubMed

Keating, Jonathan; Sankar, Gopinathan; Hyde, Timothy I; Kohara, Shinji; Ohara, Koji

2013-06-14

The PdO-Pd phase transformation in a 4 wt% Pd/Al2O3 catalyst has been investigated using in situ X-ray absorption spectroscopy (XAS) and in situ X-ray total scattering (also known as high-energy X-ray diffraction) techniques. Both the partial and total pair distribution functions (PDF) from these respective techniques have been analysed in depth. New information from PDF analysis of total scattering data has been garnered using the differential PDF (d-PDF) approach where only correlations orginating from PdO and metallic Pd are extracted. This method circumvents problems encountered in characerising the catalytically active components due to the diffuse scattering from the disordered γ-Al2O3 support phase. Quantitative analysis of the palladium components within the catalyst allowed for the phase composition to be established at various temperatures. Above 850 °C it was found that PdO had converted to metallic Pd, however, the extent of reduction was of the order ca. 70% Pd metal and 30% PdO. Complementary in situ XANES and EXAFS were performed, with heating to high temperature and subsequent cooling in air, and the results of the analyses support the observations, that residual PdO is detected at elevated temperatures. Hysteresis in the transformation upon cooling is confirmed from XAS studies where reoxidation occurs below 680 °C.

Imaging endosomes and autophagosomes in whole mammalian cells using correlative cryo-fluorescence and cryo-soft X-ray microscopy (cryo-CLXM)☆

PubMed Central

Duke, Elizabeth M.H.; Razi, Minoo; Weston, Anne; Guttmann, Peter; Werner, Stephan; Henzler, Katja; Schneider, Gerd; Tooze, Sharon A.; Collinson, Lucy M.

2014-01-01

Cryo-soft X-ray tomography (cryo-SXT) is a powerful imaging technique that can extract ultrastructural information from whole, unstained mammalian cells as close to the living state as possible. Subcellular organelles including the nucleus, the Golgi apparatus and mitochondria have been identified by morphology alone, due to the similarity in contrast to transmission electron micrographs. In this study, we used cryo-SXT to image endosomes and autophagosomes, organelles that are particularly susceptible to chemical fixation artefacts during sample preparation for electron microscopy. We used two approaches to identify these compartments. For early and recycling endosomes, which are accessible to externally-loaded markers, we used an anti-transferrin receptor antibody conjugated to 10 nm gold particles. For autophagosomes, which are not accessible to externally-applied markers, we developed a correlative cryo-fluorescence and cryo-SXT workflow (cryo-CLXM) to localise GFP-LC3 and RFP-Atg9. We used a stand-alone cryo-fluorescence stage in the home laboratory to localise the cloned fluorophores, followed by cryo-soft X-ray tomography at the synchrotron to analyse cellular ultrastructure. We mapped the 3D ultrastructure of the endocytic and autophagic structures, and discovered clusters of omegasomes arising from ‘hotspots’ on the ER. Thus, immunogold markers and cryo-CLXM can be used to analyse cellular processes that are inaccessible using other imaging modalities. PMID:24238600

Potential for Imaging Engineered Tissues with X-Ray Phase Contrast

PubMed Central

Appel, Alyssa; Anastasio, Mark A.

2011-01-01

As the field of tissue engineering advances, it is crucial to develop imaging methods capable of providing detailed three-dimensional information on tissue structure. X-ray imaging techniques based on phase-contrast (PC) have great potential for a number of biomedical applications due to their ability to provide information about soft tissue structure without exogenous contrast agents. X-ray PC techniques retain the excellent spatial resolution, tissue penetration, and calcified tissue contrast of conventional X-ray techniques while providing drastically improved imaging of soft tissue and biomaterials. This suggests that X-ray PC techniques are very promising for evaluation of engineered tissues. In this review, four different implementations of X-ray PC imaging are described and applications to tissues of relevance to tissue engineering reviewed. In addition, recent applications of X-ray PC to the evaluation of biomaterial scaffolds and engineered tissues are presented and areas for further development and application of these techniques are discussed. Imaging techniques based on X-ray PC have significant potential for improving our ability to image and characterize engineered tissues, and their continued development and optimization could have significant impact on the field of tissue engineering. PMID:21682604

How Rosalind Franklin Discovered the Helical Structure of DNA: Experiments in Diffraction

NASA Astrophysics Data System (ADS)

Braun, Gregory; Tierney, Dennis; Schmitzer, Heidrun

2011-03-01

Rosalind Franklin, a chemical physicist (1920-1958), used x-ray diffraction to determine the structure of DNA. What exactly could she read out from her x-ray pattern, shown in Fig. 1? In lecture notes dated November 1951, R. Franklin wrote the following: "The results suggest a helical structure (which must be very closely packed) containing 2, 3 or 4 co-axial nucleic acid chains per helical unit, and having the phosphate groups near the outside."2 This was 16 months before J. D. Watson and F. Crick published their description of DNA, which was based on R. Franklin's x-ray photos. How they gained access to her x-ray photos is a fascinating tale of clashing personalities and male chauvinism.2,3

Tetra- and Hexavalent Uranium Forms Bidentate-Mononuclear Complexes with Particulate Organic Matter in a Naturally Uranium-Enriched Peatland.

PubMed

Mikutta, Christian; Langner, Peggy; Bargar, John R; Kretzschmar, Ruben

2016-10-04

Peatlands frequently serve as efficient biogeochemical traps for U. Mechanisms of U immobilization in these organic matter-dominated environments may encompass the precipitation of U-bearing mineral(oid)s and the complexation of U by a vast range of (in)organic surfaces. The objective of this work was to investigate the spatial distribution and molecular binding mechanisms of U in soils of an alpine minerotrophic peatland (pH 4.7-6.6, E h = -127 to 463 mV) using microfocused X-ray fluorescence spectrometry and bulk and microfocused U L 3 -edge X-ray absorption spectroscopy. The soils contained 2.3-47.4 wt % organic C, 4.1-58.6 g/kg Fe, and up to 335 mg/kg geogenic U. Uranium was found to be heterogeneously distributed at the micrometer scale and enriched as both U(IV) and U(VI) on fibrous and woody plant debris (48 ± 10% U(IV), x̅ ± σ, n = 22). Bulk U X-ray absorption near edge structure (XANES) spectroscopy revealed that in all samples U(IV) comprised 35-68% of total U (x̅ = 50%, n = 15). Shell-fit analyses of bulk U L 3 -edge extended X-ray absorption fine structure (EXAFS) spectra showed that U was coordinated to 1.3 ± 0.2 C atoms at a distance of 2.91 ± 0.01 Å (x̅ ± σ), which implies the formation of bidentate-mononuclear U(IV/VI) complexes with carboxyl groups. We neither found evidence for U shells at ∼3.9 Å, indicative of mineral-associated U or multinuclear U(IV) species, nor for a substantial P/Fe coordination of U. Our data indicates that U(IV/VI) complexation by natural organic matter prevents the precipitation of U minerals as well as U complexation by Fe/Mn phases at our field site, and suggests that organically complexed U(IV) is formed via reduction of organic matter-bound U(VI).

The Chandra planetary nebula survey (CHANPLANS). II. X-ray emission from compact planetary nebulae

DOE Office of Scientific and Technical Information (OSTI.GOV)

Freeman, M.; Kastner, J. H.; Montez, R. Jr.

2014-10-20

We present results from the most recent set of observations obtained as part of the Chandra X-ray observatory Planetary Nebula Survey (CHANPLANS), the first comprehensive X-ray survey of planetary nebulae (PNe) in the solar neighborhood (i.e., within ∼1.5 kpc of the Sun). The survey is designed to place constraints on the frequency of appearance and range of X-ray spectral characteristics of X-ray-emitting PN central stars and the evolutionary timescales of wind-shock-heated bubbles within PNe. CHANPLANS began with a combined Cycle 12 and archive Chandra survey of 35 PNe. CHANPLANS continued via a Chandra Cycle 14 Large Program which targeted allmore » (24) remaining known compact (R {sub neb} ≲ 0.4 pc), young PNe that lie within ∼1.5 kpc. Results from these Cycle 14 observations include first-time X-ray detections of hot bubbles within NGC 1501, 3918, 6153, and 6369, and point sources in HbDs 1, NGC 6337, and Sp 1. The addition of the Cycle 14 results brings the overall CHANPLANS diffuse X-ray detection rate to ∼27% and the point source detection rate to ∼36%. It has become clearer that diffuse X-ray emission is associated with young (≲ 5 × 10{sup 3} yr), and likewise compact (R {sub neb} ≲ 0.15 pc), PNe with closed structures and high central electron densities (n{sub e} ≳ 1000 cm{sup –3}), and is rarely associated with PNe that show H{sub 2} emission and/or pronounced butterfly structures. Hb 5 is one such exception of a PN with a butterfly structure that hosts diffuse X-ray emission. Additionally, two of the five new diffuse X-ray detections (NGC 1501 and NGC 6369) host [WR]-type central stars, supporting the hypothesis that PNe with central stars of [WR]-type are likely to display diffuse X-ray emission.« less

Crystal structures, DFT calculations and Hirshfeld surface analyses of three new cobalt(III) Schiff base complexes derived from meso-1,2-diphenyl-1,2-ethylenediamine

NASA Astrophysics Data System (ADS)

Masoudi, Mohaddeseh; Behzad, Mahdi; Arab, Ali; Tarahhomi, Atekeh; Rudbari, Hadi Amiri; Bruno, Giuseppe

2016-10-01

Three new Cobalt(III) Schiff base complexes were synthesized and characterized by spectroscopic methods and x-ray crystallography. The DFT optimized structures of the complexes agreed well with the corresponding x-ray structures. According to the calculated vibrational normal modes, the observed signals in the IR spectra of the complexes were assigned. The experimental UV-Vis spectra of the complexes were also discussed considering the calculated excited states and molecular orbitals. Hirshfeld surface analysis was carried out to study the inter-contact interactions in these complexes. These studies provided comprehensive description of such inter-contact interactions by means of an appealing graphical approach using 3D Hirshfeld surfaces and 2D fingerprint plots derived from the surfaces. It indicated the dominant role of various hydrogen intermolecular interactions such as H⋯H (above 60%), C⋯H/H⋯C (near 15%-20%), O⋯H/H⋯O (about 16% or 17% for structures with counter ion ClO4-) and H⋯F (17% for structure with counter ion PF6-) contacts into the crystal packing which are discussed in details.

X-ray study of the structure of phospholipid monolayers on the water surface

NASA Astrophysics Data System (ADS)

Asadchikov, V. E.; Tikhonov, A. M.; Volkov, Yu. O.; Roshchin, B. S.; Ermakov, Yu. A.; Rudakova, E. B.; D'yachkova, I. G.; Nuzhdin, A. D.

2017-10-01

The possibility of laboratory X-ray reflectometry study of the structure of dimyristoyl phosphatidylserine (DMPS) phospholipid monolayers on the water surface in various phase states has been demonstrated.

De-MA: a web Database for electron Microprobe Analyses to assist EMP lab manager and users

NASA Astrophysics Data System (ADS)

Allaz, J. M.

2012-12-01

Lab managers and users of electron microprobe (EMP) facilities require comprehensive, yet flexible documentation structures, as well as an efficient scheduling mechanism. A single on-line database system for managing reservations, and providing information on standards, quantitative and qualitative setups (element mapping, etc.), and X-ray data has been developed for this purpose. This system is particularly useful in multi-user facilities where experience ranges from beginners to the highly experienced. New users and occasional facility users will find these tools extremely useful in developing and maintaining high quality, reproducible, and efficient analyses. This user-friendly database is available through the web, and uses MySQL as a database and PHP/HTML as script language (dynamic website). The database includes several tables for standards information, X-ray lines, X-ray element mapping, PHA, element setups, and agenda. It is configurable for up to five different EMPs in a single lab, each of them having up to five spectrometers and as many diffraction crystals as required. The installation should be done on a web server supporting PHP/MySQL, although installation on a personal computer is possible using third-party freeware to create a local Apache server, and to enable PHP/MySQL. Since it is web-based, any user outside the EMP lab can access this database anytime through any web browser and on any operating system. The access can be secured using a general password protection (e.g. htaccess). The web interface consists of 6 main menus. (1) "Standards" lists standards defined in the database, and displays detailed information on each (e.g. material type, name, reference, comments, and analyses). Images such as EDS spectra or BSE can be associated with a standard. (2) "Analyses" lists typical setups to use for quantitative analyses, allows calculation of mineral composition based on a mineral formula, or calculation of mineral formula based on a fixed amount of oxygen, or of cation (using an analysis in element or oxide weight-%); this latter includes re-calculation of H2O/CO2 based on stoichiometry, and oxygen correction for F and Cl. Another option offers a list of any available standards and possible peak or background interferences for a series of elements. (3) "X-ray maps" lists the different setups recommended for element mapping using WDS, and a map calculator to facilitate maps setups and to estimate the total mapping time. (4) "X-ray data" lists all x-ray lines for a specific element (K, L, M, absorption edges, and satellite peaks) in term of energy, wavelength and peak position. A check for possible interferences on peak or background is also possible. Theoretical x-ray peak positions for each crystal are calculated based on the 2d spacing of each crystal and the wavelength of each line. (5) "Agenda" menu displays the reservation dates for each month and for each EMP lab defined. It also offers a reservation request option, this request being sent by email to the EMP manager for approval. (6) Finally, "Admin" is password restricted, and contains all necessary options to manage the database through user-friendly forms. The installation of this database is made easy and knowledge of HTML, PHP, or MySQL is unnecessary to install, configure, manage, or use it. A working database is accessible at http://cub.geoloweb.ch.

The possible importance of synchrotron/inverse Compton losses to explain fast MM-wave and hard X-ray emission of a solar event

NASA Technical Reports Server (NTRS)

Correia, E.; Kaufmann, P.; Costa, J. E. R.; Vaz, A. M. Z.; Dennis, B. R.

1986-01-01

The solar burst of 21 May 1984 presented a number of unique features. The time profile consisted of seven major structures (seconds), with a turnover frequency or approx. 90 GHz, well correlated in time to hard X-ray emission. Each structure consisted of multiple fast pulses (.1 seconds), which were analyzed in detail. A proportionality between the repetition rate of the pulses and the burst fluxes at 90 GHz and or approx. 100 keV hard X-rays, and an inverse proportionality between repetition rates and hard X-rays power law indices have been found. A synchrotron/inverse Compton model has been applied to explain the emission of the fast burst structures, which appear to be possible for the first three or four structures.

The possible importance of synchrotron/inverse Compton losses to explain fast mm-wave and hard X-ray emission of a solar event

NASA Technical Reports Server (NTRS)

Correia, E.; Kaufmann, P.; Costa, J. E. R.; Zodivaz, A. M.; Dennis, B. R.

1986-01-01

The solar burst of 21 May 1984, presented a number of unique features. The time profile consisted of seven major structures (seconds), with a turnover frequency of greater than or approximately 90 GHz, well correlated in time to hard X-ray emission. Each structure consisted of multiple fast pulses (0.1 seconds), which were analyzed in detail. A proportionality between the repetition rate of the pulses and the burst fluxes at 90 GHz and greater than or approximately 100 keV hard X-rays, and an inverse proportionality between repetition rates and hard X-ray power law indices were found. A synchrotron/inverse Compton model was applied to explain the emission of the fast burst structures, which appear to be possible for the first three or four structures.

The X-ray corona and the photospheric magnetic field.

NASA Technical Reports Server (NTRS)

Krieger, A. S.; Vaiana, G. S.; Van Speybroeck, L. P.

1971-01-01

Soft X-ray photographs of the solar corona have been obtained on four flights of a rocket-borne grazing incidence telescope having a resolution of a few arc sec. The configuration of the X-ray emitting structures in the corona has been compared to the magnetic field distribution measured by photospheric longitudinal magnetograms. The X-ray structures trace the three-dimensional configuration of the magnetic field through the lower corona. Active regions in the corona take the form of tubular structures connecting regions of opposite magnetic polarity within the same or adjacent chromospheric active regions. Higher, larger structures link widely separated active regions into complexes of activity covering substantial fractions of the disk. The complexes are separated by areas of low average field in the photosphere. Interconnections across the solar equator appear to originate over areas of preceding polarity.

Activated carbon-supported CuO nanoparticles: a hybrid material for carbon dioxide adsorption

NASA Astrophysics Data System (ADS)

Boruban, Cansu; Esenturk, Emren Nalbant

2018-03-01

Activated carbon-supported copper(II) oxide (CuO) nanoparticles were synthesized by simple impregnation method to improve carbon dioxide (CO2) adsorption capacity of the support. The structural and chemical properties of the hybrid material were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction (https://www.google.com.tr/url?sa=t&rct=j&q=&esrc=s&source=web&cd=3&cad=rja&uact=8&ved=0CCsQFjAC&url=http%3A%2F%2Fwww.intertek.com%2Fanalytical-laboratories%2Fxrd%2F&ei=-5WZVYSCHISz7Aatqq-IAw&usg=AFQjCNFBlk-9wqy49foh8tskmbD-GGbG9g&sig2=eKrhYjO75rl_Id2sLGpq4w&bvm=bv.96952980,d.bGg) (XRD), X-ray photoelectron spectroscopy (XPS), atomic absorption spectroscopy (AAS), and Brunauer-Emmett-Teller (BET) analyses. The analyses showed that CuO nanoparticles are well-distributed on the activated carbon surface. The CO2 adsorption behavior of the activated carbon-supported CuO nanoparticles was observed by thermogravimetric analysis (TGA), temperature programmed desorption (TPD), Fourier transform infrared (FTIR), and BET analyses. The results showed that CuO nanoparticle loading on activated carbon led to about 70% increase in CO2 adsorption capacity of activated carbon under standard conditions (1 atm and 298 K). The main contributor to the observed increase is an improvement in chemical adsorption of CO2 due to the presence of CuO nanoparticles on activated carbon.

Publications - GMC 420 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 420 Publication Details Title: X-Ray fluorescence spectroscopy and 40Ar/39Ar analyses of core more information. Quadrangle(s): Ikpikpuk River; Umiat Bibliographic Reference Shimer, G., 2013, X-Ray

Application of a magnetograph and X-ray telescope to the study of coronal structure variations

NASA Technical Reports Server (NTRS)

Rust, D. M.

1980-01-01

The application of magnetographs and X-ray imaging techniques to determine the magnitude, structure, origin, and evolution of the solar coronal magnetic field is examined. The spatial and temporal resolution of the X-ray telescope is discussed and a comparison of ground based magnetogram sequences versus a magnetograph in space is presented. Skylab photographs of the evolution of transient coronal holes are provided.

Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

NASA Astrophysics Data System (ADS)

Parrot, I. M.; Urban, V.; Gardner, K. H.; Forsyth, V. T.

2005-08-01

The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar® or Twaron®.

Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance

PubMed Central

Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

2016-01-01

The structure of nanocrystalline calcium silicate hydrates (C–S–H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH)2-like structure, nanocrystalline and intermixed with C–S–H layers, at high Ca/Si ratios. PMID:27275135

Large-area soft x-ray projection lithography using multilayer mirrors structured by RIE

NASA Astrophysics Data System (ADS)

Rahn, Steffen; Kloidt, Andreas; Kleineberg, Ulf; Schmiedeskamp, Bernt; Kadel, Klaus; Schomburg, Werner K.; Hormes, F. J.; Heinzmann, Ulrich

1993-01-01

SXPL (soft X-ray projection lithography) is one of the most promising applications of X-ray reflecting optics using multilayer mirrors. Within our collaboration, such multilayer mirrors were fabricated, characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors were produced by electron beam evaporation in UHV under thermal treatment with an in-situ X-ray controlled thickness in the region of 2d equals 14 nm. The reflectivities measured at normal incidence reached up to 54%. Various surface analysis techniques have been applied in order to characterize and optimize the X-ray mirrors. The multilayers were patterned by reactive ion etching (RIE) with CF(subscript 4), using a photoresist as the etch mask, thus producing X-ray reflection masks. The masks were tested in the synchrotron radiation laboratory of the electron accelerator ELSA at the Physikalisches Institut of Bonn University. A double crystal X-ray monochromator was modified so as to allow about 0.5 cm(superscript 2) of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto the resist (Hoechst AZ PF 514), which was mounted at an average distance of about 7 mm. In the first test-experiments, structure sizes down to 8 micrometers were nicely reproduced over the whole of the exposed area. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

Polyclonal chromosomal evolution in a benign mixed salivary gland tumor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mark, J.; Ekedahl, C.

1987-10-01

Banding analyses of a human benign pleomorphic adenoma in the parotid gland revealed a polyclonal pattern where structural rearrangements predominated. These deviations were different from the anomalies previously observed in 100 mixed tumors. The reason found for the differences in all likelihood was x-ray treatment of tuberculous lymphadenitis in the neck during childhood. Implications regarding origin and development of pleomorphic adenomas are discussed.

A covalent G-site inhibitor for glutathione S-transferase Pi (GSTP1-1).

PubMed

Shishido, Yuko; Tomoike, Fumiaki; Kimura, Yasuaki; Kuwata, Keiko; Yano, Takato; Fukui, Kenji; Fujikawa, Haruka; Sekido, Yoshitaka; Murakami-Tonami, Yuko; Kameda, Tomoshi; Shuto, Satoshi; Abe, Hiroshi

2017-10-10

We herein report the first covalent G-site-binding inhibitor for GST, GS-ESF (1), which irreversibly inhibited the GSTP 1-1 function. LC-MS/MS and X-ray structure analyses of the covalently linked GST-inhibitor complex suggested that 1 reacted with Tyr108 of GSTP 1-1 . The mechanism of covalent bond formation was discussed based on MD simulation results.

Thermal expansion in UO 2 determined by high-energy X-ray diffraction

DOE PAGES

Guthrie, M.; Benmore, C. J.; Skinner, L. B.; ...

2016-06-24

In this study, we present crystallographic analyses of high-energy X-ray diffraction data on polycrystalline UO 2 up to the melting temperature. The Rietveld refinements of our X-ray data are in agreement with previous measurements, but are systematically located around the upper bound of their uncertainty, indicating a slightly steeper trend of thermal expansion compared to established values. This observation is consistent with recent first principles calculations.

X-rays from supernova 1987A

NASA Technical Reports Server (NTRS)

Xu, Yueming; Sutherland, Peter; Mccray, Richard; Ross, Randy R.

1988-01-01

Detailed calculations of the development of the X-ray spectrum of 1987A are presented using more realistic models for the supernova composition and density structure provided by Woosley. It is shown how the emergence of the X-ray spectrum depends on the parameters of the model and the nature of its central energy source. It is shown that the soft X-ray spectrum should be dominated by a 6.4 keV Fe K(alpha) emission line that could be observed by a sensitive X-ray telescope.